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Hardware Guide

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100% found this document useful (1 vote)
387 views366 pages

Hardware Guide

Uploaded by

Green Life Style
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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Notice

The information contained in this document is subject to change without notice.


PERKIN-ELMER MAKES NO WARRANTY OF ANY KIND WITH REGARD TO THIS
MATERIAL, INCLUDING, BUT NOT LIMITED TO, THE IMPLIED WARRANTIES OF
MERCHANTABILITY AND FITNESS FOR A PARTICULAR PURPOSE. Perkin-Elmer shall not
be liable for errors contained herein or for incidental consequential damages in connection with the
furnishing, performance, or use of this material.

Copyright Information
Reproduction or publication of this document in any form or format prohibited without written
permission of The Perkin-Elmer Corporation or any of its subsidiaries.
Copyright © 1998 The Perkin-Elmer Corporation.
All rights reserved.
Printed in the United States of America.

Software programs are protected by copyright. It is unlawful to duplicate these programs in any
manner other than for the user's personal use. Specifically, it is unlawful to use or duplicate these
programs other than for use with the purchaser's original computer.

Release Information
Manual
Part No. Release Release Date
0993-6088 Rev. E June 1998

Trademarks
Perkin-Elmer is a registered trademark of The Perkin-Elmer Corporation.
Intensitron is a registered trademark of The Perkin-Elmer Corporation.
GemTip is a trademark of The Perkin-Elmer Corporation.
Lumina is a trademark of The Perkin-Elmer Corporation.
AAnalyst is a trademark of The Perkin-Elmer Corporation.
FIAS is a trademark of The Perkin-Elmer Corporation.
HGA is a trademark of The Perkin-Elmer Corporation.
AA WinLab is a trademark of The Perkin-Elmer Corporation.
MS-DOS, Windows, and Microsoft are registered trademarks of Microsoft Corporation.
Registered names, trademarks, etc. used in this document, even when not specifically marked as
such, are protected by law.
Contents

Contents......................................................................................i

Safety and Regulatory Information ...........................................xv


Introduction.............................................................................................................. xv
Location of Safety Information ................................................................................. xv
FCC Compliance (United States)............................................................................. xvi
Electrical Protection Compliance............................................................................. xvi
Electrical Warnings................................................................................................. xvi
Symbols Used on the Instrument............................................................................. xvii
Warnings and Labels on the Instrument ................................................................ xviii
Customer Service ................................................................................................... xxii

Introduction............................................................................ xxv
What is Atomic Absorption?....................................................................................xxv
What is Flame AA? ............................................................................................... xxvi
What is Graphite Furnace AA?.............................................................................. xxvi
The AAnalyst Series Instruments ......................................................................... xxvii
Manuals and Documents ..................................................................................... xxviii
What’s in this Hardware Guide?............................................................................. xxx
ii
Using this Manual .................................................................................................. xxx
Manual Conventions ....................................................................................... xxxi
Using the Index ............................................................................................... xxxi
A Word on Troubleshooting ............................................................................ xxxi

Chapter 1 Safety Practices.................................................... 1-1


Introduction to this Chapter..................................................................................... 1-1
Using This Chapter ................................................................................................. 1-1
Laboratory Safety Guidelines................................................................................... 1-2
General Safety Guidelines ................................................................................. 1-2
Environmental Safety Conditions ...................................................................... 1-2
Handling the Instrument Safely ......................................................................... 1-3
Laboratory Ventilation Safety ............................................................................ 1-3
General Safety Practices .......................................................................................... 1-3
Ultraviolet Radiation Safety............................................................................... 1-3
Electrical Safety ................................................................................................ 1-4
Hazardous Chemicals Warnings ........................................................................ 1-7
Safe Handling of Gas Cylinders......................................................................... 1-8
Identifying Cylinders .............................................................................. 1-9
Storing Cylinders .................................................................................... 1-9
Handling Cylinders ............................................................................... 1-10
Safe Handling of Atomizers............................................................................. 1-10
Safe Use of Chemical Reagents........................................................................ 1-11
Protective Equipment ............................................................................ 1-11
Reagent Use, Storage, and Disposal ...................................................... 1-11
Waste Disposal Procedures .............................................................................. 1-12
Flame Analyses Safety Practices ............................................................................ 1-13
Safety Interlocks.............................................................................................. 1-13
Burner Gases (in General) ............................................................................... 1-13
Air Supply....................................................................................................... 1-14
Acetylene ........................................................................................................ 1-14
Nitrous Oxide.................................................................................................. 1-15
Safety Checks Before Ignition.......................................................................... 1-16
Burner Head.......................................................................................... 1-17
Burner Chamber and End Cap .............................................................. 1-17
Nebulizer .............................................................................................. 1-17
Drain System ........................................................................................ 1-17
Hazards with Flame Analyses.......................................................................... 1-18
General Precautions .............................................................................. 1-18
Flashbacks ............................................................................................ 1-18
Ultraviolet Radiation Hazards ............................................................... 1-19
iii
High Temperatures ............................................................................... 1-19
Acetone Carryover ................................................................................ 1-19
Acetylides ............................................................................................. 1-20
Organic Solvents................................................................................... 1-20
Cyanide Solutions ................................................................................. 1-20
Graphite Furnace Analyses Safety Practices........................................................... 1-21
Safety Interlocks.............................................................................................. 1-21
Inert Gas Supply.............................................................................................. 1-21
Argon.............................................................................................................. 1-21
Safety Checks.................................................................................................. 1-22
Hazards with Furnace Analyses ....................................................................... 1-22
UV Radiation........................................................................................ 1-22
High Temperatures ............................................................................... 1-23
Mercury/Hydride Analyses Safety Practices ........................................................... 1-24
Inert Gas Supply.............................................................................................. 1-24
Quartz Cells .................................................................................................... 1-24
Safety Checks.................................................................................................. 1-24
Hazards with Mercury/Hydride Determination System Analyses...................... 1-25
High Temperatures ............................................................................... 1-25
Sodium Tetrahydroborate (Sodium Borohydride) .................................. 1-25
Tin (II) Chloride (Stannous Chloride) ................................................... 1-26
Hydrofluoric Acid ................................................................................. 1-26
Magnesium Perchlorate......................................................................... 1-27
Sample Preparation Safety Practices ...................................................................... 1-28
Dissolving Solid Samples in Organics ............................................................. 1-28
Dissolving Solid Samples Using Acids ............................................................ 1-29
Acid Digestions............................................................................................... 1-29
Fusion Mixtures .............................................................................................. 1-31
References............................................................................................................. 1-33
iv

Chapter 2 System Descriptions............................................. 2-1


Introduction to this Chapter..................................................................................... 2-1
AAnalyst 100 Overview........................................................................................... 2-2
AAnalyst 100 System Information ........................................................................... 2-3
AAnalyst 100 Instrument Details............................................................................. 2-6
Spectrometer Portion Description ...................................................................... 2-8
Lamp Compartment Description...................................................................... 2-10
Deuterium Arc Background Corrector (Optional) ............................................ 2-11
Sample Area Description................................................................................. 2-11
Burner System Description .............................................................................. 2-12
Flame Gas Control Description........................................................................ 2-14
Interlocks Description ..................................................................................... 2-14
User Interface Description ............................................................................... 2-16
Keypad/Display..................................................................................... 2-16
Data Handling Features......................................................................... 2-17
AA WinLab System Controller (Optional Upgrade) .............................. 2-17
AAnalyst 300 Overview......................................................................................... 2-19
AAnalyst 300 System Information ......................................................................... 2-20
AAnalyst 300 Instrument Details........................................................................... 2-23
Spectrometer Portion Description .................................................................... 2-24
Lamp Compartment Description...................................................................... 2-26
Deuterium Arc Background Corrector ............................................................. 2-26
Sample Area Description................................................................................. 2-27
Burner System Description .............................................................................. 2-27
Flame Gas Control Description........................................................................ 2-28
Interlocks Description ..................................................................................... 2-28
User Interface Description ............................................................................... 2-28
AA WinLab System Controller ............................................................. 2-29
AA WinLab Software............................................................................ 2-30
Atomizers.............................................................................................................. 2-32
Burner System (Supplied)................................................................................ 2-32
Graphite Furnace System (HGA-800) .............................................................. 2-32
Mercury/Hydride Determination System (MHS-10) ......................................... 2-34
Flow Injection Analysis System (FIAS-100 or FIAS-400) ................................ 2-36
Autosamplers ........................................................................................................ 2-38
Flame or FIAS Autosampler (AS-90 and AS-91) ............................................. 2-38
Graphite Furnace Autosampler........................................................................ 2-40
v
Options And Upgrades .......................................................................................... 2-41
HGA-800 Graphite Furnace System (B300-1294)............................................ 2-41
Water Cooling System..................................................................................... 2-41
Mercury/Hydride Determination System (MHS-10) ......................................... 2-41
Flow Injection Analysis System (FIAS 100 or FIAS 400)................................. 2-41
Flame or FIAS Autosampler (AS-90 and AS-91) ............................................. 2-42
Graphite Furnace Autosampler........................................................................ 2-42
Quartz Cell Holder (B300-0348)...................................................................... 2-42
Electrical Heater Assembly Adapter (N040-1183)............................................ 2-42
Deuterium Arc Background Corrector ............................................................. 2-42
Lamp Options.................................................................................................. 2-43
Burner Head Options....................................................................................... 2-44
Computer System Upgrade .............................................................................. 2-45
AA WinLab Controller Kit (N040-0110)............................................... 2-45
AA WinLab Software Kit (N040-0109)................................................. 2-46
AA WinLab Upgrade Kit (N040-0111) ................................................. 2-47
Printer Options (and accessories)..................................................................... 2-47
Okidata Microline 320 Printer............................................................... 2-47
H-P LaserJet IV Printer (0942-1038)..................................................... 2-47
H-P DeskJet 660C Printer (0942-1082) ................................................. 2-47
Parallel Printer Cable (0941-0001)........................................................ 2-48

Chapter 3 Preparing Your Laboratory................................... 3-1


Introduction to this Chapter..................................................................................... 3-1
Environmental Requirements .................................................................................. 3-2
Bench Requirements................................................................................................ 3-2
Exhaust Vent Requirements .................................................................................... 3-5
Blower and Vent Kit.......................................................................................... 3-7
Blower Information ........................................................................................... 3-7
Exhaust Vent Tubing......................................................................................... 3-8
Installing a Venting System............................................................................... 3-8
Gas Supply Requirements...................................................................................... 3-11
General ........................................................................................................... 3-11
Air Supply Requirements................................................................................. 3-12
Acetylene Supply Requirements....................................................................... 3-14
Nitrous Oxide Supply Requirements ................................................................ 3-16
Argon Requirements........................................................................................ 3-18
Electrical Requirements......................................................................................... 3-19
Cooling Accessories .............................................................................................. 3-20
vi

Chapter 4 Installation ........................................................... 4-1


Introduction to this Chapter..................................................................................... 4-1
Installation Summary: AAnalyst 100 ....................................................................... 4-2
Inspecting the Shipment .......................................................................................... 4-3
Unpacking the AAnalyst 100 Instrument ................................................................. 4-3
Instrument Part Numbers................................................................................... 4-3
How to Unpack the Instrument .......................................................................... 4-4
Carton Recycling Instructions............................................................................ 4-6
Shipping Lists ................................................................................................... 4-8
Spares Kits ...................................................................................................... 4-10
Who to Call? ................................................................................................... 4-12
Assembling the AAnalyst 100 ............................................................................... 4-12
Place Instrument on the Bench ........................................................................ 4-12
Assembly Overview, What’s Next?.................................................................. 4-13
Assembling the Quick-Change Burner Mount Assembly ................................. 4-15
Installing the Nebulizer on the Burner .................................................. 4-15
Checking that the Burner End Cap is Secure......................................... 4-18
Connecting and Securing the Gas Hoses to the Burner .......................... 4-19
Installing and Securing the Burner Head............................................... 4-21
Checking that the Ignitor Box Connectors are Plugged In ..................... 4-22
Installing the Quick-Change Burner Mount Assembly ..................................... 4-23
Plugging in the Main Interlock Connector ....................................................... 4-24
Installing the Burner Drain System ................................................................. 4-25
Connecting the Burner Drain System .................................................... 4-25
Adding Water to the Drain Float Assembly ........................................... 4-27
Installing the Burner Door............................................................................... 4-28
Installing the Lamp Compartment Cover......................................................... 4-29
Installing the Sample Trays ............................................................................. 4-30
Installing the Lamp(s) ..................................................................................... 4-31
Setting Up the EDL Power Supply................................................................... 4-50
Connecting the Gas Supplies ................................................................................. 4-52
Connecting to the Air Supply .......................................................................... 4-53
Requirements ........................................................................................ 4-53
Air Compressor Setup ........................................................................... 4-53
Air Cylinder Setup ................................................................................ 4-54
Connecting to the Acetylene Supply ................................................................ 4-55
Requirements ........................................................................................ 4-55
Acetylene Warnings .............................................................................. 4-55
Air/Acetylene Filter Assembly Setup..................................................... 4-55
Recommended Acetylene Supply Setup ................................................. 4-56
vii
Connecting to the Nitrous Oxide Supply.......................................................... 4-57
Requirements ........................................................................................ 4-57
Recommended Nitrous Oxide Supply Setup........................................... 4-57
Connecting to the Argon Supply...................................................................... 4-58
Requirements ........................................................................................ 4-58
Recommended Argon Supply Setup ...................................................... 4-59
Connecting the Electrical Supply........................................................................... 4-60
A Review of the Electrical Specifications......................................................... 4-60
How to Find Out the Instrument Voltage Setting ............................................. 4-61
If You Have 220 VAC in Your Lab ................................................................. 4-62
Changing the Instrument Operating Voltage ................................................... 4-62
Changing a Fuse.............................................................................................. 4-64
Changing the Setting on the Voltage Selector Board........................................ 4-65
Installing the AC Line Cord ............................................................................ 4-66
Setting Up the Okidata 320 Printer........................................................................ 4-68
Powering Up the Instrument.................................................................................. 4-72
Post Installation Adjustments and Checks.............................................................. 4-73
Aligning the Lamp(s) ...................................................................................... 4-73
Adjusting the Burner Height............................................................................ 4-74
Adjusting the Gas Flows for Ignition ............................................................... 4-76
Igniting the Flame ........................................................................................... 4-78
Adjusting the Burner Position.......................................................................... 4-78
Adjusting the Nebulizer................................................................................... 4-79
Sample Introduction System Pre-Conditioning ................................................ 4-80
Checking the Nitrous Oxide Flame (for Nitrous Oxide-Acetylene Analysis) .... 4-81

Chapter 5 Lamps .................................................................. 5-1


Introduction to this Chapter..................................................................................... 5-1
General Lamp Information ...................................................................................... 5-1
An Explanation: Hollow Cathode Lamps (HCLs) .................................................... 5-3
Lumina Hollow Cathode Lamps ........................................................................ 5-4
Intensitron Hollow Cathode Lamps.................................................................... 5-4
An Explanation: Electrodeless Discharge Lamps (EDLs)......................................... 5-6
Lamp Installation .................................................................................................... 5-7
Lamp Alignment ..................................................................................................... 5-7
Lamp Maintenance and Cleaning ............................................................................ 5-7
Lamp Life ............................................................................................................... 5-7
Lamp Troubleshooting ............................................................................................ 5-7
viii
Replacing the Lamps ............................................................................................... 5-8
Lamp Compartment Location ............................................................................ 5-8
Replacing the Lumina HCL............................................................................... 5-9
Replacing the Lumina HCL (Turret Model)..................................................... 5-10
Replacing the Coded Intensitron HCL ............................................................. 5-11
Replacing the Coded Intensitron HCL (Turret Model) ..................................... 5-13
Replacing the Non-Coded Intensitron HCL ..................................................... 5-14
Replacing the Non-coded Intensitron HCL (Turret Model) .............................. 5-16
Replacing the Coded Electrodeless Discharge Lamp........................................ 5-18
Replacing the Coded Electrodeless Discharge Lamp (Turret Model)................ 5-20
Replacing the Non-Coded Electrodeless Discharge Lamp ................................ 5-22
Replacing the Non-Coded Electrodeless Discharge Lamp (Turret)................... 5-24
The Deuterium Arc Background Corrector ............................................................ 5-26
An Explanation: The Deuterium Arc Background Corrector.................................. 5-26
Replacing the Deuterium Arc Background Corrector Lamp ................................... 5-26
Equipment Needed .......................................................................................... 5-27
Removing the Deuterium Lamp Assembly....................................................... 5-27
Replacing the Deuterium Lamp ....................................................................... 5-28
Reassembling the Deuterium Lamp Assembly ................................................. 5-29
Aligning the Deuterium Arc Lamp Assembly .................................................. 5-30

Chapter 6 Burner System...................................................... 6-1


Introduction to this Chapter..................................................................................... 6-1
Burner System Details ............................................................................................. 6-2
How the Burner System Works.......................................................................... 6-4
Burner Part Details............................................................................................ 6-6
Burner Installation ................................................................................................ 6-12
Burner Pre-Ignition Checklist................................................................................ 6-12
Check: Burner Head is Securely Latched ......................................................... 6-13
Check: Ignitor Box Connectors are Plugged In ................................................ 6-14
Check: Burner End Cap is Tightened Securely ................................................ 6-15
Check: AUX Oxidant, NEB Oxidant and Fuel Hoses are Secure...................... 6-15
Check: Nebulizer is Securely Clamped to the Burner End Cap ........................ 6-16
Check: Main Interlock Connector is Plugged in............................................... 6-17
Check: Drain Interlock is Plugged In............................................................... 6-18
Check: Drain Hose is Securely Attached to the Burner End Cap ...................... 6-18
Check: Water is Present in the Drain System Float Assembly .......................... 6-19
Lighting the Burner............................................................................................... 6-20
Burner System Maintenance.................................................................................. 6-20
Burner System Troubleshooting............................................................................. 6-20
Burner Spare Parts and Accessories....................................................................... 6-20
ix

Chapter 7 Maintenance......................................................... 7-1


Introduction to this Chapter..................................................................................... 7-1
General Maintenance Checklist ............................................................................... 7-2
Instrument Maintenance Checklist .......................................................................... 7-2
Cleaning the Instrument .......................................................................................... 7-3
Burner System Maintenance Checklist .................................................................... 7-4
Removing the Burner Door...................................................................................... 7-5
Replacing the Burner Door...................................................................................... 7-6
Removing the Burner Assembly from the Instrument............................................... 7-7
Removing the Burner Head ..................................................................................... 7-8
Cleaning the Burner Head ....................................................................................... 7-9
Frequency.......................................................................................................... 7-9
Quick Cleaning Procedure................................................................................. 7-9
Complete Cleaning Procedure ........................................................................... 7-9
Cleaning the Burner Chamber ............................................................................... 7-11
Cleaning the Burner Chamber After Use with Organic Solvents ...................... 7-11
Cleaning the Burner after Aspirating Cu, Ag, or Hg Samples .......................... 7-12
Disassembling the Burner Chamber....................................................................... 7-12
Thoroughly Cleaning the Burner Chamber Parts ............................................. 7-14
Reassembling the Burner....................................................................................... 7-15
Pre-Conditioning a New Burner or Drain Tube...................................................... 7-16
Cleaning the Nebulizer.......................................................................................... 7-17
To Clear an Obstruction in the Capillary or Teflon Tubes................................ 7-17
To Clear an Obstruction in the Nebulizer ........................................................ 7-17
Removing the Nebulizer ........................................................................................ 7-18
Disassembling the Nebulizer ........................................................................... 7-19
Cleaning the Disassembled Nebulizer.............................................................. 7-20
Reassembling the Nebulizer................................................................................... 7-20
Cleaning the High-Sensitivity Nebulizer.......................................................... 7-22
Drain System Maintenance.................................................................................... 7-23
Cleaning (or Flushing) the Drain System......................................................... 7-24
Replacing the Drain Tubing ............................................................................ 7-24
Preparing the New Drain Tubing for Use......................................................... 7-25
Cleaning the Drain Float Assembly ................................................................. 7-26
Adding Water to the Drain Float Assembly ..................................................... 7-27
Changing a Fuse.................................................................................................... 7-28
x
Ordering Supplies and Accessories........................................................................ 7-30
Lamp Maintenance................................................................................................ 7-30
Primary Source Lamps .................................................................................... 7-30
Deuterium Arc Lamps ..................................................................................... 7-30
Acetylene Gas Tank Maintenance.......................................................................... 7-31
AS-90 and AS-91 Autosampler Maintenance ........................................................ 7-32
Routine Maintenance....................................................................................... 7-32
Spare Parts ...................................................................................................... 7-32
Servicing ......................................................................................................... 7-32
MHS-10 Mercury/Hydride System Maintenance .................................................... 7-33
Replacing or Installing the MHS-10 Quartz Cell Holder.................................. 7-33
Replacing or Installing the MHS-10 Quartz Cell onto the Holder .................... 7-34
HGA-800 Graphite Furnace Maintenance.............................................................. 7-36
Routine Maintenance Checklist ....................................................................... 7-36
FIAS-100/400 Maintenance................................................................................... 7-36
Routine Maintenance Checklist ....................................................................... 7-36
Spare Parts and Accessories................................................................................... 7-37
Burner and Accessories ................................................................................... 7-37
Burner Gasket Kit (0047-0988) ....................................................................... 7-37
Burner Heads .................................................................................................. 7-37
Nebulizers and Accessories.............................................................................. 7-38
Drain System................................................................................................... 7-38
Deuterium Arc Background Correction Lamp.................................................. 7-38

Chapter 8 Troubleshooting ................................................... 8-1


Introduction to this Chapter..................................................................................... 8-1
Flame Analysis Troubleshooting.............................................................................. 8-2
Flame/Burner Troubleshooting ................................................................................ 8-7
Lamp Troubleshooting .......................................................................................... 8-10
Troubleshooting Deuterium Background Corrector Problems ................................ 8-13
Error Messages...................................................................................................... 8-14

Index
xi

List of Figures

Safety and Regulatory Information


Figure A. Labels located on the right side of the AAnalyst.................................. xviii
Figure B. Labels located on the back of the AAnalyst. .......................................... xix
Figure C. Warning labels located inside the top of an instrument with the
Deuterium Arc Background Corrector option. ....................................... xx

Introduction
Figure D. Simplified drawing of a basic flame atomic absorption system. .............xxv
Figure E. The basic AAnalyst 100 instrument.................................................... xxvii
Figure F. The basic AAnalyst 300 instrument.................................................... xxvii

Chapter 2 System Descriptions


Figure 2-1. The AAnalyst 100 instrument............................................................. 2-2
Figure 2-2. Block diagram representation of the AAnalyst 100 system.................. 2-4
Figure 2-3. Possible configurations of the AAnalyst 100 system............................ 2-5
Figure 2-4. General location of subassemblies in the AAnalyst 100. ..................... 2-7
Figure 2-5. The optical schematic of the AAnalyst 100......................................... 2-9
Figure 2-6. Single lamp mount and an HCL in the AAnalyst 100. ...................... 2-10
Figure 2-7. Sample compartment door (the burner door)..................................... 2-11
Figure 2-8. The burner system and its parts. ....................................................... 2-12
Figure 2-9. Location of the main interlock connector.......................................... 2-15
Figure 2-10. AAnalyst 100 keypad and display................................................... 2-16
Figure 2-11. The basic AAnalyst 300 instrument................................................ 2-19
Figure 2-12. Block diagram representation of the AAnalyst 300 systems. ........... 2-21
Figure 2-13. Possible configurations of the AAnalyst 300 system........................ 2-22
Figure 2-14. General location of subassemblies in the AAnalyst 300. ................. 2-23
Figure 2-15. The optical schematic for the AAnalyst 300.................................... 2-25
Figure 2-16. The HGA-800 Graphite Furnace with optional Autosampler. ......... 2-32
Figure 2-17 The MHS-10 and its parts............................................................... 2-34
Figure 2-18. The MHS-10 sample cell mounted on the burner. ........................... 2-35
Figure 2-19. A view of the FIAS-400 system. ..................................................... 2-36
Figure 2-20. The Intensitron coded lamp adapter cable....................................... 2-43
Figure 2-21. The Intensitron non-coded lamp adapter cable................................ 2-43
Figure 2-22. Lamp coding plug for the EDLs...................................................... 2-44
xii

Chapter 3 Preparing Your Laboratory


Figure 3-1. Dimensions of the AAnalyst 100. ....................................................... 3-3
Figure 3-2. Dimensions of the AAnalyst 300, HGA-800 Furnace and chiller. ....... 3-4
Figure 3-3. Location of exhaust vent (typical both instruments). ........................... 3-6
Figure 3-4. Dimensions of the exhaust vent. ......................................................... 3-9
Figure 3-5. Dimensions of the blower. .................................................................. 3-9
Figure 3-6. The PE cooling system recirculator attached to the HGA-800. .......... 3-20

Chapter 4 Installation
Figure 4-1. An exploded view of the shipping carton. ........................................... 4-4
Figure 4-2. Lifting the instrument out of the box. ................................................. 4-5
Figure 4-3. Breaking down the shipping carton for storage................................... 4-7
Figure 4-4. The quick-change burner mount assembly. ....................................... 4-13
Figure 4-5. Installing the nebulizer onto the burner end cap. .............................. 4-15
Figure 4-6. Nebulizer clamp securing the nebulizer flange in place. ................... 4-16
Figure 4-7. Checking that the burner end cap is secure. ...................................... 4-18
Figure 4-8. Securing the gas hoses to the burner end cap. ................................... 4-19
Figure 4-9. Confirm that the burner head is in place and latched securely........... 4-21
Figure 4-10. Rear view of the ignitor box assembly............................................. 4-22
Figure 4-11. Installing the “quick-change” burner mount assembly. ................... 4-23
Figure 4-12. Plugging in the main interlock connector. ...................................... 4-24
Figure 4-13. Installing the burner drain system................................................... 4-25
Figure 4-14. Connecting the drain tubing and drain interlock cable.................... 4-26
Figure 4-15. Installing the burner door. .............................................................. 4-28
Figure 4-16. Installing the lamp compartment cover........................................... 4-29
Figure 4-17. Installing the sample trays onto the front of the AAnalyst............... 4-30
Figure 4-18. Location of the lamp compartment. ................................................ 4-32
Figure 4-19. Installing the Lumina hollow cathode lamp (single mount)............. 4-33
Figure 4-20. Installing the Lumina HCL (turret model). ..................................... 4-34
Figure 4-21. Installing the coded Intensitron HCL (single mount). ..................... 4-35
Figure 4-22. Installing the coded Intensitron HCL (turret model). ...................... 4-36
Figure 4-23. Installing the non-coded Intensitron HCL (single mount). .............. 4-38
Figure 4-24. Installing the non-coded Intensitron HCL (turret model). ............... 4-40
Figure 4-25. Installing the coded EDL (single mount). ....................................... 4-42
Figure 4-26. Installing the coded EDL (turret model). ........................................ 4-44
Figure 4-27. Installing the non-coded EDL (single mount). ................................ 4-46
Figure 4-28. Installing the non-coded EDL (turret model). ................................. 4-48
Figure 4-29. Wiring the EDL power supply to the AAnalyst instrument. ............ 4-50
Figure 4-30. Rear view of the AAnalyst - the gas hoses. ..................................... 4-52
Figure 4-31. Air supply connections to the AAnalyst instrument. ....................... 4-53
Figure 4-32. Acetylene supply connections. ........................................................ 4-56
xiii
Figure 4-33. Nitrous oxide supply connections.................................................... 4-57
Figure 4-34. Argon supply connections (for accessories only). ............................ 4-59
Figure 4-35. Location of the power entry module and ON/OFF switch................ 4-61
Figure 4-36. Pry off the power entry module cover.............................................. 4-62
Figure 4-37. Location of the instrument fuse block and fuses. ............................ 4-63
Figure 4-38. Changing a fuse. ............................................................................ 4-64
Figure 4-39. Location and removal of the voltage selector board......................... 4-65
Figure 4-40. Orientation of the indicator pin on the voltage selector board. ........ 4-65
Figure 4-41. The AC line cord selections for the AAnalyst instrument................ 4-67
Figure 4-42. Connecting the printer to the keypad controlled AAnalyst. ............. 4-68
Figure 4-43. Locating the light beam above the burner. ...................................... 4-74
Figure 4-44. Burner adjustment knobs. ............................................................... 4-75
Figure 4-45. The gas flowmeters and control knobs. ........................................... 4-77
Figure 4-46. Adjusting the nebulizer. ................................................................. 4-80

Chapter 5 Lamps
Figure 5-1. The workings of a hollow cathode lamp (HCL)................................... 5-3
Figure 5-2. Drawing of a Lumina hollow cathode lamp. ....................................... 5-4
Figure 5-3. The Intensitron hollow cathode lamps (coded and non-coded). ........... 5-5
Figure 5-4. The adapter cables necessary to use the Intensitron HCLs.................. 5-5
Figure 5-5. An Electrodeless Discharge Lamp (EDL). ......................................... 5-6
Figure 5-6. Accessing the lamp compartment. ..................................................... 5-8
Figure 5-7. Replacing the Lumina HCL............................................................... 5-9
Figure 5-8. Replacing the Lumina HCL (turret model). ..................................... 5-10
Figure 5-9. Replacing the coded Intensitron HCL. ............................................. 5-11
Figure 5-10. Replacing the coded Intensitron HCL (turret model)....................... 5-13
Figure 5-11. Replacing the non-coded Intensitron HCL. ..................................... 5-14
Figure 5-12. Replacing the non-coded Intensitron HCL (turret model)................ 5-16
Figure 5-13. Replacing the coded electrodeless discharge lamp........................... 5-18
Figure 5-14. Replacing the coded EDL (turret model)......................................... 5-20
Figure 5-15. Replacing the non-coded electrodeless discharge lamp. .................. 5-22
Figure 5-16. Replacing the non-coded EDL (turret model).................................. 5-24
Figure 5-17. Underside view of the deuterium lamp assembly............................. 5-28
Figure 5-18. Location of the alignment screws of the deuterium lamp................. 5-30
Figure 5-19. Centering of the two lamp beams.................................................... 5-32
xiv

Chapter 6 Burner System


Figure 6-1. The burner assembly and its parts....................................................... 6-2
Figure 6-2. The major parts of the burner. ............................................................ 6-3
Figure 6-3. Block diagram of the complete burner system..................................... 6-5
Figure 6-4. Details of the Burner (Mixing) Chamber. ........................................... 6-6
Figure 6-5. The four available burner heads.......................................................... 6-8
Figure 6-6. The gas adjustment knobs on the AAnalyst 100.................................. 6-9
Figure 6-7. The burner drain system and its parts. .............................................. 6-11
Figure 6-8. Secure the burner head in place with the safety latch. ....................... 6-13
Figure 6-9. Location of the ignitor box connectors.............................................. 6-14
Figure 6-10. Things to check on the burner end cap............................................ 6-15
Figure 6-11. Nebulizer clamp securing the nebulizer flange in place................... 6-16
Figure 6-12. Plugging in the main interlock connector. ...................................... 6-17
Figure 6-13. Location of the drain interlock connector........................................ 6-18
Figure 6-14. The drain system float assembly. .................................................... 6-19

Chapter 7 Maintenance
Figure 7-1. Removing the burner door. ................................................................. 7-5
Figure 7-2. Replacing the burner door. ................................................................. 7-6
Figure 7-3. Removing the burner assembly from the instrument. .......................... 7-7
Figure 7-4. Removing the burner head from the burner chamber. ......................... 7-8
Figure 7-5. Exploded view of the burner chamber assembly................................ 7-13
Figure 7-6. Removing the burner end cap. .......................................................... 7-14
Figure 7-7. A close up of the nebulizer. .............................................................. 7-17
Figure 7-8. Removing the nebulizer from the burner end cap.............................. 7-18
Figure 7-9. Exploded view of the nebulizer......................................................... 7-19
Figure 7-10. Attaching new capillary tubing to the nebulizer Teflon tubing. ....... 7-21
Figure 7-11. The burner drain system. ................................................................ 7-23
Figure 7-12. Replacing the drain tubing. ............................................................ 7-24
Figure 7-13. The drain trap assembly. ................................................................ 7-26
Figure 7-14. Pry off the power entry module cover.............................................. 7-28
Figure 7-15. Changing a fuse. ............................................................................ 7-29
Figure 7-16. Mounting the quartz cell-holder onto the burner head..................... 7-33
Figure 7-17. Adjusting the position of the cell-holder bracket. ............................ 7-34
Figure 7-18. Installing the quartz cell onto the holder......................................... 7-35
Safety and Regulatory
Information
Introduction
This manual contains important information regarding potential hazards that may
arise during the operation of the instrument. It is essential that this information is
read and thoroughly understood by all potential users of the instrument.

Caution The instrument should be used according to the instructions provided in this
manual. If used otherwise, the protection provided by the instrument may be
impaired.

Location of Safety Information


Extensive safety information is contained in Chapter 1 of this manual(Safety
Practices). Before setting up and operating this instrument, carefully read the
safety precautions described in Chapter 1. Observe these precautions at all times.
xvi Safety and Regulatory Information

FCC Compliance (United States)


This product is classified as a digital device used exclusively as industrial,
commercial, or medical test equipment. It is exempt from the technical standards
specified in Part 15 of the FCC Rules and Regulations, based on Section
15.103(c).

Electrical Protection Compliance

Insulation
Class I as defined in IEC-1010-1.

Installation Category
This instrument is able to withstand transient over voltage according to Installation
Category II as defined in IEC 1010–1 and IEC 664.

Pollution Degree
This equipment will operate safely in environments that contain nonconductive
foreign matter up to Pollution Degree 2 in IEC 1010–1 and IEC 664.

Electrical Warnings

Read all the electrical warnings located in Chapter 1,Safety Practices in this
manual. They are located in the section calledGeneral Safety Practices -
Electrical Safety.
Safety and Regulatory Information xvii

Symbols Used on the Instrument

The three different types of warning symbols that appear on the AAnalyst
instrument are reprinted below:

This symbol indicates an operation (or condition on the


instrument) that could causepersonal injury if precautions
are not followed. This can be any type of hazard.
When you see this symbol, refer to the safety pages or pertinent
information in the manual for further information.
Consulter les documents d’accompagnement.

This symbol indicates the danger of electric shock, if precautions


are not followed, due to the presence of high voltage.
AVERTISSEMENT: Risque d'électrocution.

This symbol indicates the danger of burns, if precautions are not


followed, due to the presence of heat in this area or the
instrument. There may also be hot surfaces that can be easily
touched.
AVERTISSEMENT: Surface chaude.

The following graphic symbols are also found on the instrument:

Indicates the OFF position of the main power switch.

Indicates the ON position of the main power switch.

Alternating current.

This protective grounding terminal must be connected to earth


ground before any other electrical connections are made to the
instrument.
xviii Safety and Regulatory Information

Warnings and Labels on the Instrument

The labels shown below appear on the right side of the instrument.

E
Warning
Grounding circuit continuity is vital
for safe operation of equipment.
Neveroperateequipmentwith
g r o u n d i n gc o n d u c t o rd i s c o n n e c t e d .

Warning
Toavoidelectricalshock,disconnect
power supply before changing fuse.
Disconnnect supply whenever cover
i sr e m o v e d .
D
Caution
For protection against fire hazard,
replace only with same type and
rating of fuse.

A B C1
C
F1 F1/F2
Warning 100 VAC 50/60 Hz 220 VAC 50/60 Hz
For protection against fire hazard, 120 VAC 50/60 Hz 230/240 VAC 50/60 Hz
replace only with same type and 6.25 AMP SLOW BLOW 3.15 AMP TT
rating of fuse. 250 V 250 V
MAX POWER 248 VA

Caution
Do not restrict air intake or exhaust

A C1
WARNING: For protection against fire CAUTION: This unit contains protective circuitry.
hazard, replace only with same type Contact Perkin-Elmer qualified service
and rating of fuse. personnel before performing any AC line tests.
AVERTISSEMENT: Pour éviter tout risque ATTENTION: Cet appareil contient un circuit
d'incendie, ne remplacez les fusibles que par protecteur. Contactez le personnel qualifi é de
d'autres du même type et de la même Perkin-Elmer avant d'effectuer un quelconque
puissance. contrôle de circuit en courant alternatif.

B D
WARNING: To avoid electrical shock, disconnect
F1 F1/F2 power supply before changing fuse.
Disconnect supply whenever cover is removed.
100 VAC 50/60 Hz 220 VAC 50/60 Hz
120 VAC 50/60 Hz 230/240 VAC 50/60 Hz AVERTISSEMENT: Afin d’éviter les risques
6.25 AMP SLOW BLOW 3.15 AMP TT
d’électrocution, mettez l'appareil hors tension
250 V 250 V
avant de changer le fusible. Mettez l'appareil hors
MAX POWER 248 VA tension chaque fois que vous retirez le couvercle.

C E
CAUTION: Do not restrict air intake or WARNING: Grounding circuit continuity is vital
exhaust. for safe operation of equipment. Never operate
equipment with grounding conductor
ATTENTION: N 'obstruez pas l 'arriv ée ou disconnected.
l 'é vacuation d ' air.
AVERTISSEMENT: La continuité du circuit de
mise à la terre est essentielle pour le bon
fonctionnement de l'appareil. N'utilisez jamais
l'appareil lorsque le câble de mise à la terre est
débranché.

Figure A. Labels located on the right side of the AAnalyst.


Safety and Regulatory Information xix

The labels shown below appear on the back of the instrument and are
detailed in Figure B.

F Warning
To reduce the chance of electrical shock
do not remove covers that require
tool access.
Nouserserviceablepartsareinside.
Refer servicing to Perkin-Elmer qualified
service personnel.

Norwalk, CT 06859 USA

G
AAnalyst 100

Part No.

Serial No.

Patents pending

Serial Number

J
F
WARNING: To reduce the chance of electrical shock,
do not remove covers that require tool access.
No user serviceable parts are inside. Refer servicing
to Perkin-Elmer qualified service personnel.

AVERTISSEMENT: Pour réduire les risques


d’électrocution, ne retirez pas les couvercles don’t
l'ouverture nécessite des outils. Il n'y a aucune pièce
réparable par l'utilisateur à l'intérieur. Contactez le
personnel qualifié de Perkin-Elmer.

G J
Serial Number
Norwalk, CT 06859 USA
AAnalyst 100

Part No.

Serial No.

Patents pending

Figure B. Labels located on the back of the AAnalyst.


xx Safety and Regulatory Information

The labels shown below appear at the end of the hoses at the back of the
instrument.

Figure C. Labels located at the end of the hoses at the back of the AAnalyst.

The translations of the word “Air” that appears on the gas label are provided in the
following table.

Language Air Language Air

German Luft Dutch Lucht

French Air Norwegian Luft

Danish Luft Portuguese Ar

Finnish Ilma Spanish Aire

Greek ΑΕΡΑΣ Swedish Luft

Italian Aria
Safety and Regulatory Information xxi

The warning labels shown below appear when you lift the top cover of an
instrument that has the deuterium arc background corrector lamp. The labels are
affixed to the cover plate of the Deuterium Arc Background Corrector assembly.

Inside Top View


of Instrument

Sample Compartment
(Top View) K
Warning
To avoid electrical shock,
disconnect power cord before servicing

Warning
Hot Lamp

Warning
UV Light Source
Wear Protective Glasses
When Working With Lid Open
L
M
K L
WARNING: To avoid electrical shock,
disconnect power cord before servicing. WARNING: Hot Lamp
AVERTISSEMENT: La Lampe est chaude.
AVERTISSEMENT: Afin d'eviter tout
risque d'electrocution, débranchez le
cordon d'alimentation avant d'effectuer
toute réparation.
M
WARNING: UV Light Source. Wear protective
glasses when working with lid open.

AVERTISSEMENT: Cet appareil émet des rayons


ultraviolets. Portez des lunettes de protection
lorsque vous ouvrez le couvercle.

NOTE: These labels appear only on instruments that have the deuterium arc lamp.

Figure D. Warning labels located inside the top of an instrument with the
Deuterium Arc Background Corrector option.
xxii Safety and Regulatory Information

Customer Service

Company Name and Address:

The Perkin-Elmer Corporation


761 Main Avenue
Norwalk, Connecticut 06859-0010 U.S.A.
Tel: (800) 762-4000 or (203) 762-4000. Fax: (203) 762-4222

Bodenseewerk Perkin-Elmer GmbH


Postfach 10 17 61, D-88647
Überlingen, Germany
Tel: (07551) 810. Fax: (07551) 1612

SUPPLIES, ACCESSORIES, AND REPLACEMENT PARTS can be ordered


directly from Perkin-Elmer using the eight digit part numbers provided in this
manual. Perkin-Elmer offers a full selection of high-quality atomic spectroscopy
supplies through the Atomic Spectroscopy Supplies Catalog. For further
information, please contact your local Perkin Elmer representative.

To place an order, request a free catalog, or ask for information, call your local
Perkin-Elmer representative.
Introduction
What is Atomic Absorption? .................................................................................xxv
What is Flame AA? ..............................................................................................xxvi
What is Graphite Furnace AA? ...........................................................................xxvi
The AAnalyst Series Instruments........................................................................xxvii
Manuals and Documents ................................................................................... xxviii
What’s in this Hardware Guide? ..........................................................................xxx
Using this Manual..................................................................................................xxx
Manual Conventions ......................................................................................... xxxi
Using the Index................................................................................................. xxxi
A Word on Troubleshooting .............................................................................. xxxi
Introduction
What is Atomic Absorption?
Atomic absorption (AA) is the process that occurs when a ground state atom
absorbs energy in the form of light of a specific wavelength and is elevated to an
excited state. The amount of light energy absorbed at this wavelength will increase
as the number of atoms of the selected element in the light path increases. The
relationship between the amount of light absorbed and the concentration of analyte
present in known standards can be used to determine unknown concentrations by
measuring the amount of light the unknown concentrations absorb. Instrument
readouts can be calibrated to display concentrations directly.

The basic instrumentation for atomic absorption requires a primary light source, an
atom source, a monochromator to isolate the specific wavelength of light to be
used, a detector to measure the light accurately, electronics to treat the signal, and a
data display or logging device to show the results (see figure). The light source
normally used is either a hollow cathode lamp or an electrodeless discharge lamp.

Figure D. Simplified drawing of a basic flame atomic absorption system.


xxvi Introduction

What is Flame AA?


The atom source used in the system just described must produce free analyte atoms
from the sample. The source of energy for free atom production is heat, most
commonly in the form of an air-acetylene or nitrous oxide-acetylene flame. The
sample is introduced as an aerosol into the flame (via a burner and nebulizer). This
system is referred to as flame sampling or flame AA. The flame burner head is
aligned so that the light beam passes through the flame, where the light is absorbed.

What is Graphite Furnace AA?


The major limitation of atomic absorption using flame sampling (flame AA) is that
the burner-nebulizer system is a relatively inefficient sampling device. Only a small
fraction of the sample reaches the flame, and the atomized sample passes quickly
through the light path. An improved sampling device would atomize the entire
sample and retain the atomized sample in the light path for an extended period to
enhance the sensitivity of the technique. Electrothermal vaporization using a
graphite furnace provides those features.

With graphite furnace atomic absorption (GFAA), the flame is replaced by an


electrically heated graphite tube. The sample is introduced directly into the tube
and the sample is then heated in a programmed series of steps to remove the solvent
and major matrix components. The remaining sample is atomized. All of the
analyte is atomized, and the atoms are retained within the tube for an extended
period. With this method, atoms are retained in the light path, which passes through
the tube. As a result, sensitivity and detection limits are significantly improved.

Graphite furnace analysis times are longer than those for flame sampling, and
fewer elements can be determined using GFAA. However, the enhanced sensitivity
of GFAA and the ability of GFAA to analyze very small samples and directly
analyze certain types of solid samples significantly expand the capabilities of
atomic absorption.
The AAnalyst Series Instruments xxvii

The AAnalyst Series Instruments


The AAnalyst series includes two basic instruments. The basic AAnalyst 100
works as a flame AA instrument, but can be upgraded to work with a graphite
furnace. The basic AAnalyst 300 works as both a flame and graphite furnace
instrument.

Figure E. The basic AAnalyst 100 instrument.

Figure F. The basic AAnalyst 300 instrument.


xxviii Introduction

Manuals and Documents


The following table lists the documentation available for the AAnalyst instruments.
Should you need to order any of these documents, contact your local Perkin-Elmer
sales or service office.

Table 1. Documentation related to the AAnalyst instruments.


Part
Numbers Document Titles
0993-6088 AAnalyst 100 and AAnalyst 300 Atomic Absorption
Spectrometer - Hardware Guide (this manual)
0993-6149 AAnalyst 100 Atomic Absorption Spectrometer -User’s Guide
0993- 6175 AAnalyst 100 Atomic Absorption Spectrometer -Installation
Guide
0993-6190 AA WinLab Software Guide
(used with AAnalyst 300 Instrument)
0993-6178 AA WinLab Software Installation Instructions

(continued on the next page . . . )


Manuals and Documents xxix

In addition, if your system is configured with a computer system (EDS), a


tutorial manual appropriate to your specific configuration is also provided.
For hardware information on accessories such as the graphite furnace,
autosampler, mercury/hydride system, or FIAS system, refer to the manuals
provided with each accessory. They are listed below:
Table 2. Accessory manuals.

Part No.’s Document Titles

0993-5242 HGA 800 Graphite Furnace System: Hardware Guide (includes


Graphite Furnace Autosampler info.)

(see above) Graphite Furnace Autosampler Manual


(see manual number 0993-5242 above)

B050-3858 AS-90 Autosampler for Atomic Spectroscopy -


Installation, Maintenance and System Description Manual

B050-9569 AS-91 Autosampler for Atomic Spectroscopy -


Installation, Maintenance and System Description Manual

B009-8670 MHS-10 Operator's Manual

x FIAS-100/400 Manual (P/N unknown at time of print)

Table 3. Additional helpful documents.

Part No.’s Document Titles

L-301 Preparing Your Lab for Perkin-Elmer Atomic Absorption

0303-0152 Analytical Methods for Atomic Absorption Spectrometry (the


“AA Cookbook”)

L-655F The Guide to Techniques and Applications


of Atomic Spectroscopy

PEX-A8 Atomic Spectroscopy Supplies Catalog


xxx Introduction

What’
s in this Hardware Guide?
This manual (0993-6088) is your hardware guide to both the AAnalyst 100 and the
AAnalyst 300 instruments. Topics include:
• safety practices
• system descriptions
• preparing your laboratory
• installation
• lamps
• burner system
• maintenance
• troubleshooting

Using this Manual

Caution The instrument should be used according to the instructions provided in this
manual. If used otherwise, the protection provided by the instrument may be
impaired.

We recommend the following approach to using the AAnalyst 100/300 Atomic


Absorption Spectrometer Hardware Guide:

1. Thoroughly read Chapter 1, Safety Practices, before using the instrument.


Consult the appropriate reference materials listed at the end of that chapter.
In addition, read the safety information in the manuals for your accessories.

2. Read Chapter 2, System Descriptions, to familiarize yourself with the functions


of the hardware components included with your system.

3. Read Chapter 3, Preparing Your Laboratory, if you have any questions


regarding the preparation of your laboratory (for example, the installation of
a venting system or of the various gas supplies).

4. The remaining chapters contain information on installation, maintenance and


troubleshooting for the AAnalyst system.
Using this Manual xxxi

Manual Conventions

In this manual, the following special formats are used to set apart important
information, warnings and notes:

A warning indicates an operation that could cause personal injury if


precautions are not followed.

Caution A caution indicates an operation that could cause instrument damage if


precautions are not followed.

NOTE: Statements designated as a NOTE emphasize


significant information in a procedure or description.

Using the Index

Use the index to look up information on the hardware components. If you need to
find information on cleaning the burner head, for example, look up "burner head" in
the index. Also, use the index to look up information on the following topics:
• installation
• maintenance
• troubleshooting
• part numbers

A Word on Troubleshooting

We recommend that you consult the troubleshooting information included in this


manual before you call Perkin-Elmer for service. The troubleshooting section
contains suggestions to help you determine systematically whether instrument
problems are due to improper analytical techniques, improper selection of
instrument parameters, or malfunction of the instrument.
xxxii Introduction
Safety Practices 1
Introduction to this Chapter.................................................................................. 1-1
Using This Chapter................................................................................................ 1-1
Laboratory Safety Guidelines ............................................................................... 1-2
General Safety Guidelines................................................................................... 1-2
Environmental Safety Conditions ........................................................................ 1-2
Handling the Instrument Safely ........................................................................... 1-3
Laboratory Ventilation Safety.............................................................................. 1-3
General Safety Practices ....................................................................................... 1-3
Ultraviolet Radiation Safety ................................................................................ 1-3
Electrical Safety .................................................................................................. 1-4
Hazardous Chemicals Warnings .......................................................................... 1-7
Safe Handling of Gas Cylinders .......................................................................... 1-8
Identifying Cylinders ......................................................................................1-8
Storing Cylinders ............................................................................................1-9
Handling Cylinders ....................................................................................... 1-10
Safe Handling of Atomizers .............................................................................. 1-10
Safe Use of Chemical Reagents ......................................................................... 1-11
Protective Equipment.................................................................................... 1-11
Reagent Use, Storage, and Disposal .............................................................. 1-11
Waste Disposal Procedures................................................................................ 1-12
Flame Analyses Safety Practices ......................................................................... 1-13
Safety Interlocks ............................................................................................... 1-13
Burner Gases (in General)................................................................................. 1-13
Air Supply ........................................................................................................ 1-14
1-2 Safety Practices

Acetylene .......................................................................................................... 1-14


Nitrous Oxide ................................................................................................... 1-15
Safety Checks Before Ignition ........................................................................... 1-16
Burner Head ................................................................................................. 1-17
Burner Chamber and End Cap ...................................................................... 1-17
Nebulizer ...................................................................................................... 1-17
Drain System ................................................................................................ 1-17
Hazards with Flame Analyses ........................................................................... 1-18
General Precautions ...................................................................................... 1-18
Flashbacks .................................................................................................... 1-18
Ultraviolet Radiation Hazards ....................................................................... 1-19
High Temperatures ....................................................................................... 1-19
Acetone Carryover ........................................................................................ 1-19
Acetylides ..................................................................................................... 1-20
Organic Solvents........................................................................................... 1-20
Cyanide Solutions ......................................................................................... 1-20
Graphite Furnace Analyses Safety Practices...................................................... 1-21
Safety Interlocks ............................................................................................... 1-21
Inert Gas Supply ............................................................................................... 1-21
Argon ............................................................................................................... 1-21
Safety Checks.................................................................................................... 1-22
Hazards with Furnace Analyses......................................................................... 1-22
UV Radiation................................................................................................ 1-22
High Temperatures ....................................................................................... 1-23
Mercury/Hydride Analyses Safety Practices...................................................... 1-24
Inert Gas Supply ............................................................................................... 1-24
Quartz Cells...................................................................................................... 1-24
Safety Checks.................................................................................................... 1-24
Hazards with Mercury/Hydride Determination System Analyses ....................... 1-25
High Temperatures ....................................................................................... 1-25
Sodium Tetrahydroborate (Sodium Borohydride) .......................................... 1-25
Tin (II) Chloride (Stannous Chloride) ........................................................... 1-26
Hydrofluoric Acid ......................................................................................... 1-26
Magnesium Perchlorate................................................................................. 1-27
Sample Preparation Safety Practices.................................................................. 1-28
Dissolving Solid Samples in Organics ............................................................... 1-28
Dissolving Solid Samples Using Acids .............................................................. 1-29
Acid Digestions................................................................................................. 1-29
Fusion Mixtures................................................................................................ 1-31
References............................................................................................................ 1-33
Safety Practices 1
Introduction to this Chapter

This chapter describes general practices written to aid you in safely operating the
atomic absorption spectrometer and accessories.

This advice is intended to supplement, not supersede, the normal safety codes in the
country of operation. The information provided does not cover every safety
procedure that should be practiced. Ultimately, maintenance of a safe laboratory
environment is the responsibility of the user and the user's organization.

Please consult all manuals supplied with the AAnalyst instrument and any
accessories before you start working with the instrument. Carefully read all the
safety information in this and any other manuals supplied. When setting up the
instrument or performing analyses or maintenance procedures, strictly follow the
instructions provided.

Using This Chapter

This safety chapter is divided into sections that cover both general practices as well
as practices related to specific types of atomic absorption analyses.

We recommend the following approach to using this chapter:


1-2 Safety Practices

1. Read the first two sections which cover general laboratory guidelines and
safety practices for all atomic absorption analyses.

2. Read the appropriate sections listed below, according to the types of analyses
you will be performing:
l Flame Analyses Safety Practices
l Furnace Analyses Safety Practices
l Mercury/Hydride Analyses Safety Practices.

3. Read the last section, Sample Preparation Safety Practices. This section
describes general precautions related to sample preparation methods as well as
some specific chemical hazards.

In addition, consult the References listed at the end of this chapter.

Laboratory Safety Guidelines


This section describes some general laboratory safety guidelines. For additional
information, we recommend The CRC Handbook of Laboratory Safety (1) and
Prudent Practices for Handling Hazardous Chemicals in Laboratories (2).

General Safety Guidelines


For safety reasons and to avoid contaminating samples, be sure that the instrument
and work area are kept scrupulously clean. This is especially important when
working with toxic elements or when measuring trace amounts of any element.
Clean up spilled chemicals immediately and dispose of them properly.

Do not allow smoking in the work area. Smoking is a source of significant


contamination as well as a potential route for ingesting harmful chemicals.

Food should not be stored, handled, or consumed in the work area.

Environmental Safety Conditions

Do not use the instrument in an area where explosion hazards may exist. The
instrument should be used indoors in a laboratory having the environmental
conditions recommended in the Preparing Your Laboratory chapter.
General Safety Practices 1-3

Handling the Instrument Safely

Contact a Perkin-Elmer service engineer if you feel you need assistance in installing
or moving the system. If you need to move the system, do so carefully.

In general, the AAnalyst 100 instrument alone weighs 65.3 kg (144 lbs.) and the
AAnalyst 300 weighs 68 kg (150 lbs.). Be sure to use proper lifting posture when
moving or lifting the instrument out of the carton. Figure 4-2 in the Installation
Chapter (Chapter 4) shows how to lift it safely.

Depending on the specific instrument configuration and the added accessories, be


aware that the total weight on the laboratory bench may be as much as 300 kg (661
lbs.). Make sure that the bench is capable of sustaining this weight.

Laboratory Ventilation Safety

Toxic combustion products, fumes, vapors, and ozone can be generated by the
system, depending upon the type of analysis. Therefore, an efficient ventilation
system must be provided for your instrument. Specifications for a recommended
ventilation system are described in the section called Exhaust Vent Requirements in
the Preparing Your Laboratory chapter.

General Safety Practices

This section describes potential hazards with any atomic absorption analysis and
recommended safety practices.

Ultraviolet Radiation Safety

Hazardous ultraviolet radiation can be emitted by the flame (especially the nitrous
oxide-acetylene flame) the graphite furnace when it is heated to incandescence,
hollow cathode or electrodeless discharge lamps, and deuterium background
corrector lamps. Prolonged exposure to ultraviolet radiation can cause serious
damage to your eyes.
1-4 Safety Practices

To avoid any exposure to ultraviolet radiation, always wear safety glasses


when using the instrument. The safety glasses should be warranted or otherwise
certified to protect the eyes from ultraviolet radiation. Side shields will provide an
extra margin of safety as well as mechanical protection for your eyes.

Electrical Safety

The instrument has been designed to protect the operator from potential electrical
hazards. This section describes some recommended electrical safety practices.

The instrument must be correctly connected to a suitable electrical supply. The


supply must have a correctly installed protective conductor (earth/ground) and
must be installed or checked by a qualified electrician before you connect the
instrument.

Grounding circuit continuity is vital for safe operation of equipment. Never


operate equipment with grounding conductor disconnected.

Any interruption of the protective conductor (earth/ground) inside or outside the


instrument or disconnection of the protective conductor terminal is likely to make
the instrument dangerous. Intentional interruption is prohibited.

Connect the instrument to an AC line power outlet that has a protective


ground connection. To ensure satisfactory and safe operation of the instrument, it
is essential that the protective ground conductor (the green/yellow lead) of the line
power cord is connected to true electrical ground. Any interruption of the protective
ground conductor, inside or outside the instrument, or disconnection of the
protective ground terminal may impair the protection provided by the instrument.

Do not operate the instrument with any covers or parts removed. Disconnect
supply whenever cover is removed.

To reduce the chance of electrical shock, do not remove covers that require
tool access. No user serviceable parts are inside. Refer servicing to Perkin-Elmer
qualified service personnel.
General Safety Practices 1-5

To ensure safe operation, servicing of the instrument should only be performed


by a Perkin-Elmer service engineer or similarly authorized and trained person.

Do not attempt to make adjustments, replacements or repairs to this


instrument except as described in the accompanying User Documentation. Only
a Perkin-Elmer service representative or similarly trained and authorized person
should be permitted to service the instrument..

When the instrument is connected to line power, opening instrument covers is


likely to expose live parts. Lethal voltages are present at certain areas in the
instrument. Even when the power switch is off, high voltages can still be present.
Capacitors inside the instrument may still be charged even if the instrument has
been disconnected from line power.

To avoid electrical shock, disconnect power supply before changing fuse.


Disconnect supply whenever cover is removed

Use only fuses with the required current rating and of the specified type for
replacement.

(continued on next page)


1-6 Safety Practices

When working with the instrument, observe the following:


l Connect the instrument to a correctly installed line power outlet that has a
protective conductor connection (earth/ground).
l Do not operate the instrument with any covers or internal parts removed.
l Do not attempt to make internal adjustments or replacements except as
directed in the manuals.
l Disconnect the instrument from all voltage sources before opening it for
any adjustment, replacement, maintenance, or repair. If afterwards, the
opened instrument must be operated for further adjustment, maintenance,
or repair, this must only be done by a qualified person who is aware of the
hazard involved.
l Use only fuses having the specified current rating and type for
replacement. Do not use makeshift fuses or short circuit the fuse holders.
l Whenever it is possible that the instrument is no longer electrically safe for
use, make the instrument inoperative and secure it against any
unauthorized or unintentional operation. The electrical safety of the
instrument is likely to be impaired if, for example, the instrument shows
visible damage, fails to perform the intended measurement, has been
subjected to prolonged storage under unfavorable conditions, or has been
subjected to severe stress during transportation.
General Safety Practices 1-7

Hazardous Chemicals Warnings

Before using any chemicals or solvents with the instrument, you should be
thoroughly familiar with all hazards and safe handling practices. Observe the
manufacturer’s recommendations for use, storage and disposal. These
recommendations are normally provided in the material safety data sheets (MSDS)
supplied with the solvents

Some chemicals used with this instrument may be hazardous or may become
hazardous after completion of an analysis. The responsible body (e.g., Lab
Manager) must take the necessary precautions to ensure that the surrounding
workplace and that the instrument operators are not exposed to hazardous levels of
toxic substances (chemical or biological) as defined in the applicable Material
Safety Data Sheets (MSDS) or OSHA, ACGIH, or COSHH documents. Venting
for fumes and disposal of waste must be in accordance with all national, state and
local health and safety regulations and laws.

Some definitions of terms used in the “Hazardous Chemicals Warning” above are
given next.

Responsible body: “Individual or group responsible for the use and maintenance
of equipment, and for ensuring that operators are adequately trained.”
[per IEC 1010-1, Amendment 2].

Operator: “Person operating equipment for its intended purpose.” [per IEC
1010-1, Amendment 2].

OSHA: Occupational Safety and Health Administration (United States)

ACGIH: American Conference of Governmental Industrial Hygienists

COSHH: Control of Substances Hazardous to Health (United Kingdom)


1-8 Safety Practices

Safe Handling of Gas Cylinders

NOTE: The permanent installation of gas supplies is the


responsibility of the user and should conform to local
safety and building codes.

Listed in this section are some general safety practices for the proper identification,
storage, and handling of gas cylinders. Consult References 3, 4, and 5 at the end of
this chapter for more detailed information and additional guidelines. Also, refer to
the information on specific gases in subsequent sections of this chapter.

Hazards associated with the different gases used in atomic absorption spectroscopy
are described in the Table 1-1.

Table 1-1. Summary of gas hazards.


Spontaneous
Decomposition
Gas Suffocation Explosion or Combustion

Air – – –

Argon 4 – –

Nitrogen 4 – –

Acetylene 4 4 4

Nitrous Oxide 4 – 4

Contact the gas supplier for a safety data sheet containing detailed information
on the potential hazards associated with the gas.

Carefully use, store, and handle compressed gases in cylinders. Gas cylinders can
be hazardous if they are mishandled.

Identifying Cylinders

• Legibly mark cylinders to clearly identify the contents and status (full, empty,
etc.). Use the chemical name or commercially accepted name for the gas.
General Safety Practices 1-9

Storing Cylinders

• Store cylinders in accordance with the regulations and standards applicable to


your locality, state, and country.

• When gas cylinders are stored in confined areas, such as a storage room,
ventilation should be adequate to prevent toxic or explosive accumulations.
The storage room should be well ventilated and dry. This is particularly
important in small or confined areas.

• Do not store cylinders near elevators, gangways, or in locations where heavy


moving objects may strike or fall against them.

• Use and store cylinders away from exits and exit routes.

• Locate gas cylinders away from heat sources, including heat lamps.
Compressed gas cylinders should not be subjected to temperatures above 52 °C
(125 °F).

• Do not allow ignition sources in the storage area and keep cylinders away from
readily ignitable substances such as gasoline or waste, or combustibles in bulk,
including oil.

• Store all gas cylinders only in a vertical position, with the valve cap in place,
and fastened securely to an immovable bulkhead or a permanent wall.

• If you are storing cylinders outdoors, store them above ground on a suitable
floor where they are protected against temperature extremes (including the
direct rays of the sun).
1-10 Safety Practices

Handling Cylinders

• Move cylinders with a suitable hand truck after insuring that the valve cap is
securely in place and the cylinder properly fastened to the hand truck.

• Use only approved regulators, tubing, and hose connectors. When connecting
fittings, keep in mind that left-hand thread fittings are used for fuel gas tank
connections (e.g., acetylene), whereas right-hand fittings are used for oxidant
and support gas connections (e.g., nitrous oxide, air).

• Arrange gas hoses where they will not be damaged or stepped on and where
things will not be dropped on them.

• Do not "crack the valve" or open the valve of an acetylene cylinder before
attaching a regulator.

• Do not attempt to refill gas cylinders.

• Check the condition of pipes, hoses, and connectors regularly. Perform periodic
gas leak tests at all joints and seals of the gas system regularly by applying an
approved gas leak detection solution.

• When the equipment is turned off for the day, close all gas cylinder valves
tightly at the tank. Bleed the remainder of the line to the atmosphere before
turning the exhaust vent off.

Safe Handling of Atomizers

Atomizers (e.g., burner head, graphite furnace, quartz cell) become very hot during
use and can present a potential hazard to the user.

To avoid serious burns, be sure the burner head, graphite furnace, quartz cell,
or heating mantle has cooled to room temperature before you touch it.
General Safety Practices 1-11

Safe Use of Chemical Reagents

In this section, we have provided some general safety practices that you should
observe when working with any chemicals. In addition, information on specific
chemicals used in mercury/hydride analyses and in sample preparation is covered in
other sections of this chapter.

Give careful attention to the hazards associated with the chemical reagents you
are using, referring to the safety data sheets provided by the manufacturer,
for example, Material Safety Data Sheets (MSDS) in the USA). See Reference
6.

Protective Equipment

• Wear appropriate eye protection at all times while handling chemicals. Use
safety glasses with side shields, goggles, or full-face shields, depending on the
types of chemicals you will be handling.

• Wear suitable protective clothing, including gloves specifically resistant to the


chemicals being handled.

Reagent Use, Storage, and Disposal

• Use, store, and dispose of chemicals in accordance with the manufacturer's


recommendations and regulations applicable to the locality, state, and/or
country.

• When preparing chemical solutions, always work in a fume hood that is


suitable for the chemicals you are using.

• Conduct sample preparation away from the instrument to minimize corrosion


and contamination.

• Clean up spills immediately using the appropriate equipment and supplies such
as spill cleanup kits.

• Do not put open containers of solvent near the instrument.


1-12 Safety Practices

• Store solvents in an approved cabinet (with the appropriate ventilation, as


required) away from the instrument.

Waste Disposal Procedures

In flame, mercury/hydride and flow injection analyses, drain vessel contents must
be disposed of properly. Primary source lamps (hollow cathode and electrodeless
discharge lamps) used for all types of analyses must be disposed of properly.

Dispose of waste in accordance with the regulations applicable to your locality,


state, and/or country.

Drain Vessel Contents

• Carefully monitor the collection of effluent in the drain vessel and empty the
drain vessel frequently.

• When switching between organic and aqueous solutions, flush the drain tube
thoroughly and empty and flush out the drain vessel.

• Drain vessels may contain flammable, acidic, caustic, or organic solutions, and
small amounts of the elements analyzed. The collected effluent may have to be
disposed of as hazardous waste. Refer to applicable regulations for proper
disposal practices.

Primary Source Lamps (Lamps)

• Hollow cathode lamps and electrodeless discharge lamps contain small


quantities of the element listed on the label. When you dispose of lamps
containing toxic elements, you must regard them as hazardous waste.

• Hollow cathode lamps are maintained under reduced pressure. Handle and
dispose of them correctly to minimize the implosion risk.
Flame Analyses Safety Practices 1-13

Flame Analyses Safety Practices

This section describes safety practices for the burner gases, provides a list of safety
checks for the burner system, and identifies potential hazards in running flame
analyses.

Safety Interlocks

The burner system has safety interlocks which monitor gas pressure and check for
the proper setup of the burner head, nebulizer and drain system. In addition, a
flame sensor checks for the presence of the flame and a sensor monitors the
temperature of the sample compartment. All interlocks must be satisfied before you
can operate the system.

Do not attempt to defeat the safety interlocks. This would compromise


operator or equipment safety and could cause a serious explosion.

Burner Gases (in General)

Hazards and safety practices for acetylene, nitrous oxide, and air are described
next. In addition to this information, the Preparing Your Laboratory chapter in this
manual discusses the gas supply requirements and specifications for each gas. The
Installation chapter has information on connecting the gas supplies.

To avoid explosion hazards, carefully maintain the gas supplies as follows:


Regularly check the condition of pipes, hoses, and connectors in the gas lines.
Apply an approved leak test solution to all joints and seals. A leak in a gas line,
connection, or gas control system can result in a serious explosion or fire.
Before you turn off the equipment for the day, close all gas cylinder and
regulator valves tightly at the tank. Bleed the remainder of the line to the
atmosphere before turning off the exhaust system.
Do not attempt to service the gas control system yourself. Contact a Perkin-
Elmer service engineer.
1-14 Safety Practices

Air Supply

An air compressor is recommended for the burner system. Cylinders of compressed


air should only be used as an emergency or short-term solution.

Never use oxygen as the oxidant gas. Use of oxygen will result in a serious
explosion.

If using compressed air in cylinders, be sure that the oxygen content is less
than 20%.

Acetylene

This section describes recommended safety practices for acetylene. References 7, 8,


and 9 describe the physical properties of acetylene, its toxicity, and the hazardous
reactions associated with this gas.

Contact the gas supplier for a safety data sheet containing detailed information
on the potential hazards associated with acetylene. Use safe handling and
storage procedures. Do not use acetylene that is dissolved in a solvent other than
acetone.

Acetylene is supplied dissolved in acetone to prevent explosive decomposition.


You should not use acetylene that is dissolved in any other solvent. Experience
indicates that these other solvents can be carried through the regulator with the
acetylene and can weaken, to the point of rupture, the walls of the tubing that
carries the acetylene to the burner, causing a hazardous situation.

Piping, Tubing, and Fittings: Use galvanized iron, steel, or wrought iron tubing.

Acetylene may react with copper to form a readily explosive compound. Never
use copper tubing or fittings for acetylene gas lines.

Joints may be welded or made up of threaded or flanged fittings, typically stainless


steel or aluminum, or brass composed of less than 65% copper. Rolled, forged, or
cast steel or malleable iron fittings may also be used. Cast iron fittings can not be
used safely for acetylene lines. For more information, see Reference 4.
Flame Analyses Safety Practices 1-15

Storage and Handling: Follow the General Safety Practices given earlier
in this chapter for the Safe Handling of Gas Cylinders discussed there. In addition:
Store acetylene cylinders in a safe location preferably outside of the lab.
Do not store acetylene cylinders in close proximity to oxygen or oxidizing
gases, including nitrous oxide.
Always store and use acetylene cylinders in a vertical position to prevent
acetone from blocking the cylinder outlet and gauge.
Use an outlet gauge pressure of 85 to 100 kPa (12-14 psig) for acetylene.
Never allow the outlet gauge pressure of the acetylene cylinder to exceed
103 kPa (15 psig). At higher pressures, acetylene can decompose with
explosive force.
Change the acetylene cylinder before the cylinder pressure drops below
600 kPa (85 psig). Failure to do so may cause damage to valves or tubing
within the burner gas control system due to acetone contamination. Such
damage can lead to a serious explosion.
Attach a regulator and proper flow restrictor. Do not attempt to clear the
cylinder valve by opening it slightly before attaching the regulator. This
practice, referred to as "cracking" the valve, should be avoided.

Consult References 3 and 4 for more detailed information and additional


recommended practices.

Nitrous Oxide

This section describes recommended safety practices for nitrous oxide. References
7 through 9 describe the physical properties of nitrous oxide, its toxicity, and the
hazardous reactions associated with this gas.

Contact the gas supplier for a safety data sheet containing detailed information
on the potential hazards associated with nitrous oxide. Use safe handling and
storage procedures.

Piping, Tubing, and Fittings: Consult Reference 5 for nitrous oxide piping,
tubing, and fittings requirements.
1-16 Safety Practices

Make sure tubing and fittings carrying nitrous oxide are free of grease, oil, or
other organic material. Spontaneous combustion may occur if nitrous oxide
comes into contact with these materials.

Storage and Handling: Follow the General Safety Practices given earlier in this
chapter for the Safe Handling of Gas Cylinders discussed there. In addition:
Store nitrous oxide cylinders in a well-ventilated area preferably outside the
laboratory. Nitrous oxide is an asphyxiant; it is a potential hazard when stored
or used in a confined space. In addition, nitrous oxide enriched atmospheres
may collect temporarily in confined areas in the event of a gas leakage. In
nitrous oxide enriched atmospheres, ignition of combustible materials may
occur more readily, with combustion proceeding at a faster rate.
Do not store nitrous oxide cylinders in close proximity to flammable gases
(e.g., acetylene).
Use a heated regulator for nitrous oxide. This will prevent freezing of the
diaphragm, which causes a lack of pressure regulation and can lead to erratic
flame conditions, or in the most extreme cases, a flashback.

Consult References 3 and 5 for more detailed information and additional


recommended practices.

Safety Checks Before Ignition

Before igniting the flame, perform the following general safety checks:
The vent is on and drawing properly.
The burner door is closed.
There is sufficient gas in the cylinders for your intended analyses.
A fire extinguisher is located near the instrument.

Use the safety checks that follow to make sure that all components are
properly installed and in good condition for safe operation. Inadequate
inspection or maintenance of the burner system can cause the escape of fuel gas or
the fuel gas mixture, which can cause a serious explosion or fire.
Flame Analyses Safety Practices 1-17

Burner Head

Be sure that:
The burner head o-ring is in good condition. The o-ring is easily frayed when
burner heads are interchanged and should be replaced when worn.
The proper burner head has been selected based on your flame and sample
conditions. The five-centimeter N2O/C2H2 burner head is required for a
nitrous oxide-acetylene flame.
The burner head slot is clean.
The burner head is fully seated into the burner mixing chamber.

Burner Chamber and End Cap

Be sure that:
The standard end cap gasket (for aqueous solutions) or an organic-resistant
gasket is properly seated and in good condition.
The end cap is securely tightened.
The fuel and auxiliary oxidant tubing connected to the burner is in good
condition and the fittings have been properly tightened.

Nebulizer

Be sure that:
The nebulizer o-rings that seal to the end cap are in good condition.
The proper nebulizer has been selected based on the type of solutions that will
be aspirated.
The nebulizer is securely clamped in place.
The nebulizer tubing is in good condition and the connection is tight.
The nebulizer tubing is connected to the nebulizer side arm.
The nebulizer interlock is intact.

Drain System

Be sure that:
The drain system has been properly installed.
1-18 Safety Practices

The drain tubing is securely connected to the front of the burner and in good
condition (i.e., it does not show signs of cracking or discoloration). The drain
tubing should be checked regularly, especially if using organic solvents.
Any waste collected in the drain vessel has been properly disposed of and the
vessel and drain loop refilled as specified for your system.

Be sure to check the Installation chapter for more detailed information regarding
the proper drain setup and the Maintenance chapter for maintenance procedures.

Hazards with Flame Analyses

Potential hazards for both general flame analyses and for analyses with special
sample types are described below.

General Precautions
Never leave the flame unattended.
Do not adjust the nebulizer when using a nitrous oxide-acetylene flame. This
can cause erratic flame conditions or a flashback.
Keep open containers of flammable liquids and solvents away from the flame.

Flashbacks

The seepage of fuel or a fuel gas mixture from the burner chamber may cause a fire
or a flashback. A flashback is an explosion of the premixed gases in the burner
chamber.

It is essential to carefully follow proper procedures and regularly inspect and


maintain the burner system to avoid flashbacks.

Should a flashback ever occur:


Thoroughly check the burner and drain system. Refer to Chapter 6 - Burner
System for the Burner Pre-Ignition Checklist. Replace damaged parts.
Refer to the Troubleshooting chapter. See the table listing possible causes of
flashback. Do not reignite the flame until the problem has been corrected.

Contact a Perkin-Elmer service engineer if you need any assistance.


Flame Analyses Safety Practices 1-19

Ultraviolet Radiation Hazards

The flame, especially the nitrous oxide flame, emits ultraviolet radiation.

Keep the flame door closed while the flame is lit and never directly view the
flame without wearing UV-absorbing safety glasses. Safety glasses with side
shields will provide extra protection.

High Temperatures

The burner head becomes very hot during use. Flame temperature is over 2000 °C
(3600 °F).

To avoid serious burns, let the burner head cool to room temperature before
you touch it.

Acetone Carryover

Acetylene is dissolved in acetone. As the cylinder pressure falls, the concentration


of acetone in the gas stream rises, increasing the possibility of acetone carryover
which can damage valves or tubing within the gas control system. Such damage
can lead to a serious explosion. Acetone carryover may also result if tanks are
overfilled, improperly filled, or stored on their sides.

To avoid acetone carryover and explosion hazards, replace acetylene cylinders


when the cylinder pressure falls below 600 kPa (85 psig).
1-20 Safety Practices

Acetylides

When high concentrations of mercury, copper, or silver are aspirated into the
air-acetylene flame, unstable acetylide compounds may form in the burner
chamber. When permitted to dry, these compounds are likely to explode.

To avoid explosion hazards when aspirating high concentrations of mercury,


copper, or silver (acetylides):

Aspirate solution continuously during the analysis to prevent any residues


from drying.

Thoroughly flush the burner mixing chamber and drain system with water
immediately after the analysis. Visually inspect the chamber to be sure
that all traces of residue have been removed.

Organic Solvents

Some safety precautions for organic solvents are described below.

Take suitable precautions when using volatile organic solvents. A potentially


flammable organic vapor "cloud" can form around the opening of the sample
container. Feeding the capillary tubing through a small hole in a covered sample
container is one way of reducing the possibility for ignition.

While running organic solvents, frequently empty the drain vessel.


After aspirating organic solvents, clean the burner mixing chamber and
thoroughly flush the drain tube with water and empty the drain vessel. For
instructions to do this, see the Maintenance chapter. (Always dispose of
hazardous or corrosive solutions properly.)

Cyanide Solutions

Read the following warning when using cyanide solutions:

When using cyanide solutions, check the pH of the liquid trap and drain vessel.
The liquid must always be alkaline (pH greater than 10) to prevent highly toxic
hydrogen cyanide gas from forming.
Graphite Furnace Analyses Safety Practices 1-21

Graphite Furnace Analyses Safety Practices

Safety Interlocks

The interlocks check that the furnace is properly cooled, monitor argon pressure,
and monitor the temperature of the power supplies. All interlocks must be satisfied
before you can operate the system.

Do not attempt to defeat the safety interlocks as this would compromise


operator or equipment safety.

Inert Gas Supply

The graphite furnace requires a supply of inert gas for flushing the graphite tube.
Perkin-Elmer recommends argon for the inert gas.

Nitrogen is not recommended for the inert gas supply. At furnace temperatures
above 2300 °C (4170°F), nitrogen combines with carbon to produce toxic
cyanogen gas (C 2N2).

Argon

As just mentioned, the graphite furnace requires a supply of inert gas for flushing
the graphite tube. Perkin-Elmer recommends argon for the inert gas. This section
describes recommended safety practices for argon. References 7 through 9 describe
the physical properties of argon, its toxicity, and the hazardous reactions associated
with this gas.

Contact the gas supplier for a safety data sheet containing detailed information
on the potential hazards associated with argon. Use safe handling and storage
procedures.

The major hazard associated with argon is suffocation. This can occur if the gas is
allowed to escape in an enclosed area and displaces the oxygen in air. Argon is
neither explosive nor combustible.
1-22 Safety Practices

If liquid argon is used, the gas cylinder must be fitted with an over-pressure
regulator. The over-pressure regulator will vent the cylinder as necessary to keep
the argon cool enough to remain in its liquid state, thus preventing the cylinder
from exploding due to pressure build-up.

Gaseous argon tanks do not require venting and consequently can be stored for
extended periods without loss.

Storage and Handling: Follow the General Safety Practices given earlier in this
chapter for the Safe Handling of Gas Cylinders.

Consult Reference 3 for more detailed information and additional recommended


practices.

Safety Checks

Before starting the analysis, check the following:


The vent is on and drawing properly.
If a fume extraction unit device is used for your furnace, be sure it is in place.
The inert gas supply is connected and set to the correct pressure.
The water cooling hoses are connected and the cooling system is turned on.
The autosampler drain bottle is empty.

Hazards with Furnace Analyses

The following additional potential hazards are associated with furnace analyses.

UV Radiation

The graphite furnace, when it is heated to incandescence, can generate ultraviolet


radiation.

Never directly view the furnace during the atomization step without wearing
UV-absorbing safety glasses. Safety glasses with side shields will provide extra
protection.
Graphite Furnace Analyses Safety Practices 1-23

High Temperatures

Graphite furnaces can generate temperatures of up to 3000 °C (5432 °F).

Let the graphite furnace and tube cool to room temperature before you
touch it.

Do not attempt to inject a sample into the graphite tube while the furnace is
very hot (i.e., significantly higher than the boiling temperature of the solvent).
You may be subjected to fumes from the sudden vaporization of the sample, you
may damage the pipette, and you may be burned.
1-24 Safety Practices

Mercury/Hydride Analyses Safety Practices

This section covers mercury/hydride analyses performed with the MHS-10 or with
Flow Injection (FIAS).

Inert Gas Supply

Either argon or nitrogen may be used as the inert gas. Follow the General Safety
Practices given earlier in this chapter for the Safe Handling of Gas Cylinders.

Quartz Cells

The FIAS accessories require different quartz cells.

To avoid an explosion hazard, never use the wrong size FIAS quartz cell. The
wrong diameter of the FIAS cell will cause a pressure build-up in the system. This
could force the acidic reaction mixture back into the sodium tetrahydroborate
storage container. Large quantities of hydrogen would be produced, resulting in an
explosion.

Safety Checks

Before starting the analysis, check the following:


The vent is on and drawing properly.
The exhaust hose is securely connected to the two outlets of the quartz cell and
leads to the exhaust system.
The exhaust hose and transfer tubing cannot become pinched or kinked. This
can lead to a pressure buildup in the system.
If you are using FIAS, the tubing is properly assembled, in good condition, and
all tubing connections have been finger-tightened.
The drain tubing leads to the waste container and this container is empty.
In addition, if you are using a flame to heat the quartz cell, refer to the safety
checks given previously for flame analyses.
Mercury/Hydride Analyses Safety Practices 1-25

Hazards with Mercury/Hydride Determination System Analyses

High temperatures and certain chemical hazards are associated with


mercury/hydride analyses.

High Temperatures

The quartz cell and heating mantle can be heated to temperatures up to 1000 °C
(1832 °F).

To avoid serious burns, let the heating mantle and quartz cell cool to room
temperature before you touch them.

Sodium Tetrahydroborate (Sodium Borohydride)

Sodium tetrahydroborate (NaBH4) is commonly used as a reducing agent in


mercury/hydride analyses. It is toxic, corrosive, and flammable. During the course
of mercury/hydride analyses, sodium tetrahydroborate comes into contact with the
acidic carrier solution and releases hydrogen. Hydrogen can form explosive
mixtures with air.

Before using sodium tetrahydroborate, you should be thoroughly familiar with


all hazards and safe handling practices. Observe the manufacturer's
recommendations for use, storage and disposal.
The work area must have an adequate exhaust system to prevent the build-up
of explosive hydrogen/air mixtures.
Wear goggles, protective clothing and gloves.
Protect sodium tetrahydroborate solutions from temperature variations. Keep
out of direct sunlight, away from open flames, and in an area with an efficient
ventilation system.
Prepare sodium tetrahydroborate solutions fresh daily. Do not store overnight.
Handle solutions with care since they are corrosive.
Before disposing of any remaining solution, neutralize it with a diluted acid
inside a fume hood.
1-26 Safety Practices

When using FIAS:


- Make sure that all tubing connections are tight to prevent air from entering
the system.
- Do not loosen or remove any connections while the system is running.
- Never use a concentration greater than 0.5% of sodium tetrahydroborate.
- Pump deionized water through the tubing system at the end of the day to
remove all traces of sodium tetrahydroborate.

Tin (II) Chloride (Stannous Chloride)

Tin (II) chloride (SnCl 2) can also be used as the reducing agent in mercury/hydride
analyses. It is toxic and corrosive.

Before using tin (II) chloride, you should be thoroughly familiar with all
hazards and safe handling practices. Observe the manufacturer's
recommendations for use, storage and disposal.
Wear goggles, protective clothing and gloves.
When preparing solutions, work in a fume hood. Make sure the solid is
completely dissolved and the solution is clear. Use a filter if necessary.
Handle solutions with care since they are corrosive.
When changing from sodium tetrahydroborate, use a separate analyzer
assembly or FIAS tubing assembly.
When using FIAS:
- Make sure that all tubing connections are tight to prevent leaks.
- Do not loosen or remove any connections while the system is running.
- Pump deionized water through the tubing system at the end of the day to
remove all residue.

Hydrofluoric Acid

Hydrofluoric acid (HF) is used to condition the quartz cell. It is toxic and extremely
corrosive. Hydrofluoric acid will readily burn skin, and if the fumes are inhaled,
may also burn lung tissue. Burns may not be immediately painful or visible.
Contact with eyes could result in blindness.
Mercury/Hydride Analyses Safety Practices 1-27

Before using hydrofluoric acid, you should be thoroughly familiar with all
hazards and safe handling practices. Observe the manufacturer's
recommendations for use, storage and disposal.

Always wear suitable protective equipment, including goggles, a face shield,


acid-resistant gloves, and protective clothing.
Do not breathe HF vapors. Always work in a fume hood.
Do not use a glass beaker. Hydrofluoric acid attacks glass.
Observe the additional hazards and precautions outlined in References 1 & 2.

Magnesium Perchlorate

Magnesium perchlorate is sometimes used in the drying tube of the amalgam


system accessory. Magnesium perchlorate is toxic and a powerful oxidizing agent.
Magnesium perchlorate presents severe fire and explosion hazards.

Before using magnesium perchlorate, you should be thoroughly familiar with


all hazards and safe handling practices. Observe the manufacturer's
recommendations for use, storage and disposal.

Wear suitable protective clothing, including a face shield.


Always work in a fume hood.
1-28 Safety Practices

Sample Preparation Safety Practices

Sample preparation for atomic spectroscopy may require the handling of organic or
corrosive solutions. Dilution of samples and adding dilute acid to a liquid sample is
generally less hazardous than putting a solid sample into solution. This section will
deal specifically with the potential hazards associated with dissolving solid
samples, although the information can be applied to any sample handling situation.
Also, refer to the general safety practices for handling chemicals described earlier
in this chapter, General Safety Practices - Safe Use of Chemical Reagents.

Reference 10 contains general information on sample preparation procedures as


well as an appendix on laboratory safety. Reference 11 contains information on
laboratory safety and sample preparation methods prescribed by the United States
Environmental Protection Agency (EPA).

Solid samples may be put into solution by dissolving the sample in an organic
solvent or acidic solution, digesting the sample, or reacting the sample with a
fusion mixture. Each of these techniques has certain hazards associated with it.

Always wear appropriate eye protection while preparing samples. Use safety
glasses with side shields, goggles, or full-face shields, depending on the chemicals
you are handling.

Dissolving Solid Samples in Organics

Always work in a fume hood so that flammable and/or toxic solvents do not
concentrate in the work area.

Wear protective clothing and gloves. Some solvents are readily absorbed
through the skin.

When selecting a solvent, consider the following:


• Is the solvent compatible with the equipment?
Aliphatic hydrocarbons, ketones and esters, alcohols, and xylene are the
most frequently used solvents. Make sure that all the equipment that will
come into contact with the solvent is compatible with the solvent (e.g.,
tubing, sample cups, storage and waste containers, etc.).
Sample Preparation Safety Practices 1-29

• Is the solvent toxic?


Avoid solvents known to be health hazards, such as benzene or methyl
isobutyl ketone (MIBK), which are carcinogenic.
Some solvents, such as the halogenated hydrocarbons, generate toxic gases
when heated.
Consult the data sheets provided by the manufacturer (see Reference 6) for
information on health hazards.

More information about the behavior of organic solvents with atomic spectroscopy
equipment is given in Reference 12 .

Dissolving Solid Samples Using Acids

Dissolving solid samples in aqueous solutions often requires the use of


concentrated acids.

When using acids, use the following precautions:


Always work in an acid-resistant fume hood.
Wear protective clothing, including gloves specifically resistant to the acid
being used.
Attempt to dissolve the sample in a dilute acid solution before using
concentrated acid.
Add concentrated acid to a sample cautiously. Dissolving a sample in
concentrated acid may provoke a vigorous reaction.

Acid Digestions

Acid digestions, either at atmospheric pressure or at increased pressure, require


special care. Spattering and foaming of the sample/acid mixture may expose you to
a hazard, as well as compromise the sample integrity. A digested sample containing
concentrated acid will react violently with water.

Perchloric acid and hydrofluoric acid are particularly hazardous to work with.
1-30 Safety Practices

Perchloric Acid

Perchloric acid (HClO4) is extremely corrosive and a powerful oxidizing agent. It


presents severe fire and explosion hazards.

Before using perchloric acid, you should be thoroughly familiar with its
hazards and safe handling practices. Observe the manufacturer's
recommendations for use, storage and disposal.

Use hoods, ducts, and other devices for removing vapors specifically designed
to accommodate this kind of fume. There is a severe explosion hazard if a
normal hood is used, or if the hood is not properly used and maintained.
Use goggles and face shields. Wear protective clothing and polyvinyl chloride,
not rubber gloves.
Observe the additional hazards and precautions outlined in References 1, 2, 7
and 8.

Hydrofluoric Acid

Hydrofluoric acid (HF) is also used for digestions. It is toxic and extremely
corrosive. Hydrofluoric acid will readily burn skin, and if the fumes are inhaled,
lung tissue. Burns may not be immediately painful or visible. Contact with eyes
could result in blindness.

Before using hydrofluoric acid, you should be thoroughly familiar with its
hazards and safe handling practices. Observe the manufacturer's
recommendations for use, storage and disposal.

Always wear suitable protective equipment, including goggles, a face shield,


acid-resistant gloves, and protective clothing when using hydrofluoric acid.
Do not breathe HF vapors. Always work in a fume hood when using
hydrofluoric acid.
Do not use a glass beaker. Hydrofluoric acid attacks glass.
Observe the additional hazards and precautions outlined in References 1, 2, 7
and 8.
Sample Preparation Safety Practices 1-31

Performing Digestions

When carrying out sample digestions:


Always work in a hood suitable for the chemicals you are using.
Add very small quantities of the acid dropwise, while observing the magnitude
of the reaction.
Apply heat to a digestion solution slowly in case a further vigorous reaction is
initiated.
Cool the completed digest before transferring it and diluting it. Add water
cautiously.

Digestions at Elevated Pressure

Acid digestions in a pressure digestion apparatus require special care at several


points, in addition to the precautions described above.

When using high pressure digestion vessels, consult the manufacturer's


instructions and recommendations, particularly regarding organic material
and possible explosive reactions.

Never use perchloric acid in a pressure digestion.

Use only the manufacturer's recommended amounts of sample and acid for the
type of sample you are preparing.
Be sure the apparatus is in good condition and provides safe release of pressure
in the case of excess pressure buildup.
Cool the apparatus to room temperature before attempting to open it.
Open the apparatus in a fume hood to vent the entrapped fumes safely.

Fusion Mixtures

Dissolving a sample by reacting with a fusion-flux mixture is generally chosen


when other techniques for sample dissolution fail. The fusion-flux mixture should
be carefully selected. Knowledge of fusion-flux mixture/crucible compatibility is
1-32 Safety Practices

essential. Heating the sample-flux mixture may initiate a vigorous or explosive


reaction.
Heat the mixture slowly and intermittently until the system is characterized.
If you use a muffle furnace rather than a flame for heating, make a trial using
the standard amount of flux but with a smaller amount of sample.
Most reacted fusion mixtures are dissolved in acidic solutions. Observe the
precautions described previously for handling acids.
References 1-33

References

1
Furr, K., ed., CRC Handbook of Laboratory Safety, 3rd ed., The Chemical Rubber Co.
Press, Florida, USA, 1990.
2
National Research Council, Prudent Practices for Handling Hazardous Chemicals in
Laboratories, National Academy Press, Washington, D.C., USA, 1981.
3
Compressed Gas Association (USA), "Safe Handling of Compressed Gases in
Containers," pamphlet no. P-1, 1984.
4
Compressed Gas Association (USA), "Acetylene," pamphlet no. G-1, 1990.
5
Compressed Gas Association (USA), "Standard for Nitrous Oxide Systems at Consumer
Sites," pamphlet no. G-8.1.
6
Data sheets provided by chemical manufacturers, for example:
l Material Safety Data Sheets (MSDS), USA;
l DIN-Sicherheitsdatenblätter (genormte Formular DIN -Nr 52900), FRG;
l Product Information Sheets, UK.
7
Bretherick, L., Bretherick's Handbook of Reactive Chemical Hazards, 4th ed.,
Butterworth & Co., Ltd., London, UK, 1990.
8
Sax, N., ed., Dangerous Properties of Industrial Materials, 7th ed., Van Nostrand
Reinhold, New York, USA,1989.
9
Bretherick, L., ed., Hazards in the Chemical Laboratory, 3rd ed., Royal Society of
Chemistry, London, UK, 1981.
10
Helrich, K., ed., Official Methods of Analysis, 15th ed., Association of Official
Analytical Chemists, Inc. , Arlington, VA, USA, 1990.
11
Standard Methods for the Examination of Water and Wastewater, 17th ed., American
Public Health Association et al., USA, 1989.
1-34 Safety Practices

12
Analytical Methods for Atomic Absorption Spectrophotometry, Perkin-Elmer; part no.
0303-0152 (USA); part no. B002-9672 (Europe).
System Descriptions 2
Introduction to this Chapter.................................................................................. 2-1
AAnalyst 100 Overview ......................................................................................... 2-2
AAnalyst 100 System Information ........................................................................ 2-3
AAnalyst 100 Instrument Details .......................................................................... 2-6
Spectrometer Portion Description........................................................................ 2-8
Lamp Compartment Description ....................................................................... 2-10
Deuterium Arc Background Corrector (Optional) .............................................. 2-11
Sample Area Description .................................................................................. 2-11
Burner System Description................................................................................ 2-12
Flame Gas Control Description ......................................................................... 2-14
Interlocks Description ....................................................................................... 2-14
User Interface Description................................................................................. 2-16
Keypad/Display............................................................................................. 2-16
Data Handling Features................................................................................. 2-17
AA WinLab System Controller (Optional Upgrade) ...................................... 2-17
AAnalyst 300 Overview ....................................................................................... 2-19
AAnalyst 300 System Information ...................................................................... 2-20
AAnalyst 300 Instrument Details ........................................................................ 2-23
Spectrometer Portion Description...................................................................... 2-24
Lamp Compartment Description ....................................................................... 2-26
Deuterium Arc Background Corrector ............................................................... 2-26
Sample Area Description .................................................................................. 2-27
2-2 System Descriptions

Burner System Description................................................................................ 2-27


Flame Gas Control Description ......................................................................... 2-28
Interlocks Description ....................................................................................... 2-28
User Interface Description................................................................................. 2-28
AA WinLab System Controller ..................................................................... 2-29
AA WinLab Software.................................................................................... 2-30
Atomizers............................................................................................................. 2-32
Burner System (Supplied) ................................................................................. 2-32
Graphite Furnace System (HGA-800)................................................................ 2-32
Mercury/Hydride Determination System (MHS-10)........................................... 2-34
Flow Injection Analysis System (FIAS-100 or FIAS-400) .................................. 2-36
Autosamplers ....................................................................................................... 2-38
Flame or FIAS Autosampler (AS-90 and AS-91) ............................................... 2-38
Graphite Furnace Autosampler.......................................................................... 2-40
Options And Upgrades ........................................................................................ 2-41
HGA-800 Graphite Furnace System (B300-1294).............................................. 2-41
Water Cooling System....................................................................................... 2-41
Mercury/Hydride Determination System (MHS-10)........................................... 2-41
Flow Injection Analysis System (FIAS 100 or FIAS 400) .................................. 2-41
Flame or FIAS Autosampler (AS-90 and AS-91) ............................................... 2-42
Graphite Furnace Autosampler.......................................................................... 2-42
Quartz Cell Holder (B300-0348) ....................................................................... 2-42
Electrical Heater Assembly Adapter (N040-1183) ............................................. 2-42
Deuterium Arc Background Corrector ............................................................... 2-42
Lamp Options ................................................................................................... 2-43
Lamp Adapter Cable (for coded lamps) ......................................................... 2-43
Lamp Adapter Cable (for non-coded lamps) .................................................. 2-43
Lamp Coding Plugs (for coded EDLs)........................................................... 2-44
Burner Head Options ........................................................................................ 2-44
Computer System Upgrade................................................................................ 2-45
AA WinLab Controller Kit (N040-0110) ....................................................... 2-45
AA WinLab Software Kit (N040-0109) ......................................................... 2-46
AA WinLab Upgrade Kit (N040-0111) ......................................................... 2-47
Printer Options (and accessories) ...................................................................... 2-47
Okidata Microline 320 Printer ...................................................................... 2-47
H-P LaserJet IV Printer (0942-1038)............................................................. 2-47
H-P DeskJet 660C Printer (0942-1082) ......................................................... 2-47
Parallel Printer Cable (0941-0001)................................................................ 2-48
System Descriptions 2
Introduction to this Chapter

The AAnalyst instrument line consists of two basic instruments. The first, and most
basic instrument is the AAnalyst 100. It is self-contained with its built-in keypad
and burner system. Its purpose is to perform Flame AA determinations.

The second, fully loaded, instrument is referred to as the AAnalyst 300. Its
standard features include complete system control from a computer, a motor driven
six-lamp turret for fully automatic multielement analysis, a built-in deuterium arc
background corrector and a burner system with automatic, computer-programmed
flame gas control. It is designed for optimized, cost-effective, automatic flame,
graphite furnace, FIAS, and mercury/hydride analyses.

This chapter gives a complete description overview of the AAnalyst 100 first, and
then the AAnalyst 300 next. Shared assemblies are described only once; - therefore,
if an assembly is previously described, the reader will be referred to its earlier
description.

Next, the optional autosamplers are described (Flame/FIAS Autosampler and


Graphite Furnace Autosampler). Finally, AAnalyst 100 options and the choice of
printers are discussed.
2-2 System Descriptions

AAnalyst 100 Overview

Figure 2-1. The AAnalyst 100 instrument.

The AAnalyst 100 Atomic Absorption Spectrometer is a double-beam atomic


absorption spectrometer for flame, graphite furnace and mercury/hydride analysis.
It is a sophisticated analytical system capable of performing automated single
element determinations. The basic instrument is designed for use with flame
absorption and flame emission techniques. It can be upgraded to be used with
graphite furnace and mercury/hydride atomic absorption techniques as analytical
requirements change.
AAnalyst 100 System Information 2-3

AAnalyst 100 System Information


The AAnalyst 100 system consists of an atomic absorption spectrometer instrument,
an atomizer, an optional autosampler and other accessories. Figure 2-2 presents a
block diagram representation of the system. The available atomizers, autosamplers
and accessories are listed below and discussed in this chapter.
•Atomizers
• Burner system (standard with AAnalyst 100)
• Graphite Furnace Assembly (HGA–800)
• Manually Operated Mercury/Hydride System (MHS–10)
• Flow Injection Analysis System (FIAS–100 or FIAS–400)
•Autosamplers
• Flame AA (and FIAS) Autosampler (AS–90 or AS–91)
• Graphite Furnace AA Autosampler (AS–72)
•Other Accessories and Options
• Deuterium Arc Background Corrector
• Automatic Six-Lamp Turret
• Quartz Cell Holder
• Electrical Heater Assembly Adapter
• Computer System (with AA WinLab software)
• Printer
The basic AAnalyst 100 comes standard with an easily removable burner assembly
and easily adjusted burner mount. The premix burner system includes a high-
strength plastic mixing chamber for chemical resistance and a flow spoiler.

The AAnalyst 100 gas controls include flow control for air, nitrous oxide, and
acetylene as well as automatic flame ignition. Automatic sequencing of gases when
lighting or extinguishing a nitrous-oxide-acetylene flame (even in the event of
power failure) is provided. Purging of the gas box is controlled through the keypad.

Calibration and data handling parameters are controlled via the keypad and a self-
contained two-line alphanumeric vacuum fluorescent display. It prompts the user
through system setup for flame sampling and furnace determin ations and displays
analytical results and error conditions. Method storage is included for flame
sampling, furnace and flow injection methods (10 each).
2-4 System Descriptions

Figure 2-2. Block diagram representation of the AAnalyst 100 system.


AAnalyst 100 System Information 2-5

A complete analytical system is assembled by interfacing the spectrometer


instrument with your choice of sampling or atomization systems. By configuring
the system through different combinations of the various accessories, Flame,
Furnace, or Mercury/Hydride analyses can be performed, as shown in
Figure 2-3.
AAnalyst 100

For
For For Flame - FIAS
Flame AA Graphite Furnace AA Manual System
Manual System Manual System
- Burner
- Burner - HGA-800
- FIAS 100/400

For For For For


Flame AA Graphite Furnace AA Flame - FIAS Manually Operated
Automated System Automated System Automated System Mercury/Hydride
- Burner Determination Systems
- Burner - HGA-800 - FIAS 100/400
- AS-90 Autosampler - Graphite Furnace - AS-90 Autosampler - Burner
or Autosampler or
- AS-91 Autosampler - MHS-10
- AS-91 Autosampler

Figure 2-3. Possible configurations of the AAnalyst 100 system.


2-6 System Descriptions

AAnalyst 100 Instrument Details


The following sections provide a discussion on the theory of operation and a brief
description of the components of the instrument. The optional atomizers, auto-
samplers and AAnalyst 100 accessories available are discussed later in the chapter.

Refer to the next figure when reading about the AAnalyst 100 instrument. The
drawing will help to give you a general idea where the subassemblies are located
inside the instrument. The subassemblies are listed here:
• spectrometer • flame gas controls
• lamp compartment • interlocks
• sample area • user interface (keypad/display)
• burner system (atomizer)
AAnalyst 100 Instrument Details 2-7

User Interface (Keypad/Display) Spectrometer Portion (optics)

Sample Area Lamp Compartment

Removable
Burner Door

Atomizing
Source
(burner)

Detachable Sample Tray (1 of 2)


Flame Gas Controls
Interlock Connector (behind burner)

Drain
Vessel

Figure 2-4. General location of subassemblies in the AAnalyst 100.


2-8 System Descriptions

Spectrometer Portion Description


The spectrometer portion of the instrument provides a means of measuring light
at a specific wavelength. To perform this function, the spectrometer uses a primary
light source, monochromator optics, and a detector.

The primary light source, either a hollow cathode lamp or an electrodeless


discharge lamp, is placed in the spectrometer to emit the narrow atomic lines of the
element to be determined. The light from the lamp is optically chopped and passed
alternately through and around the flame. When the light passes through the sample
compartment, a portion of it is absorbed by the atomized sample. The beams are
then recombined and travel through to the monochromator.

The monochromator optics disperse the various wavelengths of light and isolates
the particular line of interest. A dual-blazed grating is used, which provides
optimized performance over the entire atomic absorption wavelength.

The light leaving the monochromator is directed onto the detector, a


photomultiplier tube (PMT), which produces an electrical signal proportional to the
light intensity. The electrical signal is amplified and processed to produce a signal
which is a measure of the light attenuation (i.e. absorbed) occurring in the sample
compartment. A detailed drawing of the optical system is shown next.
AAnalyst 100 Instrument Details 2-9

Figure 2-5. The optical schematic of the AAnalyst 100.


2-10 System Descriptions

Lamp Compartment Description

The basic AAnalyst 100 instrument includes a single lamp mount. It can also be
purchased as an automatic six-lamp turret. Note that the AAnalyst 300 comes
standard with the automatic six-lamp turret. If interested, you’ll find the turret
details later in this chapter under AAnalyst 300 Instrument Details - Lamp
Compartment -Automatic Six-Lamp Turret.

Figure 2-6. Single lamp mount and an HCL in the AAnalyst 100.

Access to the lamp compartment in the AAnalyst 100 is at the front of the
spectrometer, allowing for easy lamp installation and removal.

Features of the AAnalyst lamps include:


• cableless, quick-connect lamps that simplify lamp installation;
• fully automated wavelength, current, and slit selection for hollow cathode
lamps which reduce setup time;
• fully automated wavelength and slit selection for electrodeless discharge
lamps which reduces setup time;
• milliampere-hour timers on all hollow cathode lamps permit the
monitoring of lamp usage for Good Laboratory Practices compliance as
well as lamp replacement scheduling;
• the optional programmable six-lamp turret allows automated
sequential multi-element analysis (with WinLab).
AAnalyst 100 Instrument Details 2-11

Deuterium Arc Background Corrector (Optional)

The deuterium arc background corrector is an available option for the AAnalyst
100. The spectrometer is designed to use a deuterium arc lamp to correct for
background absorbance caused by non-atomic species in the atom cloud. Since it is
an option for the AAnalyst 100, detailed information on the deuterium arc
background corrector is given later in this chapter in the section called AAnalyst
300 Instrument Details -Lamp Compartment -Deuterium Arc Background
Corrector.

Sample Area Description


The sample area opens at the front for easy access via a removable burner door.
The flame can be monitored through the flame shield in the door, which transmits
about 10% of the visible radiation. (Potentially hazardous UV radiation is not
transmitted.) The large 29-cm wide by 25-cm deep (11.4 by 9.8 inch) sample
compartment accommodates a wide variety of Perkin-Elmer sampling accessories.
These include the standard burner system, an HGA graphite furnace or a
mercury/hydride system. It is designed for easy interchange between sampling
systems. Two detachable corrosion-resistant sample trays are also provided.

Figure 2-7. Sample compartment door (the burner door).


2-12 System Descriptions

Burner System Description


The basic AAnalyst 100 instrument includes a burner system for flame sampling
operation. The Perkin-Elmer burner system consists of a nebulizer, burner (mixing)
chamber, burner head, ignitor, drain system, and a quick disconnect gas supply
with a safety interlock system. All of this is assembled on a removable burner
mount. In basic terms, the heat produced by the burner converts the sample into
free atoms that can absorb the light from the source lamp for the element(s).
Flame Sensor Notch
Burner
Head

Burner (Mixing) Chamber

NEB Side Arm


Ignitor
Burner End Cap Assembly

AUX
Oxidant Hose

FUEL
Inlet Hose Main Interlock
Connector
Mechanical
Nebulizer Interlock
Knob

Capillary
Tube

Drain
Tube Burner Mount
Horizontal
Adjustment Knob NEB Oxidant Hose

Vertical Adjustment Knob Rotational Adjustment Knob

Figure 2-8. The burner system and its parts.


AAnalyst 100 Instrument Details 2-13

The burner system works in the following way. A sample solution is


aspirated through the nebulizer and sprayed as a fine aerosol mist into the burner
(mixing) chamber. Here the sample mist is thoroughly mixed with fuel and either
air or nitrous oxide gases, prior to ignition. Fuel gas enters the burner chamber
through the fuel (inlet) hose while the oxidant enters through the nebulizer side-
arm and the AUX oxidant inlet. The mix is next carried to the burner head, where
combustion and atomization occurs after ignition (via the ignitor).
To prevent incomplete sample atomization, a flow spoiler (not shown) is placed
inside the mixing chamber directly in front of the nebulizer. Larger sample droplets
not carried around the flow spoiler by the gas flow are forced by the spoiler to the
bottom of the chamber. From there, they travel through the drain system (i.e. they
are removed from the chamber through the drain tube to the drain vessel).

The manual gas control system (not shown) monitors and controls fuel and oxidant
flows. Burner operation, including flame ignition and shutoff, is controlled through
the instrument keypad on the AAnalyst 100.

An all-titanium, 10-cm, single-slot burner head for air-acetylene operation is


standard (N040-0102) with the AAnalyst 100. Other burner heads are available:
• all-titanium, 5-cm, single-slot burner head for nitrous oxide-acetylene
operation (N040-0100)
• all-titanium, 5-cm, single-slot burner head for air-acetylene operation
(N040-0101)
• all-titanium, 10-cm, three-slot burner head for analysis of high dissolved
solids content solutions with air-acetylene flames (N040-0103).

The 5-cm single-slot burner head for air-acetylene is rotatable to 90 degrees.

The burner mount provides horizontal, vertical, and rotational adjustment. The
quick-disconnect lever plate simplifies changeover to the optional HGA furnace
operation where the furnace and optional autosampler are mounted on a sampling
arm that can be easily rotated into the area.

Since this chapter is a system description overview, refer to the chapter in this
manual called Burner System for more details.
2-14 System Descriptions

Flame Gas Control Description

Individual gas controls, meters, and sensors are provided for oxidant and fuel, with
push button selection of the fuel-oxidant combination (gases off, air-acetylene, or
nitrous oxide-acetylene). The push-button-actuated automatic ignition system will
ignite the flame only when using air-acetylene.

Interlocks Description

There are six burner system interlocks. Most of them go through the interlock
connector that is located behind the quick disconnect release plate (see Figure
2-9). One is a mechanical interlock. The other five interlock sensors are: the drain,
the burner head, the flame sensor, the nebulizer, and the sample compartment
thermal shield. Other interlocks monitor fuel/oxidant pressure. Note that it is
always safe to power off the instrument to shut down the flame.

Interlocks prevent ignition if any of the following are incorrectly installed:


•the wrong type of burner head (air-acetylene or nitrous oxide-acetylene),
•the nebulizer/end cap or
•the burner drain system.

Interlocks also prevent ignition when the level of the liquid in the drain vessel is
incorrect, or gas pressures are too low. The interlocks will automatically shut down
burner gases if a flame is not detected, if fuel or oxidant pressures are not within
acceptable limits or if the thermal shield temperature is too high. Acetylene flow is
automatically incrementally adjusted prior to the oxidant change when switching to
or from nitrous oxide-acetylene operation. Provisions are included for safe
shutdown from all operating modes in the event of a power failure.
AAnalyst 100 Instrument Details 2-15

Quick Disconnect
Release Plate
Clear Rubber Button
Interlock
Mechanical Connector
Interlock Knob

Figure 2-9. Location of the main interlock connector.


2-16 System Descriptions

User Interface Description

Keypad/Display

The user interface for the AAnalyst 100 is a corrosion-resistant membrane keypad
with a two-line, 20-character/line, alphanumeric, vacuum fluorescent display.

Figure 2-10. AAnalyst 100 keypad and display.

The alphanumeric display provides prompting, allowable entry ranges, and warning
messages to simplify user interaction. A full numeric keypad with decimal and
clear entry keys is provided for data entry. Operating parameters and modes for
flame, furnace, and flow injection analysis are push button-selectable. Parameters
may be entered in a programmed mode or individually accessed. Up to 10
parameter sets (‘methods”) each may be stored and recalled for flame, furnace, and
flow injection sampling.
AAnalyst 100 Instrument Details 2-17

Data Handling Features

The AAnalyst 100 has many data handling features. Instrument readings are
linear in absorbance (-0.500 A to 3.000 A), concentration or emission intensity
with continuously variable scale expansion from 0.01 to 100 times. Integration
times are operator-selectable from 0.1 to 60 seconds in increments of 0.1 seconds.
Reading modes include time-averaged integration, non-averaged integration (peak
area), and peak height measurement. Built-in statistics include averaging (up to 99
readings), standard deviation and relative standard deviation.

Automatic zero setting and concentration calibration are included, with the
capability to use up to eight calibration standards and a choice of calibration
equations: a linear least squares fit, a nonlinear fit, or the method of additions.
Reslope of the analytical curve can be effected using a single operator-selected
calibration standard.

Results are shown using up to four significant digits with polarity indication,
adjustable decimal, and up to three leading zeros for decimal setting. Direct
connection is provided for use of a laboratory recorder (0-1 V analog) in flame
sampling mode and a printer (standard Centronics parallel) in all modes. Printer
output includes analytical results, calibration curves, and automatically scaled peak
profiles (atomic absorption and background absorption).

An IEEE-488 interface board is built-in for the use of the optional AS-90/91
Autosampler, HGA-800 Graphite Furnace, the Furnace Autosampler, FIAS-100 or
FIAS-400 Flow Injection System, and the AA WinLab Controller/Data System.
Other optional systems and devices can be connected and controlled via the
optional system controller (also known as the computer) if the user wishes to
upgrade the AAnalyst 100 at some future date.

AA WinLab System Controller (Optional Upgrade)

For laboratories that require advanced data handling capabilities, either now or in
the future, the AAnalyst 100 can be upgraded and combined with the AA WinLab
Controller kit (N040-0110). This system uses the same industry-standard personal
computer as the AAnalyst 300 and the same state-of-the-art AA WinLab software.

The Perkin-Elmer AA WinLab software was designed by practicing analysts to be


used as a friendly user interface in normal laboratory environments. It was written
2-18 System Descriptions

expressly for operation under Windows and follows the same familiar Windows
conventions, offering all the advantages of Windows.

The AA WinLab software includes all the features you need in a single package:
• advanced data handling and data control
• automatic data storage and retrieval, including final results, raw data
and graphics
• methods and results that are stored in a commercially available
database library that is compatible with a variety of off-the-shelf
database management programs for further data manipulation or
reporting
• enhancements in quality assurance protocols that make it even easier
to comply with government or contract requirements.

Refer to the section called AAnalyst 300 Instrument Details - User Interface - AA
WinLab System Controller in this chapter for more information on this computer
option.

Upgrades and options are discussed at the end of this chapter in the section called
Options and Upgrades.
AAnalyst 300 Overview 2-19

AAnalyst 300 Overview

Figure 2-11. The basic AAnalyst 300 instrument.

The AAnalyst 300 Atomic Absorption Spectrometer is a double-beam atomic


absorption system capable of performing flame, furnace, and mercury/hydride
sampling. It is a sophisticated analytical system capable of performing automated
sequential multi-element analysis.

The AAnalyst 300 is designed for optimized, cost-effective, automatic flame,


graphite furnace, FIAS, and mercury/hydride analyses. Standard features include
complete system control from a computer keyboard and mouse, a motor-driven six-
lamp turret for fully automatic multielement analyses, built-in deuterium arc
background corrector and the Perkin-Elmer burner with automatic, computer-
programmed flame gas control.

Features of the AAnalyst 300 spectrometer include:


• automatic lamp selection with an automatic six-lamp turret
• high energy, double-beam optical system providing optimum precision
and detection limits
• automatic monochromator setup for wavelength and slit width
• control of atomization systems and accessories by a central computer
• continuum source background correction.
2-20 System Descriptions

AAnalyst 300 System Information

A complete AAnalyst 300 system is assembled by interfacing the spectrometer with


a computer and selecting from various sampling or atomization systems. The
available atomizers, autosamplers, and accessories are listed below and discussed
later in this chapter.
•Atomizers
• Burner system (standard with AAnalyst 300)
• Graphite Furnace Assembly (HGA–800)
• Manually Operated Mercury/Hydride System (MHS–10)
• Flow Injection Analysis System (FIAS–100 or FIAS-400)
•Autosamplers
• Flame AA (and FIAS) Autosampler (AS–90 or AS-91)
• Graphite Furnace AA Autosampler
•Other Accessories and Options
• Printer

By configuring the system through different combinations of the various


accessories, flame, furnace, or mercury/hydride analyses can be performed,
as illustrated in the figure on the next page.
AAnalyst 300 System Information 2-21

Figure 2-12. Block diagram representation of the AAnalyst 300 systems.


2-22 System Descriptions

A complete analytical system is assembled by interfacing the spectrometer


instrument with your choice of sampling or atomization systems. By configuring
the system through different combinations of the various accessories, Flame,
Furnace, or Mercury/Hydride analyses can be performed, as shown in
Figure 2-13.

Figure 2-13. Possible configurations of the AAnalyst 300 system.


AAnalyst 300 Instrument Details 2-23

AAnalyst 300 Instrument Details

The following provides a discussion on the theory of operation and a description of


the components of the instrument. The optional atomizers, autosamplers and
accessories for the AAnalyst 300 are discussed later in this chapter.

Refer to the figure below when reading about the AAnalyst 300 instrument. The
drawing will help to give you a general idea where the sub-assemblies are located
inside the instrument. The subassemblies are listed here:
• spectrometer • burner system (atomizer)
• lamp compartment • interlocks
• sample area • user interface (computer)

Sample Area Spectrometer Portion Lamp Compartment


Removable (optics ) (turret)
Burner Door

User Interface Burner


(computer) System

Detachable Sample Tray (1 of 2)


Interlock Connector (behind burner)

Drain
Vessel

Figure 2-14. General location of subassemblies in the AAnalyst 300.


2-24 System Descriptions

Spectrometer Portion Description

The spectrometer portion provides a means of measuring light at a specific


wavelength. To perform this function, the spectrometer uses a primary light source,
monochromator optics, and a detector.

The primary light source, either a hollow cathode lamp or an electrodeless


discharge lamp, is placed in the spectrometer to emit the narrow atomic lines of the
element to be determined. The light from the lamp is optically chopped and passed
alternately through and around the flame. When the light passes through the sample
compartment, a portion of it is absorbed by the atomized sample. The beams are
then recombined and travel through to the monochromator.

The monochromator optics disperse the various wavelengths of light and isolates
the particular line of interest. A dual-blazed grating is used, which provides
excellent performance over the entire atomic absorption wavelength range.

The light leaving the monochromator is directed onto the detector, a


photomultiplier tube (PMT), which produces an electrical signal proportional to the
light intensity. The electrical signal is amplified and processed to produce a signal
which is a measure of the light attenuation (i.e. absorbed) occurring in the sample
compartment.

The AAnalyst 300 uses a deuterium arc lamp to correct for background absorbance
caused by non-atomic species in the atom cloud. The section to follow called
Deuterium Arc Background Corrector gives the details on the deuterium arc lamp.
AAnalyst 300 Instrument Details 2-25

Figure 2-15. The optical schematic for the AAnalyst 300.


2-26 System Descriptions

Lamp Compartment Description

Access to the lamp compartment in the AAnalyst 300 is from the front of the
spectrometer, allowing for easy lamp installation and removal.

Features of the AAnalyst lamps include:


• cableless, quick-connect lamps that simplify lamp installation
• fully automated wavelength, current, and slit selection for hollow cathode
lamps which reduces setup time
• fully automated wavelength and slit selection for electrodeless discharge
lamps which reduces setup time
• fully automated lamp alignment
• programmable six-lamp turret allows automated sequential
multielement analysis
• milliampere-hour timers on all hollow cathode lamps permit the
monitoring of lamp usage for Good Laboratory Practices compliance as
well as lamp replacement scheduling

The AAnalyst 300 instrument includes a six-lamp turret as a standard feature. See
the turret details next under Automatic Six-Lamp Turret.

Automatic Six-Lamp Turret

A computer-controlled motor-driven, six-lamp turret provides fully automated


operation including automatic lamp alignment with Perkin-Elmer Lumina,
Intensitron coded hollow cathode lamps and electrodeless discharge lamps. The
automatic turret is internally installed, obtaining its power from the instrument.
Access to the lamp turret is from the front of the spectrometer allowing easy lamp
installation.

Deuterium Arc Background Corrector

The Deuterium Arc Background Corrector comes standard with the AAnalyst
300. It is an internally mounted assembly that provides simultaneous correction for
molecular absorption and light-scattering. The spectrometer uses a deuterium arc
lamp to correct for background absorbance caused by non-atomic species in the
atom cloud.
AAnalyst 300 Instrument Details 2-27

When the deuterium arc background corrector is used, two alternating sets
of measurements are made: one with the primary source and a second with
the background corrector source. The primary source measures a combination
of background and atomic absorption. The continuum source measures only the
background. The difference between the two measurements yields the atomic
absorption.

A deuterium arc source is used for maximum wavelength coverage and intensity.
The AAnalyst 300 can accurately handle combined atomic plus background
absorption signals as large as three absorbance units.
The background corrector is internally installed, with its power supplied from the
instrument. Power to the source is automatically and continuously adjusted to be in
the optimum range for operation. The deuterium arc lamp is easily accessible,
allowing convenient replacement of the lamp by the users.

Sample Area Description

The sample area opens to the front for easy access via a removable burner door.
The flame can be monitored through the flame shield on the door, which transmits
about 10% of the visible radiation. (Potentially hazardous UV radiation is not
transmitted.) The large 29-cm wide by 25-cm deep (11.4 by 9.8 inch) sample
compartment accommodates a wide variety of Perkin-Elmer sampling accessories.
These include the standard burner system, an HGA graphite furnace or a
mercury/hydride system. It is designed for easy interchange between sampling
systems. Two detachable corrosion-resistant sample trays are also provided.

Burner System Description

The AAnalyst 300 is supplied with the Perkin-Elmer pre-mix burner system. The
burner system includes a high-strength mixing chamber for chemical resistance, an
adjustable Universal GemTip corrosion-resistant nebulizer, and an all-titanium
10 cm air-acetylene burner head. The entire assembly is made for quick removal
using the quick disconnect mounting system.

With the intent to avoid repeating common information, the burner details are given
earlier in this chapter in the section called AAnalyst 100 Instrument Details -
Burner System.
2-28 System Descriptions

Flame Gas Control Description

Automatic flame gas controls feature a computer-controlled oxidant selection with


automatic gas sequencing and oxidant and fuel monitoring and control. The flame
can be ignited only with air-acetylene using the automatic ignition system.

Interlocks Description

There are six burner system interlocks. Most of them go through the interlock
connector that is located behind the quick disconnect release plate (see Figure
2-9). One is a mechanical interlock. The five interlock sensors are: the drain, the
burner head, the flame sensor, the nebulizer, and the sample compartment thermal
shield. Other interlocks monitor fuel/oxidant pressure. Note that it is always safe to
power off the instrument to shut down the flame.

Interlocks prevent ignition if any of the following are incorrectly installed:


•the wrong type of burner head (air-acetylene or nitrous oxide-acetylene),
•the nebulizer/end cap or
•the burner drain system.

Interlocks also prevent ignition when the level of the liquid in the drain vessel is
incorrect, or gas pressures are too low. The interlocks will automatically shut down
burner gases if a flame is not detected, if fuel or oxidant pressures are not within
acceptable limits or if the thermal shield temperature is too high. Acetylene flow is
automatically incrementally adjusted prior to the oxidant change when switching to
or from nitrous oxide-acetylene operation. Provisions are included for safe
shutdown from all operating modes in the event of a power failure. Purging (or
bleeding) of the gas box is controlled through the keyboard.

Software will show Flame On/Off. In the event of an emergency, power off the
instrument to shut down the flame.

User Interface Description

The AAnalyst 300 system includes a system controller. Its components are
described in the next few sections.
AAnalyst 300 Instrument Details 2-29

AA WinLab System Controller

Full control of the spectrometer and optional accessories (such as Flow Injection
Systems, Flame/FIAS Autosamplers, HGA-800 Graphite Furnace and Fu rnace
Autosampler) is via an industry standard personal computer (PC) using Perkin-
Elmer AA WinLab™ software. The AA WinLab software runs under the
Microsoft® Windows operating environment.

The minimum requirements of the system controller follow:


• a personal computer with an 486 microprocessor operating at 33 MHz
• 8 MB RAM memory (or more)
• 500 MB hard disk drive
• at least one 1.4 MB 3.5" floppy disk drive
• a keyboard and mouse
• one serial and one parallel port
• SVGA color graphics board
• 640 x 400 x 16 graphics monitor
• IEEE-488 interface board
• Microsoft Windows 3.1 and
• appropriate connecting cables

The recommended computer configuration the system controller follows:


• a personal computer with an Pentium microprocessor, 75+ MHz
• 16 MB RAM memory (or more)
• 800+ MB hard disk drive
• at least one 1.4 MB 3.5" floppy disk drive
• a keyboard and mouse
• serial and parallel ports
• SVGA color graphics board
• 800 x 600 x 256 graphics monitor
• IEEE-488 interface board
• Windows 95 and
• appropriate connecting cables
2-30 System Descriptions

The system controller controls the hardware components and collects, processes,
and stores the analytical data. As previously mentioned, it provides integrated
control of the spectrometer, the gas system and all the intelligent accessories.
Specifically, the controller provides the following: single keyboard control of
wavelength, slit width, and gas flows; automatic sequencing of gases when lighting
or extinguishing a nitrous-oxide-acetylene flame (even in the event of power
failure); automatic burner head, nebulizer/end cap, flame sensing; fuel and oxidant
pressure sensing; thermal shield temperature sensing; liquid level in drain vessel
sensing; and a burner drain interlock. When used with Perkin-Elmer Lumina 
Hollow Cathode Lamps, the AAnalyst 300 will automatically align the lamp, set
lamp current, wavelength and slit settings.

Data handling is taken care of by the computer. The computer processes the signals
received from the spectrometer to produce a readout of sample concentration. The
computer communicates with the spectrometer, atomization system (i.e. burner or
furnace), and other system components through an IEEE-488 interface.
The system controller benefits include:
• state-of-the-art performance, features and reliability
• fully configured system to accommodate current and future needs
• industry-standard hardware minimizes training requirements
• directly compatible with thousands of third-party software programs
• permits easy addition of new system components

A DeskJet printer or LaserJet printer and a connecting cable is required for data
logging via the parallel interface (optional).

AA WinLab Software

The Perkin-Elmer AA WinLab software, based on the Microsoft Windows


operating system, controls the AAnalyst 300 spectrometer and its major
accessories. AA WinLab was designed by practicing analysts to be used in normal
laboratory environments. It was written expressly for operation under Windows
and follows the same familiar conventions, offering all the advantages of Windows.

The user interfaces with the system using the system controller’s keyboard or
mouse pointing device and a high resolution, bit-mapped graphics display (CRT).
The user interface includes a clear graphical design, task-oriented organization of
AAnalyst 300 Instrument Details 2-31

the windows, drop-down menus, and a toolbar to provide rapid access to


and selection of all operating functions and commands.

Common, easily understood terms are used to define user-selectable options, with
preprogrammed default values and/or allowable range prompts for numerical
entries. An on-line, context-sensitive Help is included, as are built-in “cookbooks”
providing instant access to recommended analytical parameters for use with flame,
furnace, FIAS and me rcury/hydride sampling techniques. Permanently defined
function keys are used to provide access to frequently used commands such as
FLAME ON/OFF and READ.

Single-element and multi-element method files and analytical data files may be
stored on hard disk for later recall and use. Files may also be stored on floppy disks
for archival or backup purposes. Graphic data may also be stored and recalled for
later manipulation, including replot, scaling, and factoring. The AA WinLab
software also includes automatic quality control features such as check samples
with user-specified tolerance ranges and courses of action if the results are outside
the allowable ranges. AA WinLab software allows data files to be transferred to
other Windows-based software providing advanced, customized report generation
capabilities. Both alphanumeric and graphic data may be printed with an o ptional
printer (purchased separately) for hard copy printout.

AA WinLab software includes all the necessary features in a single package - from
method development to report generation. Supplementary programs are not needed
in order to use a different accessory device, perform quality control procedures, or
prepare reports.

AA WinLab software benefits are many. They include:


• ease of use
• reduced training requirements;
• a shared common interface style with Perkin-Elmer ICP, ICP-MS
and other AA instruments - further reducing training expense
• allowing for more features and analytical options to be included
without increasing operational complexity.

The booklet A Guide to AA WinLab (Order No. L-1906) provides more


information on the AA WinLab software.
2-32 System Descriptions

Atomizers

The purpose of an atomizer is to provide the thermal energy necessary to dissociate


chemical compounds, thus providing free analyte atoms so that atomic absorption
can occur.

The various types of atomizers available for the instrument include:


• a burner system (for flame sampling analysis)
• a graphite furnace (for furnace analysis)
• a heated quartz cell for mercury/hydride determinations

Burner System (Supplied)

As mentioned previously, the burner system included as standard with both the
AAnalyst 100 and AAnalyst 300 consists of a nebulizer, burner (mixing) chamber,
burner head, drain system, and built-in gas controls with a safety interlock system.
In an effort not to repeat information, see the section called AAnalyst 100
Instrument Details - Burner System for burner system details (found earlier in this
chapter).

Graphite Furnace System (HGA-800)

The method of Graphite Furnace Atomic Absorption (GFAA) allows the


determination of over 40 elements in microliter sample volumes with detection
limits typically 100 to 1000 times better than those of Flame Atomic Absorption.

Figure 2-16. The HGA-800 Graphite Furnace with optional Autosampler.


Atomizers 2-33

The optional HGA-800 Graphite Furnace is a high sensitivity sampling


device that is controlled automatically by the AAnalyst. It consists of a furnace and
power supply. The sample is placed inside the graphite tube. The tube is
electrically heated to atomize the sample. A continuous flow of inert gas inside and
outside the tube protects the tube from air oxidation and flushes out the gaseous
products. The furnace is water-cooled, via tap water or a water cooling system, to
maintain the furnace temperature and to cool it between analyses.

Operating parameters (including a furnace program) are entered and stored in the
instrument's memory, and then implemented during analysis. When the system is
operated by a computer, the computer will instead maintain the operating
parameters.

The HGA-800 Graphite Furnace combined with either of the AAnalyst Systems
offers the following advantages for sample determination:
• atomization of the entire sample in a few seconds
• only microliters of sample are needed
• the unique mounting system lets you change easily between flame and
furnace sampling systems
• a fast heating rate (2000 oC/sec) permits lower atomization temperatures,
extends tube life and gives maximum sensitivity
• a photodiode temperature control ensures reproducible atomization
temperatures for optimum analytical precision
• complete operation of the furnace from the AAnalyst keypad or computer
• versatile temperature programming provides the flexibility to analyze a
wide variety of sample types under optimum conditions
• alternate gas selection extends system flexibility
• optional circulatory cooling system eliminates the need for an external
cooling water source

The intent of this manual is to discuss the information that pertains to the
relationship between the HGA-800 furnace and the AAnalyst instrument. For
detailed information on the HGA-800, refer to manual that came with the furnace.
2-34 System Descriptions

Mercury/Hydride Determination System (MHS-10)

Mercury/Hydride Systems are proven accessories for high sensitivity


determinations of mercury and metallic hydride-forming elements, including As, Se,
Sb, Te, Bi and Sn by atomic absorption spectroscopy.

The basic components of a mercury/hydride system are the reaction vessel and
sampling cell. The sample solution reacts with a reducing agent in the reaction
vessel. A spontaneous reaction occurs to form the gaseous hydride or to reduce
mercury to its elemental form. The gaseous products are carried to the sample cell,
a quartz cell placed in the light path of the spectrometer. The quartz cell is heated
to dissociate the hydride gas into free atoms, or in the case of mercury, to prevent
condensation of the water vapor.

Figure 2-17 The MHS-10 and its parts.

The MHS-10 is a manual system. The quartz cell is heated by the flame. Key
operating parameters are controlled by the instrument control panel. Data
collection, calibration, and calculation functions are performed by the instrument
or optional computer.
Atomizers 2-35

The MHS-10 analyzer assembly is freestanding and is located near the


sample compartment of the spectrometer. This assembly includes a reaction flask, a
reservoir for the reducing agent, and all pneumatic components for control of the
carrier gas and transport of metallic vapors to the quartz cell.

The cell assembly consists of a quartz cell and a mount. The mount installs on the
AAnalyst burner head, positioned above the single slot in the burner head,
permitting the quartz cell to be heated in the flame. See the figure below.

Figure 2-18. The MHS-10 sample cell mounted on the burner.

The intent of this manual is to discuss the information that pertains to the
relationship between the MHS-10 and the AAnalyst instrument. For detailed
information on the Mercury/Hydride System, refer to the manual that came with
the instrument.
2-36 System Descriptions

Flow Injection Analysis System (FIAS-100 or FIAS-400)

Flow Injection Analysis (FIA) is used to inject an exact, reproducible volume of


sample into a continuously flowing liquid carrier stream. Flow Injection Analysis
can be used:
• as a fully automated sample preparation system for mercury/hydride
analyses, reagent addition, dilution, analyte preconcentration, and other
preparatory procedures
• for microsampling capabilities when performing flame analyses
• for direct analysis of solutions with a high dissolved solids content.
The Perkin–Elmer Flow Injection Analysis System (FIAS) includes peristaltic
pumps, a flow injection valve, chemifold, gas/liquid separator, and tubing. The
flow injection valve is used to inject the sample solution into a carrier stream.
Different sized injection loops are available to accommodate different injection
volumes. The chemifold is used to combine different fluid streams to allow
reaction, dilution, or matrix modification.

Figure 2-19. A view of the FIAS-400 system.


Atomizers 2-37

When the AAnalyst is configured without a computer, the flow injection


system is fully controlled by the instrument. Eleven preprogrammed methods are
stored in the instrument memory and are accessed using three or four keystrokes on
the instrument control panel. When a computer is added, the restriction on the
maximum number of programs is removed.

Perkin-Elmer pioneered the use of flow injection techniques with atomic


spectroscopy, and all of the benefits are available with the AAnalyst and our flow
injection systems. Flow injection capabilities allow you to save time, costs, and -
power while extending your analytical capabilities. The FIAS System (FIAS 100
or FIAS 400) when combined with either of the AAnalyst Systems offer the
following advantages for sample determination:
• faster analyses
• automated sample dilution and reagent addition
• lower reagent usage and sample volume requirements
• reduced waste disposal expense
• automated cold vapor mercury determinations using U.S. Environmental
Protection Agency approved method 245.1
• automated cold vapor mercury determinations with preconcentration for
lowest detection limits using the optional Amalgamation System using
WinLab
• automated hydride generation determinations
• enhanced performance with high dissolved solids content solutions
• automated analyte preconcentration (requires a FIAS-400 and AA
WinLab Controller)

The intent of this manual is to discuss the information that pertains to the
relationship between the FIAS and the AAnalyst instrument. For detailed
information on the FIAS 100 or FIAS 400, refer to the manual that came with the
instrument.
2-38 System Descriptions

Autosamplers

Routine analyses using a Perkin-Elmer FIAS instrument are simplified using an


autosampler. An autosampler allows for automated flame and flow injection
sampling. Autosamplers are computer-controlled, multipurpose sampling devices.

The autosampler consists of a sample table including the sampling arm with a
stepper motor, a sample probe with transport capillary, a sample tray and
interfacing electronics. Precise stepper motors move the autosamplers sampling
arm to its programmed X-Y-Z coordinates.

Easily removable sample trays provide the flexibility of using a variety of


differently sized sample vessels to support a wide range of application requirements
and dilution volumes. The autosampler has removable trays for easy sample
loading. Once the tray is loaded, the sample is automatically pipetted using a probe
placed in a mechanically operated sampling arm. Three sample trays are available
for each autosampler model, covering a variety of sample volume and total sample
capacity requirements.

Some of the conveniences realized using an autosampler include:


• rinsing between samples (WinLab)
• running standards to calibrate and recalibrate the instrument
• running check samples to check instrument performance (WinLab)
• introduce a matrix modifier into the graphite furnace (furnace only)

Flame or FIAS Autosampler (AS-90 and AS-91)

The previous section discusses the function of an autosampler. This section


discusses the specific features of the AS-90 and AS-91. They are used for flame
sampling or FIAS analyses.

The AS-90 and AS-91 Autosamplers provide the following advantages:


• complete instrument control from the same interface as the AAnalyst
• single keypad (or keyboard) control offers simplified system operation
• autosampler parameters are saved with method files
Autosamplers 2-39

• sample trays are easily changed, allowing for “off-line” sample


preparation and tray loading, resulting in time savings and operator
convenience (sample tray capacities listed below)
• trays hold a large number of solutions and a variety of sample vessels
• sampling probe can be equipped with any of three types of capillary
tubing assembly, therefore tubing having different diameters can be used
for selected samples at minimal cost
• automatic calibration or reslope at user-specified locations automatically
corrects for changes in operating conditions and improves analytical
performance
• automatic replicate analyses where 1-99 replicate determinations can be
programmed and performed

For those using the AA WinLab Controller, the following advantages can also be
realized (in addition to the ones stated above):
• programmed sampling permits the determination of operator-selected
elements in each sample
• random access sampling permits samples and standards to be inserted in
any order allowing maximum flexibility

The difference between the AS-90 and AS-91 autosamplers is the choice of sample
trays. The following table explains:

Table 2-1. AS-90 and AS-91 autosamplers

AS-90 AS-90 AS-91 AS-91


Sample Tray Sample Sample Tray Sample
Capacity Vessel Size Capacity Vessel Size

144 sample vessels 4.5 mL, 6 mL 218 sample vessels 4.5 mL, 6 mL,
8 mL

98 sample vessels 15 mL, 16 mL 152 sample vessels 15 mL, 16 mL

36 sample vessels 50 mL 55 sample vessels 50 mL


2-40 System Descriptions

Graphite Furnace Autosampler

The Graphite Furnace Autosampler combined with the HGA-800 furnace and
either of the two AAnalyst Systems offers the following advantages for sample
determination:
• single keypad (or keyboard) control offers simplified system operation
• autosampler parameters are saved with method files
• automatic calibration or reslope at user-specified locations automatically
corrects for changes in operating conditions and improves analytical
performance
• automatic replicate analyses where 1-99 replicate determinations can be
programmed and performed
• programmable sample number that displays and prints the sequential
sample identification number with analytical results
• includes two sample trays - a 40-position and an 80-position
• 40-position tray accommodates thirty-five 1.5-mL (or 3-mL) cups and
five 25-mL containers
• 80-position tray accommodates seventy-five 1.1-mL cups and
five 25-mL containers
• sample trays are easily changed, allowing for “off-line” sample
preparation and tray loading, resulting in time savings and operator
convenience

For those using the AA WinLab System Controller, the following advantages can
also be realized (in addition to the ones stated above):
• programmed sampling permits the determination of operator-selected
elements in each sample
• random access sampling permits samples and standards to be inserted in
any order allowing maximum flexibility
• the automatic generation of calibration solutions (including those for the
method of standard additions) and spikes allows for improved accuracy
and simplified operation
• the automatic addition of one or two modifiers allows for improved
accuracy and simplified operation (note that stand-alone allows single
modifier)
Options And Upgrades 2-41

• automatic resampling with smaller sample volumes (if reading


exceeds calibration limits) simplifies operation and saves time

Options And Upgrades


HGA-800 Graphite Furnace System (B300-1294)

The Graphite Furnace system is a high sensitivity sampling device that is controlled
automatically by either of the AAnalyst instruments. It allows the determination of
over 40 elements in microliter sample volumes with detection limits typically 100 to
1000 times better than those of flame AA.

Refer to the section called Atomizers - Graphite Furnace System (HGA-800) found
earlier in this manual for the full HGA-800 details.

Water Cooling System

Used with the furnace. It is a recirculator system.

Mercury/Hydride Determination System (MHS-10)

Mercury/Hydride Systems are proven accessories for high sensitivity


determinations of mercury and metallic hydride-forming elements, including As, Se,
Sb, Te, Bi and Sn by atomic absorption spectroscopy.

Refer to the section earlier in this manual (Atomizers - Mercury/Hydride


Determination System, MHS-10) for the MHS-10 details.

Flow Injection Analysis System (FIAS 100 or FIAS 400)

Flow Injection Analysis Systems (FIAS) is used to inject an exact, reproducible


volume of sample into a continuously flowing liquid carrier stream.

Refer to the section earlier in this manual (Atomizers - Flow Injection Analysis
System) for the full FIAS details.
2-42 System Descriptions

Flame or FIAS Autosampler (AS-90 and AS-91)

In general, an autosampler allows for automated flame and flow injection sampling.
Refer to the section earlier in this chapter for the AS-90 and AS-91 autosampler
details (Autosamplers - Flame or FIAS Autosampler).

Graphite Furnace Autosampler

This autosampler is used in conjunction with the HGA-800 Graphite Furnace. In


general, an autosampler allows for automated flame and flow injection sampling.

Refer to the section earlier in this chapter for the autosampler details (Autosampler
-Graphite Furnace Autosampler).

Quartz Cell Holder (B300-0350)

Required to mount the flame-heated quartz cell of the MHS-10 Mercury/Hydride


System or the FIAS-100 Flow Injection System with the AAnalyst instrument.
(Included with the FIAS-100.)

Electrical Heater Assembly Adapter (N040-1183)

Required to mount the optional Quartz Cell Electrical Heating Assembly for the
FIAS-100 or FIAS-400 on the AAnalyst instrument.

Deuterium Arc Background Corrector

The Deuterium Arc Background Corrector is an internally mounted assembly that


provides simultaneous correction for molecular absorption and light-scattering
(standard feature with the AAnalyst 300). It includes a deuterium arc assembly and
electronics with Automatic Intensity Control. Complete details of this option are
supplied in the section called AAnalyst 300 Instrument Details - Deuterium Arc
Background Corrector. (Requires service installation if not already installed in the
AAnalyst 100.)

The replacement lamp part number is N037-0119.


Options And Upgrades 2-43

The AAnalyst 100 can be ordered with the Deuterium Arc Background
Corrector already installed at the factory. Use the following numbers:
N040-0025 - AAnalyst 100 w\ Background Corrector and Single Mount Lamp
N040-0026 - AAnalyst 100 w\ Background Corrector and Automatic Turret

The AAnalyst 300 is supplied with the Deuterium Arc Background Corrector:
N041-0025 - AAnalyst 300 with Background Corrector and Automatic Turret

Lamp Options

Lamp Adapter Cable (for coded lamps)

Allows the coded Intensitron-series hollow cathode lamps to be used with the
AAnalyst instruments. See the figure below.

Figure 2-20. The Intensitron coded lamp adapter cable.

Lamp Adapter Cable (for non-coded lamps)

Allows non-coded Intensitron-series hollow cathode lamps to be used with


AAnalyst instruments. See the figure below.

Figure 2-21. The Intensitron non-coded lamp adapter cable.


2-44 System Descriptions

Lamp Coding Plugs (for coded EDLs)

Allows coded Electrodeless Discharge Lamps to be used with AAnalyst


instruments. See the figure below.

Figure 2-22. Lamp coding plug for the EDLs.

Burner Head Options

Nitrous Oxide Burner Head, 5-cm (N040-0100)

This burner head is required when using nitrous oxide-acetylene flames for the
determination of refractory metals. It can also be used with air-acetylene flames.

Air-Acetylene Burner Head, 5-cm (N040-0101)

This burner head is designed specifically for air-acetylene operation. It features a


wider slot than the 5-cm nitrous oxide burner head to minimize blockage. It can be
rotated 90°in the AAnalyst 100 and 300.

Air-Acetylene Burner Head, 10-cm (N040-0102)

This 10-cm, single slot burner head is designed specifically for air-acetylene
operation. It comes standard with both the AAnalyst 100 and 300 instruments.

Three-Slot Air-Acetylene Burner Head, 10-cm (N040-0103)

This burner head is used for the analysis of sample solutions with very high
dissolved solids content. It is for use with air-acetylene operation only.
Options And Upgrades 2-45

Computer System Upgrade

As mentioned earlier, the optional computer system controls all the hardware
components and collects, processes, and stores the analytical data. The computer
communicates with the spectrometer, atomization system, and other system
components through an IEEE-488 interface. The computer processes the signals
received from the spectrometer to produce a readout of sample concentration -
among many other things.

The computer system specified by Perkin–Elmer includes the computer, monitor,


keyboard, and mouse. The printer is additional.

AA WinLab Controller Kit (N040-0110)


This upgrade kit is available for those AAnalyst 100 users who are ready to
upgrade from a basic AAnalyst 100 to an automatic system.

The AA WinLab Controller kit includes the following (as of June, 1996):
• AA WinLab Software Kit (N040-0109) which includes;
AA WinLab Install Set Kit - 8 disks (N040-0112)
IEEE Board (0940-1061)
IEEE Cable - 2m (0999-1355)
Keyboard Overlay (B300-0042)
Printer Cable (0941-0001)
Manual, AA WinLab Software Guide (0993-6190)
WinLab Software Installation Instructions (0993-6178)
• a personal computer
• 15-inch SVGA monitor
• LPV World Kit (0940-6045)

Service installation of the system controller is recommended.


2-46 System Descriptions

AA WinLab Software Kit (N040-0109)


This kit is available for those users who already have a personal computer that
meets the minimum computer system configuration (as listed in the NOTE box that
follows). The kit (N040-0109) includes the following equipment:
• AA WinLab Install Set Kit, 8 disks (N040-0112)
• IEEE Board (0940-1061)
• IEEE Cable - 2m (0999-1355)
• Keyboard Overlay (B300-0042)
• Printer Cable (0941-0001)
• Manual, AA WinLab Software Guide (0993-6190)
• WinLab Software Installation Instructions (0993-6178)

NOTE: The Perkin-Elmer software requires the following minimum


computer system configuration:
Intel 80486 processor, 33 MHz, with at least 8 Mbytes RAM;
400 MB hard disk drive; 1.44 Mbytes 3.5"-floppy disk drive;
IEEE-488 interface board; one serial and one parallel port;
and a 640 x 400 x 16 Monitor and SVGA graphics board.

The recommended PC configuration requirements to run the AA WinLab Software


for the AAnalyst instrument follows:
Pentium processor, 75+ MHz, with at least 16 Mbytes RAM;
800+ MB hard disk drive, 1.44 Mbytes 3.5" floppy disk drive;
16-bit AT-GPIB/TNT (IEEE-488) interface board; one serial and one
parallel port; and a 800 x 600 x 256 monitor and SVGA graphics board.

Perkin-Elmer Atomic Absorption Software assemblies are tested and certified for
use with a PE supplied computer with a minimum computer configuration as
described above. Perkin-Elmer cannot warranty the performance of the software
assembly and the corresponding spectrometer with any computer other than those
certified or with certified computers not meeting the minimum configuration
requirements.
Options And Upgrades 2-47

AA WinLab Upgrade Kit (N040-0111)


For those who have the older GEMS software supplied with earlier Perkin-Elmer
instruments, an AA WinLab upgrade kit is available. The kit includes the
following:

• AA WinLab Install Set, 7 disks (N040-0112)


• keyboard overlay (B300-0042)
• Manual, AA WinLab Software Guide (0993-6190)
• WinLab Software Installation Instructions (0993-6178)

Printer Options (and accessories)

There are a number of printers available for those who wish to have a printout of
the data results and the graphs. (Note, information as of July 1996.)

Okidata Microline 320 Printer

The Microline 320 is the only supported printer for use with the AAnalyst 100
instrument without the AA WinLab Controller. The printer is connected directly to
the parallel port of the instrument. The Microline 320 requires a parallel printer
cable (0941-0001) which is included with the controller and software assemblies.
Two models: 0942-1018 115V, 60 Hz and 0942-1019 230V, 60 Hz.

H-P LaserJet IV Printer (0942-1038)

This printer is recommended for producing a hard copy output of your analytical
data. Use this laser printer for a high quality black-and-white output. The LaserJet
IV requires a parallel printer cable (0941-0001) which is included with the
controller and software assemblies. 115 V, 60 Hz.

H-P DeskJet 660C Printer (0942-1082)

This printer is recommended for producing a hard copy output of your analytical
data. Use this printer for full color output of text and graphics. The DeskJet 660C
requires a parallel printer cable (0941-0001) which is included with the controller
and software assemblies. 115 V, 60 Hz.
2-48 System Descriptions

Parallel Printer Cable (0941-0001)

Used to connect the AAnalyst 100 directly to the Okidata Microline 320 printer.
Also used to connect either of the H-P printers to the AAnalyst 300 system
computer. This printer cable is 6 feet long.
Preparing Your
Laboratory 3
Introduction to this Chapter.................................................................................. 3-1
Environmental Requirements ............................................................................... 3-2
Bench Requirements.............................................................................................. 3-2
Lab Space and System Layout ............................................................................. 3-2
Working Area Location .......................................................................................3-4
Exhaust Vent Requirements.................................................................................. 3-5
Blower and Vent Kit ...........................................................................................3-7
Blower Information .............................................................................................3-7
Exhaust Vent Tubing ..........................................................................................3-8
Installing a Venting System ................................................................................ 3-8
Gas Supply Requirements ................................................................................... 3-12
General ............................................................................................................. 3-12
Air Supply Requirements .................................................................................. 3-13
Acetylene Supply Requirements ........................................................................ 3-15
Nitrous Oxide Supply Requirements.................................................................. 3-17
Argon Requirements ......................................................................................... 3-19
Electrical Requirements...................................................................................... 3-20
Cooling Accessories ............................................................................................. 3-21
Preparing Your
Laboratory 3
Introduction to this Chapter

This chapter describes the laboratory requirements for the AAnalyst spectrometer,
including some general information for the accessories available. Before you unpack the
various boxes that comprise the AAnalyst System, be sure that the laboratory has been
prepared according to the instructions in this manual.

The following sections describe the environmental, space, electrical and gas
requirements for your AAnalyst instrument. Make sure your laboratory meets all of
the requirements before the system is installed.
3-2 Preparing Your Laboratory

Environmental Requirements

The LABORATORY in which the instrument is installed should provide all of the
following environmental conditions:
• the laboratory must be indoors
• altitude: 0 to 2 000 meters (sea level to 6,500 feet) (operating)
• ideal operating temperature: between 10 and 35 °C (50-95 °F)
(without specification degradation) with a maximum rate of change of
2.8 °C (5 °F) per hour
• safe operating temperature: will operate safely from 5 - 40 °C (45 - 104 °F)
• relative humidity: between 20 and 80%, non-condensing
• no explosion hazard may exist
• free of dust, smoke, vibration, and corrosive fumes
• bench area out of direct sunlight and
• away from radiators.

The STORAGE AREA in which the instrument is kept (when not in use) should
provide the following environmental conditions:
• temperature range: from -20 to +60 °C (-4 to 140°F)
• altitude: 0 to 12 000 meters (0 to 40,000 feet) (non-operating)

Bench Requirements

The benchtop or area in which the AAnalyst instruments are to be installed should be
large enough to accommodate the instrument and any accessories you’ll be using.

Lab Space and System Layout

The instrument is normally installed on a laboratory work bench or table. The table
should be smooth, level, and free from vibration. The dimensions for each of the
instruments are listed below and shown in the next two figures (3-1 and 3-2). If you
are planning to use the HGA-800 Furnace, the bench will have to be wide enough to
Bench Requirements 3-3

hold both it and the instrument. The furnace dimensions are included in
Figure 3-2. For other accessories, to the manual supplied with the accessory.
The footprint of both instruments is:
Width: 97 cm (38 in.)
Depth: 87 cm (34 in.) (including sample trays)
Height: 51 cm (20 in.)
Weight - AAnalyst 100: 65.3 kg (144 lbs.)
Weight - AAnalyst 300: 68 kg (150 lbs.)

As just pointed out, the instrument itself weighs 65 to 68 kg (144 to 150 lbs.). If you
are considering the use of other accessories, the bench you choose to use should be
able to sustain as much as 300 kg (661 lbs.).
There should be sufficient space on either side of the instrument for the various
accessories. A flame autosampler or flow injection system is ideally placed on a
movable cart in front of the sample compartment to minimize the length of tubing
needed to reach the atomization system. The HGA-800 Furnace is most often used
with the PE Furnace Cooling System. An area needs to be provided for the
Recirculator (see Figure 3-2 for dimensions).

If a computer is connected to the instrument, it may be positioned on the bench next


to the instrument or on a separate computer table in front of the instrument. A suitable
computer worktable is available from Perkin-Elmer (P/N N058-1451).

51 cm
(20 in.)

* Depth indicated
87 cm* allows for sample
97 cm trays and room
(34 in.) for the rear
(38 in.) connectors/cables.

Figure 3-1. Dimensions of the AAnalyst 100.


3-4 Preparing Your Laboratory

Figure 3-2. Dimensions of the AAnalyst 300, HGA-800 Furnace and chiller.

Working Area Location

The bench should be located near the required electricity and gas supplies. Allow
additional power outlets for all your accessories. In addition, an instrument equipped
with a graphite furnace will require an argon supply nearby, a separate 230 volt AC
supply, and cooling water (see the manual supplied with the furnace and the chiller).

The AAnalyst should not be permanently placed against a wall. An area of at least 60
cm (2 ft.) should be available behind the instrument for servicing purposes. Six inches
should be available on each side of the instrument for proper ventilation. If this is not
possible, the bench on which the instrument is placed should be on wheels so that it
can be easily moved.
Exhaust Vent Requirements 3-5

Exhaust Vent Requirements

A venting system is required to remove toxic combustion fumes and vapors from the
flame or graphite furnace (if one is used).
Note that local electrical codes do not permit Perkin-Elmer service engineers to install
the blower and vent assembly.

Exhaust venting is important for the following reasons:


• It will protect laboratory personnel from toxic vapors which may be produced by
some samples.
• It will minimize the effects of room drafts and laboratory atmosphere on flame
stability.
• It will help protect the instrument from corrosive vapors which may originate from
the samples.
• It will remove heat produced by the flame.

Your laboratory must have a reliable exhaust system before you use this
instrument. Without adequate ventilation, potentially toxic vapors can build up in the
laboratory.

Caution It is strongly recommended that the instrument not be placed in a chemical hood.
If a chemical hood must be used, arrangements should be made to prevent
contamination of corrosive vapors and backdrafts from other hoods. Sample
preparation should not be carried out in the same hood with the instrument.
3-6 Preparing Your Laboratory

Using a lab bench 1 meter (36 inches) in height, the exhaust vent system should be 68
cm (27 inches) above the bench and should provide a flow rate of approximately 5400
- 8400 liters/minute (200 - 300 cubic feet/minute).

17cm (7 in.)

68 cm (27 in.)

51cm (20 in.)

91cm (36 in.)

Figure 3-3. Location of exhaust vent (typical both instruments).


Exhaust Vent Requirements 3-7

Blower and Vent Kit

Perkin-Elmer offers an accessory blower and vent kit which will fulfill the exhaust
requirements for all atomic absorption instruments. Included in the kit (see
Table 3-1) are a rotary blower with capacitor and hardware, a vent (or hood) to be
located above the instrument and an adapter to permit connection of the blower and
vent with suitable metal tubing. The metal tubing required to connect the vent to the
blower and to provide suitable exhaust from the blower is not included in the blower
and vent kit. The adapter and vent are made of stainless steel.

Table 3-1. Blower and Vent Kit (P/N 0303-0406)


Part Number Item
0998-0935 Blower Assembly, 115/230 V
0303-1911 Adapter for blower
0303-1910 Exhaust (vent) hood
0996-0922 Capacitor, 2.5 µf
0998-5888 Capacitor hardware
0998-7148 Boot
0990-9701 Instructions

Blower Information

The required capacity of the blower depends on the duct length and the number of
elbows or bends used to install the system. If an excessively long duct system or a
system with many bends is used, a stronger blower may be necessary to provide
sufficient exhaust volume.

The blower should be located at least 4 meters (12 feet) and not more than 6.5 meters
(20 feet) from the flame or the graphite furnace and should exhaust to the atmosphere
or into a considerably wider exhaust duct.

Under the above conditions, the following temperatures have been measured with a
nitrous oxide-acetylene flame: 310 °C at the vent intake; 160 °C (320 °F) at 2.4
meters (8 feet) from the vent intake; 105 °C (221 °F) at the blower intake and
50 °C (122 °F) at the blower motor housing near the front bearing.
3-8 Preparing Your Laboratory

Exhaust Vent Tubing


Always use flexible stainless steel tubing to connect the vent to the blower and to
provide suitable exhaust from the blower. Flexible stainless steel tubing can be
obtained from the companies listed in Table 3-2 and from various other firms. (Do not
use PVC tubing. PVC cannot handle the high temperatures of the flame.)

The required inner diameter of the tubing is 10 cm (4 in.). In some instances this type
of flexible metal tubing is sold only in minimum lengths of 3 meters (10 ft.) .

Alternatively, smooth stainless steel tubing may be used instead of flexible stainless
steel tubing where flexibility is not required (to reduce system friction loss or "drag").
A length of smooth stainless steel ducting has 20-30% less friction loss than a
comparable length of flexible ducting. When smooth stainless steel tubing is used,
elbows must be used to turn corners. These elbows should turn at a center line angle
of 45° to reduce friction losses, and the number of elbows should be minimized. If a
rigid tubing system is used, it is strongly recommended that flexible tubing be used
from the vent hood to the ceiling to facilitate hood alignment and service access to
the instrument.

Table 3-2. Sources of Exhaust Vent Tubing

Flexaust Co. Potomac Rubber Co.


11 Chestnut Street 9011 Hampton Overlook
Amesbury, MA 01913 Capital Heights, MD 20743
(508) 388-9700 (301) 336-7400
Triplex Inc. Fox Manufacturing Inc.
1142 Kress Street P.O. Box 1047
Houston, TX 77020 Clarkdale, AZ 86324
(713) 672-7521 (602) 634-5897
Darcoid Co. of California -
1742 Yosemite Ave.
San Francisco, CA 94124
(415) 861-6984

Installing a Venting System

The dimensions for the various parts of the blower and vent kit are shown in the next
two figures. The vent inner diameter is slightly larger than the tubing outer diameter
Exhaust Vent Requirements 3-9

to allow for tubing tolerances. A slight gap between the two units is
normal.
3-10 Preparing Your Laboratory

Figure 3-4. Dimensions of the exhaust vent.

Figure 3-5. Dimensions of the blower.

When installing a venting system, all connections should be made with metal screws or
rivets. Solder must not be used.
Exhaust Vent Requirements 3-11

Instructions for installation are provided with the blower and vent
assembly. The blower provided in the Perkin-Elmer accessory kit requires a line
voltage of 115V or 230 V. Additional recommendations include:
• Make sure the duct casing is installed using fireproof construction. Route ducts
away from sprinkler heads.
• Locate the discharge outlet as close to the blower as possible. All joints on the
discharge side should be airtight, especially if toxic vapors are being carried.
• Equip the outlet end of the system with a backdraft damper and take the necessary
precautions to keep the exhaust outlet away from open windows or inlet vents and
to extend it above the roof of the building for proper dispersal of the exhaust.
• Equip the exhaust end of the system with an exhaust stack to improve the overall
efficiency of the system.
• Make sure the length of the duct that enters into the blower is a straight length at
least ten times the duct diameter. An elbow entrance into the blower inlet causes a
loss in efficiency.
• Design local exhaust ventilation systems individually for each specific atomic
absorption instrument. Also, the opening of the exhaust vent should be large
enough to cover the graphite furnace or flame area completely.
• Provide make-up air in the same quantity as is exhausted. An "airtight" lab will
cause an efficiency loss in the exhaust system.
• Ensure that the system is drawing properly by releasing smoke into the mouth of
the collector hood (vent). A synthetic "smoke" can be generated by placing open
bottles of hydrochloric acid and ammonium hydroxide in proximity under the
hood.
• Equip the blower with a pilot light located near the instrument to indicate to the
operator when the blower is on.
3-12 Preparing Your Laboratory

Gas Supply Requirements

The permanent installation of gas supplies is the responsibility of the user and should
conform to local safety and building codes. The user must provide the gas supplies,
regulators, connectors, and valves. The AAnalyst instrument includes only the gas
hoses and necessary fittings to connect the instrument to the appropriate gas supplies.

Install gas supplies in accordance with the safety regulations and standards that
apply to your locality, state, and country. Consult the chapter called Safety
Practices in this manual for recommended safety procedures. High pressure gas
cylinders can be dangerous if mishandled or misused.

NOTE: Various regulators, connectors, and valves are available from


Perkin-Elmer as accessories. The part numbers for these items are
given in each of the following sections. The regulators and other items
listed are designed for CGA specified thread standards, which are used
in the U.S. These specifications may differ in other countries. Outside
the U.S., check local standards to determine if these regulators are
suitable for use.

General

Two types of flames are commonly used for atomic absorption flame analyses: air-
acetylene or nitrous oxide-acetylene. Air-acetylene is the preferred flame for the
determination of about 35 elements by atomic absorption. The temperature of the air-
acetylene flame is approximately 2300 °C (4200 °F). For most air-acetylene flames,
the acetylene flow used is about 4 liters per minute (or 0.14 cubic feet/min). Using a
heat combustion value of 1,450 BTU per cubic foot, the heat given off would be
approximately 12,300 BTU per hour.

The nitrous oxide-acetylene flame has a maximum temperature of approximately 2800


°C (5100 °F) and is used for the determination of elements which form refractory
oxides. It is also used to overcome chemical interferences that may occur in flames of
lower temperatures. For the nitrous oxide-acetylene flame, the acetylene flow is about
14 liters/min (or 0.5 cubic feet per min.). Using a heat of combustion value of 1,450
BTU per cubic foot, the heat given off would be approximately 43,000 BTU per hour.
Gas Supply Requirements 3-13

A supply of inert gas is required for external and internal gas streams
through the graphite furnace or as a carrier gas for mercury/hydride systems. Argon is
the recommended inert gas. In some cases, nitrogen can also be used. For more
information, refer to the manual supplied with your furnace, flow injection system, or
mercury/hydride system.

Air Supply Requirements

For the burner system, an air supply that is clean, dry, and oil-free is required. The air
supply should provide a minimum of 28 liters/min (1 cubic foot/min) at a minimum
pressure of 350 kPa (50 psig). The air supply should be suitably filtered to remove oil,
water, and solid particles.

Gas Recommended flow Recommended output pressure


Air minimum 28 liters/min 350 to 450 kPa
(1 cubic foot/min) (50 to 65 psig)

Air Compressor: A small oil-less air compressor meeting the air supply requirements
is available from Perkin-Elmer (see Table 3-3 below). Use of an air dryer filter is
strongly recommended to remove entrained water, oil, water aerosols, and solid
particles from compressed air lines. Water in the air supply can cause severe damage
to the pneumatics.

Caution Use only dry air. Bleed compressor tanks to remove water at least once a week.
Water in the air supply can cause severe damage to the pneumatics.

Air compressors are generally uncomfortably noisy to have in the immediate vicinity
of the instrument. Whenever possible, it is advisable to locate them at some distance
from laboratory workers in an area providing suitable ventilation.

Air Cylinders: Cylinders of compressed air can also be used, but are recommended
only as an emergency or short-term solution. A standard #1 size air cylinder will last
only about five hours. It is common to find other than 20% oxygen in air cylinders.
This can cause erratic burner operation and non-reproducible analytical results and, in
extreme cases, may cause a potential safety hazard.
3-14 Preparing Your Laboratory

In general, if cylinder air is to be used, it is important to specify compressed air rather


than breathing air and that the oxygen content is less than 20%. Never use pure
oxygen.

Never use oxygen as the oxidant gas. Use of oxygen will result in a serious
explosion. If using compressed air in cylinders, be sure that the oxygen content is less
than 20%.

Table 3-3. Accessory items for the air supply


Part Number Item
0303-0264 Air Regulator. Includes CGA No. 590 adapter for regulator to
cylinder connection and 1/4-in. compression fitting for regulator to
hose connection.

0303-0313 Air compressor (115 V)

0303-0314 Air compressor (230 V)

0047-0652 Air Dryer Filter Assembly. Includes a regulator and a second air
hose to use between the air supply and air filter. Instructions are
also included.

0057-0567 Black hose for air or argon (one end of the hose is connected to the
instrument). Includes 1/4-in. compression fittings on both ends.

0990-3898 Connector for joining two air hoses

Instructions to hook up the air supply to the instrument are located in the Installation
chapter.
Gas Supply Requirements 3-15

Acetylene Supply Requirements

Acetylene is used almost exclusively as the fuel for the flames used in atomic
absorption.

The acetylene supply should be of “atomic absorption” or a welding grade (99.6%


pure). The recommended output pressure for the acetylene supply is 83 to 96 kPa (12
to 14 psig).

Gas Recommended output pressure


Acetylene 83 to 96 kPa (12 to 14 psig)

Use an outlet gauge pressure between 83 and 96 kPa (12 and 14 psig) for the
acetylene supply. Never allow the outlet gauge pressure to exceed 103 kPa
(15 psig). At higher pressures, acetylene can decompose with explosive force.

Flash Arrestor: Perkin-Elmer recommends the use of the PE Flash Arrestor (P/N
N930-0068). It provides an extra measure of safety by helping to prevent flashbacks.
The Flash Arrestor provides a positive shut off of gas by checking the reverse flow
under all conditions. It also stops the gas supply when a flashback occurs. The flash
arrestor can be directly connected to the acetylene fuel line.

Grade: Suitable acetylene typically has a minimum purity specification of 99.6% with
the actual assay being about 99.8%. Acetylene is supplied dissolved in acetone to
prevent explosive decomposition. You should not use acetylene that is dissolved in any
other solvent. Experience indicates that solvents can be carried through the regulator
with the acetylene and can weaken, to the point of rupture, the walls of the tubing
carrying the acetylene to the burner, causing a potential hazard.

Cylinder Specifications: A size 1A acetylene cylinder contains about 8,500 liters


(300 cubic feet) of acetylene and usually lasts about 30 hours of burning time with an
air-acetylene flame. With a nitrous oxide-acetylene flame, the same size cylinder will
last about 10 hours.

Piping/Tubing/Fittings: Use galvanized iron, steel, or wrought iron tubing. Never use
copper tubing with acetylene. Joints may be welded or made up of threaded or flanged
3-16 Preparing Your Laboratory

fittings, typically stainless steel or aluminum, or brass composed of less than 65%
copper. Rolled, forged, or cast steel or malleable iron fittings may also be used. Cast
iron fittings can not be used safely for acetylene lines.

Never use copper tubing or fittings for acetylene gas lines. Acetylene can react with
copper to form a readily explosive compound.

Table 3-4 lists available accessories for your acetylene supply.

Table 3-4. Accessory items for the acetylene supply.


Part Number Item
0303-0106 Acetylene Regulator. Includes CGA No. 510 or CGA No. 300
adapters for regulator connection to cylinder, and includes 0990-
3031 outlet bushing for the regulator to hose connection.
0057-0559 Red fuel hose with 3/8-in. left-hand thread for additional gas
supply connection (one end of the hose is already connected to the
instrument). Connection to regulator: 9/16" left-hand thread.
0990-3196 Female adapter (1/4-in. male compression fitting to 1/4-in. pipe)
for connecting the regulator to the outlet bushing (not required on
all installations).
0990-3031 Outlet bushing (1/4-in. pipe to 9/16-in. left hand thread) for
connection from regulator to the AAnalyst gas hose.
0990-3032 Connector for joining two fuel hoses.
0930-0068 Flash Arrestor

Instructions to hook up the acetylene supply to the instrument are located in the
Installation chapter.
Gas Supply Requirements 3-17

Nitrous Oxide Supply Requirements

Nitrous oxide is the recommended oxidant for slightly less than half of the elements
determined using atomic absorption.

The nitrous oxide supply should be at least 99% pure. A heated regulator providing an
output pressure of 345 to 520 kPa (50 to 75 psig) is recommended.

Gas Recommended output pressure


Nitrous oxide 345 to 520 kPa (50 to 75 psig)

Cylinder Specifications: Cylinders of nitrous oxide (99.0% minimum purity) are


available from local suppliers and usually require a CGA 320 connection.

Nitrous oxide is supplied in the liquid state, initially at a pressure of about 5000 kPa
(750 psig). A size 1A cylinder of nitrous oxide contains about 14,800 liters (520 cubic
feet) and will typically last for 10 to 12 hours of burning time.

• Store nitrous oxide cylinders in a well-ventilated area outside the laboratory.


Nitrous oxide is an asphyxiant; it can be considered a potential hazard
whenever it is stored or used in a confined space.
• Do not store nitrous oxide cylinders in close proximity to flammable gases
(e.g., acetylene).
• Make sure tubing and fittings carrying nitrous oxide are free of grease, oil, or
other organic material. Spontaneous combustion may occur if nitrous oxide
comes into contact with these materials.

Heated Regulator: Since the nitrous oxide is in liquid form, the pressure gauge does
not give a true indication of how much nitrous oxide remains in the cylinder until the
pressure starts to fall rapidly as the residual gas is drawn off. When nitrous oxide is
rapidly removed from the cylinder, the expanding gas causes cooling of the cylinder
pressure regulator and the regulator diaphragm can freeze. This can create erratic
flame conditions or, in the most extreme case, a flashback.

It is therefore advisable to use a regulator with a built-in heater. A heated nitrous


oxide pressure regulator is available from Perkin-Elmer (see Table 3-5).
3-18 Preparing Your Laboratory

Table 3-5. Accessory items for the nitrous oxide supply.


Part Number Item
0303-0204 Nitrous oxide regulator with electric heater,
115 V. Includes male connector 0990-3946 described below.
0303-0349 Nitrous oxide regulator with electric heater,
230 V. Includes male connector 0990-3946 described below.
0990-3946 Male compression fitting connector (1/4-in. to 5/16-in.) for
connection from regulator to gas hose.
0047-0258 Blue nitrous oxide gas hose with 5/16-in. compression fitting at
each end for additional gas supply connection (one end of the
hose is already connected to the instrument).
0992-0223 Connector for joining two nitrous oxide gas hoses.

Instructions to hook up the nitrous oxide supply to the instrument are located in the
Installation chapter.

NOTE: If you are not going to use the nitrous oxide gas supply,
leave the cap plug fitting on the end of the N2O hose (P/N 0992-
0165).
Gas Supply Requirements 3-19

Argon Requirements

A supply of inert gas is required for external and internal gas streams through the
graphite furnace or as a carrier gas with mercury/hydride systems. A supply of argon
meeting the purity criteria listed in the following table is recommended for these
applications.

Table 3-6. Argon purity requirements.


Gas Specified Concentration
Argon > 99.996%
Oxygen < 5 ppm
Nitrogen < 20 ppm
Water < 4 ppm

Normally, for the graphite furnace, gaseous argon is used, although either liquid or
gaseous argon can be used. The choice of liquid or gaseous argon is determined
primarily by the availability of each and the usage rate.

Liquid argon is usually less expensive per unit volume to purchase but cannot be
stored for extended periods. If liquid argon is used, the tank should be fitted with an
over-pressure regulator which will vent the tank as necessary in order to keep the
liquid argon cool enough to remain in the liquid state.

Gaseous argon tanks do not require venting and consequently can be stored for
extended periods without loss.

Table 3-7. Accessory items for argon supply.

Part Number Item


0303-0284 Argon regulator. Regulator connection to cylinder: CGA 580.
Includes female adapter 0990-3196 described below.
0057-0567 Black gas hose for air or argon. Has 1/4-in. compression fittings
on both ends.
0990-3196 1/4-in. female adapter (1/4-in pipe to 1/4-in. male compression
fitting) for connecting the regulator end fitting to an argon hose.
0990-3898 Connector for joining two air/argon hoses.
3-20 Preparing Your Laboratory

Electrical Requirements

Both AAnalyst instruments require a grounded AC outlet providing voltage


corresponding to the voltage selected on the instrument:
• 100 VAC ±10% @ 50 Hz ±1% or @ 60 Hz ± 1%
• 120 VAC ±10% @ 50 Hz ±1% or @ 60 Hz ± 1%
• 220 VAC ±10% @ 50 Hz ±1% or @ 60 Hz ± 1%
• 230 VAC ±10% @ 50 Hz ±1% or @ 60 Hz ± 1%
• 240 VAC +6% / -10% @ 50 Hz ±1% or @ 60 Hz ± 1%
Power Consumption: 248 VOLT-AMPS maximum for the spectrometer.

Grounding circuit continuity is vital for safe operation of equipment. Never


operate equipment with grounding conductor disconnected.

In addition, the electrical supply should be free of line transients in excess of 50V
peak. If the electrical supply voltage produces large AC line voltage fluctuations,
install a voltage regulator between the AC outlet and the instrument.

All instruments are shipped configured for 220 volts AC operation, 50 or 60 Hz. If the
voltage marked on the instrument does not match your AC line voltage, change the
instrument operating voltage as described later in this manual in the Installation
chapter, in the section called Connecting the Electrical Supply - Changing the
Instrument Operating Voltage.

One standard outlet is required for the instrument. The PC and any other accessories
require separate outlets. A.C. power outlets with appropriate current ratings for the
instrumentation being installed are to be specified according to local electrical code.

Accessories such as the flow injection system and flame autosamplers also use one of
the above electrical supplies. The graphite furnace module has special electrical
requirements (220V). For more information, refer to the manual supplied with each
accessory.
Cooling Accessories 3-21

Cooling Accessories
When doing Furnace Analysis, the HGA-800 Furnace is part of the system. The
furnace needs to be water-cooled using tap water or a water cooling system to
maintain it at a specified temperature and to cool it between analyses. Perkin-Elmer
recommends a regulated source of filtered water for the purpose of cooling. A
recirculator (or chiller) is shown with dimensions below. The picture is a reprint of
Figure 3-2 shown earlier.

The water supply should meet the following specs:


• sediment and hardness free
• pH: between 6.5 and 7.5
• flow rate: minimum of ≥2 L/min.
• temperature: ≥20°C
• operating pressure: between ≥2.5 bar and ≥4.5 bar
HGA 800 AAnalyst 300

20.5cm
Depth: (8 in.)
51cm
(20 in.) P-E Furnace
Cooling System
35cm Recirculator
(13.75 in.)

Figure 3-6. The PE cooling system recirculator attached to the HGA-800.


Installation 4
Introduction to this Chapter.................................................................................. 4-1
Installation Summary: AAnalyst 100 .................................................................... 4-2
Inspecting the Shipment ........................................................................................ 4-3
Unpacking the AAnalyst 100 Instrument.............................................................. 4-3
Instrument Part Numbers .................................................................................... 4-3
How to Unpack the Instrument ............................................................................ 4-4
Carton Recycling Instructions ............................................................................. 4-6
Shipping Lists ..................................................................................................... 4-8
Spares Kits........................................................................................................ 4-10
Who to Call? ..................................................................................................... 4-12
Assembling the AAnalyst 100.............................................................................. 4-12
Place Instrument on the Bench .......................................................................... 4-12
Assembly Overview, What’s Next? ................................................................... 4-13
Assembling the Quick-Change Burner Mount Assembly ................................... 4-15
Installing the Nebulizer on the Burner .......................................................... 4-15
Checking that the Burner End Cap is Secure ................................................. 4-18
Connecting and Securing the Gas Hoses to the Burner .................................. 4-19
Installing and Securing the Burner Head ....................................................... 4-21
Checking that the Ignitor Box Connectors are Plugged In ............................. 4-22
Installing the Quick-Change Burner Mount Assembly ....................................... 4-23
Plugging in the Main Interlock Connector ......................................................... 4-24
Installing the Burner Drain System ................................................................... 4-25
Connecting the Burner Drain System ............................................................ 4-25
Adding Water to the Drain Float Assembly ................................................... 4-27
4-2 Installation

Installing the Burner Door ................................................................................ 4-28


Installing the Lamp Compartment Cover .......................................................... 4-29
Installing the Sample Trays ............................................................................... 4-30
Installing the Lamp(s) ....................................................................................... 4-31
Setting Up the EDL Power Supply .................................................................... 4-50
Connecting the Gas Supplies............................................................................... 4-52
Connecting to the Air Supply ............................................................................ 4-53
Requirements................................................................................................ 4-53
Air Compressor Setup ................................................................................... 4-53
Air Cylinder Setup ........................................................................................ 4-54
Connecting to the Acetylene Supply .................................................................. 4-55
Requirements................................................................................................ 4-55
Acetylene Warnings ...................................................................................... 4-55
Air/Acetylene Filter Assembly Setup............................................................. 4-55
Recommended Acetylene Supply Setup......................................................... 4-56
Connecting to the Nitrous Oxide Supply ........................................................... 4-57
Requirements................................................................................................ 4-57
Recommended Nitrous Oxide Supply Setup .................................................. 4-57
Connecting to the Argon Supply ....................................................................... 4-58
Requirements................................................................................................ 4-58
Recommended Argon Supply Setup .............................................................. 4-59
Connecting the Electrical Supply........................................................................ 4-60
A Review of the Electrical Specifications .......................................................... 4-60
How to Find Out the Instrument Voltage Setting ............................................... 4-61
If You Have 220 VAC in Your Lab ................................................................... 4-62
Changing the Instrument Operating Voltage ..................................................... 4-62
Changing a Fuse ............................................................................................... 4-64
Changing the Setting on the Voltage Selector Board ......................................... 4-65
Installing the AC Line Cord .............................................................................. 4-66
Setting Up the Okidata 320 Printer .................................................................... 4-68
Powering Up the Instrument ............................................................................... 4-73
Post Installation Adjustments and Checks.......................................................... 4-74
Aligning the Lamp(s) ........................................................................................ 4-74
Adjusting the Burner Height ............................................................................. 4-75
Adjusting the Gas Flows for Ignition ................................................................. 4-77
Igniting the Flame ............................................................................................. 4-79
Adjusting the Burner Position ........................................................................... 4-79
Adjusting the Nebulizer .................................................................................... 4-80
Sample Introduction System Pre-Conditioning .................................................. 4-81
Checking the Nitrous Oxide Flame (for Nitrous Oxide-Acetylene Analysis) ...... 4-82
Installation 4
Introduction to this Chapter
This chapter includes all the information you will need to completely install your
new AAnalyst 100 System. Make sure you perform the installation procedures in
the order in which they are presented.

NOTE: Service installation of the AAnalyst 300 is


required. Contact Perkin-Elmer for installation.
4-2 Installation

Installation Summary: AAnalyst 100


The complete AAnalyst 100 installation process consists of the following steps.
The steps are listed here and described through-out this chapter.

Inspecting the shipment


Unpacking the AAnalyst 100 Instrument
Assembling the AAnalyst 100
Assembling the quick-change burner mount assembly
Installing the nebulizer on the burner
Checking that the burner end cap is secure
Connecting and securing the gas hoses to the burner
Installing and securing the burner head
Checking that the ignitor box connectors are plugged in
Installing the Quick-Change Burner Mount Assembly
Plugging in the Main Interlock Connector
Installing the Burner Drain System
Installing the Burner Door
Installing the Lamp Compartment Cover
Installing the Sample Trays
Installing the Lamp(s)
Connecting the gas supplies
Connecting the electrical supply
Setting up the printer
Powering up the instrument
Post-installation adjustments and checks
Inspecting the Shipment 4-3

Inspecting the Shipment


Upon receipt of the instrument, the exterior of all the shipping cartons should be
inspected. All cartons should arrive unopened and undamaged. If the examination
reveals that damage has occurred in shipment, notify the carrier and Perkin-Elmer
immediately. A representative of the shipping carrier must be present for insurance
purposes.

Unpacking the AAnalyst 100 Instrument


Carefully read these instructions before you unpack the AAnalyst instrument to
avoid damaging the instrument. The AAnalyst 100 is shipped in a single carton.
The carton contains the instrument in the lower portion of the box with an inner
“tray” designed to hold items in the upper portion of the box. For example, the
burner assembly is located in a bag, in a box, and packed securely in the inner tray.
The drain bottle assembly, instrument documentation, spares kit and various other
parts are also located and packed securely in the inner tray.

There may be other cartons, too, depending on what options you chose to use with
the AAnalyst 100.

Note that the shipping carton is recyclable. See the section later in this document.

Instrument Part Numbers


There are three versions of the AAnalyst 100 system, each assembled with different
options. There is one version of the AAnalyst 300. The various models are listed:

Background Automatic
Instrument Part No. Corrector Six-Lamp Turret
AAnalyst 100 N040-0027 - -
AAnalyst 100 N040-0025 Yes -
AAnalyst 100 N040-0026 Yes Yes
AAnalyst 300 N041-0025 Yes Yes
4-4 Installation

How to Unpack the Instrument


1. Place the instrument carton on the floor in front of the bench in which the
instrument will be placed.
2. Cut the two bands that hold the carton together, lift off the top of the carton.
3. There is an inner tray on top of the instrument that holds the various parts of
the instrument in separate boxes. Empty the contents of the inner tray.

Figure 4-1. An exploded view of the shipping carton.

4. Remove the inner tray of the carton and set it aside.


Unpacking the AAnalyst 100 Instrument 4-5

5. Pull out the two foam pieces that secure the instrument in the box.
6. Lift up and remove the carton sleeve (the sides of the box).
7. Next remove the protective wrapping around the instrument (not shown).
8. Prepare to lift the instrument out of the carton. You will need two people to do
this. The bench should be nearby.

The instrument weighs from 65 - 68 kg (144-150 lbs.). Use proper lifting


posture when lifting the instrument out of the carton. Be aware that most of the
weight is located at the right front corner of the instrument. It will want to tip
forward when it is lifted out of the carton, so be prepared to support that corner.

Figure 4-2. Lifting the instrument out of the box.


4-6 Installation

9. Position a person on each side of the instrument as shown. Squat down and
place both hands underneath the instrument - palms up. Spread your hands as
far apart as possible (against the foam corners) while grasping the underside of
the instrument.
10. With knees bent, simultaneously lift the instrument out of the carton as you end
up in a standing position. Carefully place the instrument on the bench.
11. If you have the instrument with a six-position lamp turret, you must next
remove the two wedges of foam located around the turret (inside the lamp
compartment on the right side of the instrument, not shown).

Carton Recycling Instructions


The instrument carton was designed in such a manor that it folds up considerably
smaller for easy storage. You can either store the compact carton for future use (to
transport the instrument), recycle it by returning it to Perkin-Elmer, or break it
down completely and give it to your local recycling center.

To collapse and store the carton, follow these instructions and refer to the next
figure.
Unpacking the AAnalyst 100 Instrument 4-7

Figure 4-3. Breaking down the shipping carton for storage.


1. Place the two foam pieces in the carton base as shown in the figure above.

2. Collapse the sides of the carton that made up the carton sleeve.

3. Place the inner tray upside down around the four foam corners in the base.

4. Lay the collapsed sleeve on top of the inverted inner tray.

5. Place the carton top over the entire assembly. You may want to secure the
carton by wrapping plastic or metal bands around the carton to hold it together.

6. Store this compact carton in a safe place for possible future use. If desired, the
carton may be returned to Perkin-Elmer for recycling (you must band it). If you
do send the carton back and in the future you find that the instrument needs to
be shipped to a new installation sight, contact Perkin-Elmer for another carton.
4-8 Installation

Shipping Lists
The following items are included in the AAnalyst 100 shipment.

Description

AAnalyst 100 Instrument

Burner Assembly (in a box)

Drain Assembly (including the drain vessel)

Spares Kit (including manuals)

Burner Door

Nebulizer Assembly
Unpacking the AAnalyst 100 Instrument 4-9

The following items are included in the AAnalyst 300 shipment:

Description

AAnalyst 300 Instrument

Burner Assembly (in a box)

Drain Assembly (including the drain vessel)

Spares Kit (including manuals)

Burner Door

Nebulizer Assembly
4-10 Installation

Spares Kits
The following items are included in the AAnalyst 100 Spares Kit
(P/N N040-0099). The kit is shipped with the instrument.

Part Number Part Name QTY


0303-0477 Recorder Cable Assembly 1
0303-1573 N2O Burner Head Cleaner 1
0900-2219 O-Ring, Burner Head 1
(B004-7207) 0.984 ID 0.139 WD
0990-2147 O-Ring, End Cap (rubber) 1
1.862 I.D. 0.103 WD
0047-2014 Gasket, End Cap (cork) 5
0990-3031 Adapter, Outlet Bushing 1/4 NPT Male 1
0990-8265 Clear Polyeth Tubing 0.023 ID 1
0990-3004 Hose Clamp 1/4 - 5/8 SST 2
0998-1761 Fuse, Slow Blow 3AG 6.25A 250V 1
0999-1675 Fuse, Metric Slow Blow 3.15A 250V 2
N040-1043 Molding, Sample Tray (Right) 1
N040-1169 Molding, Sample Tray (Left) 1
0303-0152 Analyst Methods for AA 1
0993-6088 AAnalyst 100/300 Hardware Guide 1
0993-9533 AA Concepts Manual 1
0990-9390 AA Newsletter Subscription Form 1
0993-6149 AAnalyst 100 User’s Guide 1
0993-6175 AAnalyst 100 Installation Guide 1
N041-1063 AAnalyst 100 Param Entry Index 1
Unpacking the AAnalyst 100 Instrument 4-11

The following items are included in the AAnalyst 300 Spares Kit
(P/N N041-0099). The kit is shipped with the instrument.

Part Number Part Name QTY


0303-0477 Recorder Cable Assembly 1
0303-1573 N2O Burner Head Cleaner 1
0900-2219 O-Ring, Burner Head 1
(B004-7207) 0.984 ID 0.139 WD
0990-2147 O-Ring, End Cap (rubber) 1
1.862 I.D. 0.103 WD
0047-2014 Gasket, End Cap (cork) 5
0990-3031 Adapter, Outlet Bushing 1/4 NPT Male 1
0990-8265 Clear Polyeth Tubing 0.023 ID 1
0990-3004 Hose Clamp 1/4 - 5/8 SST 2
0998-1761 Fuse, Slow Blow 3AG 6.25A 250V 1
0999-1675 Fuse, Metric Slow Blow 3.15A 250V 2
N040-1043 Molding, Sample Tray Right 1
N040-1169 Molding, Sample Tray Left 1
0303-0152 Analyst Methods for AA 1
0993-6088 AAnalyst 100/300 Hardware Guide 1
0993-9533 AA Concepts Manual 1
0990-9390 AA Newsletter Subscription Form 1
4-12 Installation

Who to Call?
SUPPLIES, ACCESSORIES, AND REPLACEMENT PARTS can be ordered
directly from Perkin-Elmer. Perkin-Elmer offers a full selection of high-quality
atomic spectroscopy supplies through the Atomic Spectroscopy Supplies Catalog.
For further information, please contact your local Perkin-Elmer representative.

Assembling the AAnalyst 100

NOTE: Service installation of the AAnalyst 300 is


required. Contact Perkin-Elmer for installation.

This section describes how to assemble the AAnalyst 100. The AAnalyst 100 is
designed to be installed by the user, if s/he decides to do so. The basic instrument
comes pre-assembled, minus the burner and drain assemblies. Be sure to perform
the assembly procedures in the order in which they are presented.

Place Instrument on the Bench


By this time, you should have inspected and unpacked all the boxes in the
shipment. The instrument should be in the laboratory and on the bench in which it
will be used. Make sure you have read and complied with all the information in
the Preparing Your Laboratory chapter of this manual before you continue.
Assembling the AAnalyst 100 4-13

Assembly Overview, What’


s Next?
Locate the “quick-change” burner mount assembly in the upper tray of the shipping
carton (pictured next). Unpack it (if not already done). Place the assembly on a
bench. Next you will assemble parts to it.

Figure 4-4. The quick-change burner mount assembly.


4-14 Installation

The next few sections describe the steps necessary to prepare the quick-change
burner mount assembly for installation into the instrument:

• installing the nebulizer on the burner


• check that the burner end cap is secure
• connecting and securing the gas hoses to the burner
• installing and securing the burner head
• checking that the ignitor box connectors are plugged in

Again, be sure to perform the procedures in the order in which they appear.

After the burner is completely assembled and checked on the bench, the entire
quick-change burner mount assembly will be installed into the instrument. Then,
various hoses and connectors will be attached, including the burner drain system.
Next, the burner door, the lamp compartment cover, the sample trays and the
instrument lamp(s) will be assembled to the instrument. Then you will hook up to
the gas supplies. The electrical supply is next to be hooked up. At this point, if
necessary, the instrument voltage setting will be changed to match the voltage
supply in your lab. Last to set up is the optional printer. Assembly of a basic
AAnalyst 100 will then be complete.

Finally, after the instrument is assembled, you are ready to power it up. At this
point, some post-installation adjustments and checks are performed.

When all the above procedures just described are done, the AAnalyst 100
installation will be complete.
Assembling the AAnalyst 100 4-15

Assembling the Quick-Change Burner Mount Assembly


Before the burner assembly can be put into the instrument, a few items need to be
added or checked. The following sections give full procedures to do so.

Installing the Nebulizer on the Burner


Refer to Figure 4-5 and install the nebulizer onto the burner end cap.

Burner Chamber

Burner End Cap

Nebulizer Clamp

O-rings
Nebulizer

Side Arm Slot


Nebulizer Side Arm
Ridges
Plastic Nut

Nebulizer Oxidant Tubing

Capillary Tubing

Figure 4-5. Installing the nebulizer onto the burner end cap.
4-16 Installation

1. Feed at least 6-8 inches of capillary tubing onto the nebulizer inlet.
2. Lightly lubricate the nebulizer o-rings with the Apiezon grease supplied in the
nebulizer kit.
3. Locate the nebulizer clamp (Figure 4-6, Detail A) and slide it up while
inserting the nebulizer into the burner end cap. Be sure to orient the nebulizer
side arm so that it will lay in the slot provided. (A gentle twisting and pushing
motion might be necessary to fully seat the nebulizer in the burner end cap.)
4. Lower the nebulizer clamp until it presses against the barrel and flange of the
nebulizer (shaded area). Ensure that the nebulizer is pushed in all the way and
clamped in correctly. Warning, the nebulizer clamp must be lowered and
locked OVER the nebulizer flange. Figure 4-6, Detail B, shows the clamp
lowered and locked correctly over the nebulizer flange.

Figure 4-6. Nebulizer clamp securing the nebulizer flange in place.


Assembling the AAnalyst 100 4-17

5. Next you’ll connect the nebulizer oxidant hose to the nebulizer side arm.
Remove the plastic nut from the nebulizer side arm. Slide the nut on the end of
the hose hanging free on the burner base (hose shown in Figure 4-4). The hose
has white tape on it printed with the word “NEB.”
6. Slide the NEB oxidant tubing onto the ridges on the nebulizer side arm (Figure
4-5).
7. Using the Apiezon grease, lightly lubricate the OUTSIDE of the tubing where
the nut will screw onto the nebulizer ridges.
8. Finally, slide the plastic nut up the black tubing and gently thread it over the
ridges on the side arm. Tighten the plastic nut just finger tight. The nebulizer is
now assembled in place and secure.
4-18 Installation

Checking that the Burner End Cap is Secure


The burner end cap is assembled to the burner chamber at the factory. It is always
a good idea to confirm that the screws are tight. To do so, hand-tighten (in an
alternating pattern) the four knurled screws holding the burner end cap to the
burner chamber. Tightening them in an alternating pattern (diagonally opposite
nuts) will allow the o-ring to form a good seal. See the figure below for the location
of the four knurled screws. Tighten them only hand tight.

Burner Chamber

Burner End Cap

Knurled Screws
(typical 4 places)

Figure 4-7. Checking that the burner end cap is secure.


Assembling the AAnalyst 100 4-19

Connecting and Securing the Gas Hoses to the Burner


There are three gas hoses that are connected to the end cap on the burner assembly:
the nebulizer oxidant hose, the auxiliary oxidant hose, and the fuel hose. They are
pointed out in the next figure. At this point, all three hoses should already be
connected to the burner. If they are not, do so now. The next few paragraphs
discuss how to check them.

Nebulizer Clamp
Burner End Cap
Nebulizer
Auxiliary
Oxidant Hose Nebulizer Side Arm

Connector Nut

Nebulizer
Compression Fittings Oxidant Hose

Fuel Hose

Figure 4-8. Securing the gas hoses to the burner end cap.

The first hose is the nebulizer oxidant hose (also called the NEB). It is connected
right after the nebulizer is installed. If it is not already connected, do so now.
Follow steps 5- 8 in the section called Assembling the Quick-Change Burner
Mount Assembly - Installing the Nebulizer on the Burner.

The second gas hose is referred to as the auxiliary oxidant hose (AUX). It is the
other “clear” hose coming up from under the burner mounting plate and attached to
the burner end cap. The hose is connected at the factory. Confirm that it is
connected and that the compression fitting is tight. If it is not, do the following:

PROCEDURE: Tighten the compression fitting hand tight plus a 1/4 turn using
two wrenches: one wrench to hold the nebulizer fitting and the other to turn the
compression fitting.
4-20 Installation

The third hose connected to the burner is the fuel hose. It is the “clear” tubing
attached to the burner end cap. (Refer to Figure 4-8.) That hose, too, is connected
at the factory. Confirm that it is connected and that the compression fitting is tight.
If it is not, tighten it using the procedure that follows:

PROCEDURE: Tighten the compression fitting hand tight plus a 1/4 turn using
two wrenches: one wrench to hold the nebulizer fitting and the other to turn the
compression fitting.
Assembling the AAnalyst 100 4-21

Installing and Securing the Burner Head


The burner head is shipped from the factory already attached to the burner
assembly (10 cm air/acetylene N040-0102). If it was removed or you need to
change it, follow these instructions to put it back on. Make sure the magnetic strip
is facing the ignitor box. You must also confirm that the burner head safety latch is
positioned above the burner head ring. This procedure will make sure the safety
latch is correctly positioned over the burner head ring.

Figure 4-9. Confirm that the burner head is in place and latched securely.

1. Press the tab on the safety latch while lowering the burner head into place
inside the o-ring (see figure above).
2. Confirm that the magnetic strip on the burner head ring is positioned around
back and “facing” the ignitor box. (See the left-most drawing above.)
3. Make sure to completely seat the burner head onto the chamber by gently
pushing and twisting the burner head into the chamber. (See the right-most
drawing above.) You will know that the burner head is fully seated because
the ignitor will swing over the burner.
4. Let go of the safety latch. Look at it closely to confirm that the safety latch
“hook” is positioned over the ring.
4-22 Installation

Checking that the Ignitor Box Connectors are Plugged In


There are five interlock “sensors” in the instrument: 1) burner head, 2) flame
sensor, 3) nebulizer, 4) drain, and 5) sample compartment thermal shield. The first
three route through the ignitor box. All but one of them are finally routed through
a large connector mounted on the sample compartment wall. If the main interlock
connector or the sensors are disconnected, the AAnalyst won’t ignite.

Refer to the next figure. Locate the three sensor wire connectors inside the rear of
the Ignitor Box Assembly. Confirm that all three connectors are plugged into the
PC Board. Note that the drain interlock sensor will be checked after the drain is
hooked up. The thermal shield interlock sensor has no access. The main interlock
connector will be plugged in after the burner is installed.

Rear View of the


Ignitor Box Assembly

3 Connectors
to be Plugged In

Ignitor Box
PC Board

Figure 4-10. Rear view of the ignitor box assembly.


Assembling the AAnalyst 100 4-23

Installing the Quick-Change Burner Mount Assembly


The previous group of procedures prepared the burner assembly for mounting into
the instrument. The mounting instructions are next. Refer to the next figure.

(Rear of
Sample Compartment)

Tracks (1of 2)
Quick-Disconnect
Release Plate
(Interlock Connector, ref)

Fittings (1 of 3)

Quick Change
Burner Mount Assembly

Figure 4-11. Installing the “quick-change” burner mount assembly.


1. Orient the assembly to slide into the tracks as shown in the figure above.
2. Slide the assembly (along the tracks) into place in front of the instrument.
When the assembly is pushed all the way in, you will hear a “clicking” sound
as the three fittings seat themselves and lock into the back of the sample
compartment.
4-24 Installation

Plugging in the Main Interlock Connector

(Rear of
Sample
Compartment)

Socket

Quick-Disconnect Release Plate


Clear Rubber Button
Main Interlock Connector
Mechanical Interlock Knob

Quick-Change Burner Mount Assembly

Figure 4-12. Plugging in the main interlock connector.

1. Once the quick-change burner mount assembly is in place (previous


procedure), grasp the body of the main interlock connector with your right
hand and place your thumb on the “clear rubber button.”
2. Next, plug the main interlock connector into the socket on the back wall of the
sample compartment. You must push it in until the connector mechanically
snaps into place. While doing so, use the interlock connector body to press
down on the mechanical interlock knob. When the interlock connector is
completely plugged into the socket (by pressing down on the mechanical
interlock knob), the burner assembly will be locked in place.
Assembling the AAnalyst 100 4-25

Installing the Burner Drain System


Locate and unpack the drain system from the upper tray of the shipping carton. It
includes all of the parts marked in Figure 4-13.

Connecting the Burner Drain System


1. Refer to the next figure when installing the drain system. Position the drain
vessel on the floor underneath the front of the instrument and attach the retainer
cap assembly (cap, trap and loop) to the drain vessel.
2. Hold up the free end of the drain tubing and pour approximately 250 mL of
water into it until you hear the water start to drip into the vessel.

Retainer
Cap

Drain
Trap
Switch
Assembly

Drain
Spiral Wrap Loop

Drain Interlock
Connector
Interlock Cable
Drain Tubing

Drain
Vessel

Figure 4-13. Installing the burner drain system.


4-26 Installation

3. Refer to the detailed figure below. Now attach the free end of the drain tubing
to the drain outlet on the burner end cap. Hand tighten the drain clamp.

Burner End Cap Burner Assembly

Drain
Outlet
Drain Clamp

Drain
Tubing Drain
Interlock
Plug
Spiral Drain
Wrap Interlock
Connector
Drain
Interlock
Cable

Figure 4-14. Connecting the drain tubing and drain interlock cable.

4. Finally, you need to connect the drain interlock cable. Plug the drain interlock
connector into the drain interlock plug located on the burner assembly as
shown above.
Assembling the AAnalyst 100 4-27

Adding Water to the Drain Float Assembly


Enough water must be present in the drain system to fill the drain loop and to
activate the drain float assembly. If not, carry out the following procedure:

1. Loosen the drain clamp and remove the drain tubing from the drain outlet on
the burner end cap (see Figure 4-14 above).
2. Pour about 250 mL of water into the drain tubing.
3. Reconnect the drain tubing to the burner end cap. Replace the drain clamp and
tighten securely. Installation of the burner drain is complete.
4-28 Installation

Installing the Burner Door


Locate the burner door (packed separately). Refer to the figure below when
installing the door.

Figure 4-15. Installing the burner door.

1. Hold the door in place next to the burner compartment shown in Figure 4-15.
2. Swing the door to the open position. Tilt the top of the door away from the
upper door pin while you push the lower pin up into the hole in the door mount.
3. Drop the top pin down into the upper hole in the door mount while holding the
bottom pin in place. Swing the door while letting it drop down and lock into
place on the hinges.
4. Close the door. Installation is complete.
Assembling the AAnalyst 100 4-29

Installing the Lamp Compartment Cover


Locate the lamp compartment cover (if it is not already on the instrument). Install
the cover by following the procedures below.

Figure 4-16. Installing the lamp compartment cover.

1. Hold the cover in the up position shown above (left) in front of the instrument.
2. With the cover in the up position, line up the holes in the cover with the hinge
pins on the instrument.
3. Slide the cover to the left over the pins until it hits the stops.
4. Lower the cover into place on the lamp compartment. Installation is complete.
4-30 Installation

Installing the Sample Trays


Locate the two sample trays and unpack them (if not yet done). Install them by
following the procedures below.

1. Hold the tray with both hands in the position shown in front of the instrument.

Sample Tray

Sample Tray

Figure 4-17. Installing the sample trays onto the front of the AAnalyst.

2. Tilt the tray mounting posts downward on a slight angle as you insert them into
the slots in the front of the instrument.
3. Slide the tray all the way into the front of the instrument base until it hits the
stop. At that point, gently push the tray edge downward to secure it into place.
You’ll feel it lock into place.
4. Repeat the above steps for the second tray. Tray installation is complete.
Assembling the AAnalyst 100 4-31

Installing the Lamp(s)


There are a number of different lamps that can be used with the AAnalyst 100: the
Lumina Hollow Cathode Lamp (HCL); the Intensitron Hollow Cathode Lamp
(coded and non-coded); and the Electrodeless Discharge Lamp (EDL) (coded and
non-coded). The variety exists because many labs are currently using these lamps
in their other Perkin-Elmer AA instruments. These existing lamps can also be used
in the AAnalyst instrument. As a point of interest, the Lumina HCL is a new,
coded, cableless lamp design that plugs directly into the AAnalyst 100 (and 300).
The older lamps will require adapter cables. Instructions follow on how to install
your particular type of lamp.
Always wear UV-absorbing safety glasses when installing, replacing or
aligning hollow cathode lamps or electrodeless discharge lamps. The ultraviolet
radiation emitted by these lamps can harm your eyes.
4-32 Installation

Lamp Compartment Location

Access to the lamp compartment is at the front of the spectrometer. The lamp
compartment is exposed when you lift the lamp compartment cover (it is hinged on
the top). It’s location at the front of the instrument allows for easy lamp installation
and removal.
Lamp Compartment Cover

Figure 4-18. Location of the lamp compartment.


Assembling the AAnalyst 100 4-33

Installing the Lumina Hollow Cathode Lamp

As previously mentioned, the Lumina hollow cathode lamp (HCL) was designed
with the correct socket to plug directly in to the AAnalyst 100 and the AAnalyst
300. Since these lamps were designed with the AAnalyst in mind, the right socket
and coding information are standard on each. With the lamp plugged in, the
instrument will set up and store the correct lamp current, slit and wavelength
settings. Refer to the next figure when installing the Lumina HCL.

Figure 4-19. Installing the Lumina hollow cathode lamp (single mount).

1. Decide which element you want to use for your determination and then select a
Lumina HCL for this element.
2. Locate and open the lamp compartment cover on the right side of the
instrument (if it is not already open). Figure 4-18 shows the location.
3. Hold the lamp in the position shown in the figure above. Make sure the lamp
socket is lined up with the plug on the mount.
4. Carefully insert the lamp into the mount, gently plugging in the socket to the
plug. Gently push the lamp in until it is fully seated in the mount.
5. Close the lamp compartment cover. Installation of the Lumina HCL is
complete.
4-34 Installation

Installing the Lumina Hollow Cathode Lamp (Turret Model)

Refer to the next figure when installing the Lumina HCL into the six-lamp turret.

Figure 4-20. Installing the Lumina HCL (turret model).

1. Decide which element you want to use for your determination and then select a
Lumina HCL for this element.
2. Locate and open the lamp compartment cover on the right side o f the
instrument (if it is not already open). Figure 4-18 shows the location.
3. Hold the lamp in the position shown in the figure above. Make sure the lamp
socket is lined up with the plug on the turret.
4. Carefully insert the lamp into the turret, gently plugging in the socket to the
plug. Gently push the lamp in until it is fully seated in the turret.
5. Close the lamp compartment cover. Installation is complete.
Assembling the AAnalyst 100 4-35

Installing the Coded Intensitron Hollow Cathode Lamp (Single Mount)


As previously mentioned, the Intensitron hollow cathode lamp (HCL) can also be
used with the AAnalyst instrument. These older lamps require a suitable adapter
cable in order to use the coded Intensitron HCLs with the AAnalyst instrument.
There is an adapter cable for each element/lamp. Contact your PE sales office or
representative for adapter cable part numbers if you need to. Refer to the following
figure when performing the installation steps below.

Figure 4-21. Installing the coded Intensitron HCL (single mount).

1. Decide what element you want to use for your determination and then select the
Intensitron HCL for this element.
2. Locate and open the lamp compartment door on the right side of the instrument
(if it is not already open). Figure 4-18 shows the location.
3. Plug the correct adapter cable into the connector on the end of the lamp cable.
4-36 Installation

4. Hold the lamp in front of the mount in the position shown in Figure 4-21.
Then carefully insert the lamp into the mount. Gently slide the lamp in until it
hits the stop.
5. Plug the free end of the adapter cable into the plug on the single lamp mount.
6. Close the lamp compartment cover. Installation of the Intensitron HCL is
complete.

Installing the Coded Intensitron Hollow Cathode Lamp (Turret Model)


As previously mentioned, the Intensitron hollow cathode lamp (HCL) can also be
used with the AAnalyst instrument. These older lamps require a suitable adapter
cable in order to use the coded Intensitron HCLs with the AAnalyst instrument.
There is an adapter cable for each type of element. Contact your PE sales office or
representative for adapter cable part numbers if you need to. Refer to the following
figure when performing the installation steps below.

Figure 4-22. Installing the coded Intensitron HCL (turret model).


Assembling the AAnalyst 100 4-37

1. Decide what element you want to use for your determination and then select the
Intensitron HCL for this element.
2. Locate and open the lamp compartment door on the right side of the instrument
(if it is not already open). Figure 4-18 shows the location.
3. Plug the correct adapter cable into the connector on the end of the lamp cable.
4. Hold the lamp in front of the mount in the position shown in Figure 4-22.
Then carefully insert the lamp into the mount. Gently slide the lamp in until it
hits the stop.
5. Plug the free end of the adapter cable into the plug on the single lamp mount.
6. Close the lamp compartment cover. Installation of the Intensitron HCL is
complete.
4-38 Installation

Installing the Non-coded Intensitron HCL (Single Mount)

As previously mentioned, the Intensitron hollow cathode lamp (HCL) can also be
used with the AAnalyst instrument. These older lamps require a suitable adapter
cable in order to use the Intensitron HCLs with the AAnalyst instrument. There is
one adapter cable used for all of the noncoded Intensitron HCLs (cable part number
N305-0197). Contact your PE sales office or representative to get the adapter
cable if you need to. Refer to the following figure when performing the installation
steps below.

Figure 4-23. Installing the non-coded Intensitron HCL (single mount).

1. Decide which element you want to use for your determination and then select
the Intensitron HCL for this element.
2. Locate and open the lamp compartment door on the right side of the instrument
(if it is not already open). Figure 4-18 shows the location.
3. Plug the adapter cable into the connector on the end of the lamp cable.
Assembling the AAnalyst 100 4-39

4. Hold the lamp in front of the mount in the position shown in Figure
4-23. Then carefully insert the lamp into the mount. Gently slide the lamp in
until it hits the stop.
5. Plug the free end of the adapter cable into the plug on the single lamp mount.
6. Close the lamp compartment cover. Installation of the Intensitron HCL is
complete.
4-40 Installation

Installing the Non-coded Intensitron HCL (Turret Model)

As previously mentioned, the Intensitron hollow cathode lamp (HCL) can also be
used with the AAnalyst instrument. These older lamps require an adapter cable in
order to use the Intensitron HCLs with the AAnalyst instrument. There is one
adapter cable used for all of the non-coded Intensitron HCLs (cable part number
N305-0197). Contact your PE sales office or representative to get the adapter
cable if you need to. Refer to the following figure when performing the installation
steps below.

Figure 4-24. Installing the non-coded Intensitron HCL (turret model).

1. Decide which element you want to use for your determination and then select
the Intensitron HCL for this element.
2. Locate and open the lamp compartment door on the right side of the instrument
(if it is not already open). Figure 4-18 shows the location.
3. Plug the adapter cable into the connector on the end of the lamp cable.
Assembling the AAnalyst 100 4-41

4. Hold the lamp in front of the turret in the position shown in Figure
4-24. Then carefully insert the lamp into the turret. Gently slide the lamp in
until it hits the stop.
5. Plug the free end of the adapter cable into the appropriate plug on the turret.
6. Close the lamp compartment cover. Installation is complete.
4-42 Installation

Installing the Coded Electrodeless Discharge Lamp (EDL) (Single Mount)

An Electrodeless Discharge Lamp (EDL) can also be used with the AAnalyst
instrument. These older lamps can be used with a suitable coding plug if you want
the AAnalyst to recognize the EDL as coded (coding plug shown in Figure 4-25).
There is a coding plug for each type of element. If you bought the EDL with the
AAnalyst, the EDL will come with the proper coding plug. Contact your PE sales
office or representative for the part number if you have an EDL without the proper
coding plug (Note that you can also use an EDL without coding, if you wish. That
installation is discussed in the next section.)

Refer to the following figure when performing the installation steps below.

Figure 4-25. Installing the coded EDL (single mount).

1. Decide which element you want to use for your determination and then select
the EDL for this element.
Assembling the AAnalyst 100 4-43

2. Refer to Figure 4-25. Assemble the lamp by sliding the lamp driver into the
sleeve, being sure to depress the locking pin as the sleeve slides into place.
Check that the locking pin is extended through the locating hole in the sleeve.
3. Locate and open the lamp compartment door on the right side of the instrument
(if it is not already open). Figure 4-18 shows the location.
4. Plug the proper coding plug for the element used into the socket on the single
mount lamp.
5. Hold the lamp in front of the mount. Then carefully in sert the lamp into the
mount. Gently slide the lamp in until it hits the stop. The lamp is now installed
into the instrument.

NOTE: Due to the size of the electrodeless discharge lamps, the


lamp compartment cover must remain open once the EDLs are
installed.

6. Next you need to set up the lamp power supply. You’ll find the steps in the
section called Setting Up the EDL Power Supply.
4-44 Installation

Installing the Coded Electrodeless Discharge Lamp (EDL) (Turret Model)

An Electrodeless Discharge Lamp (EDL) can also be used with the AAnalyst
instrument. These older lamps can be used with a suitable coding plug if you want
the AAnalyst to recognize the EDL as coded (coding plug shown in Figure 4-25).
There is a coding plug for each type of element. If you bought the EDL with the
AAnalyst, the EDL will come with the proper coding plug. Contact your PE sales
office or representative for the part number if you have an EDL without the proper
coding plug (Note that you can also use an EDL without coding, if you wish. That
installation is discussed in the next section.)

Refer to the following figure when performing the installation steps below.

Figure 4-26. Installing the coded EDL (turret model).


Assembling the AAnalyst 100 4-45

1. Decide which element you want to use for your determination and then select
the EDL for this element.
2. Refer to Figure 4-26. Assemble the lamp by sliding the lamp driver into the
sleeve, being sure to depress the locking pin as the sleeve slides into place.
Check that the locking pin is extended through the locating hole in the sleeve.
3. Locate and open the lamp compartment door on the right side of the instrument
(if it is not already open). Figure 4-18 shows the location.
4. Plug the proper coding plug for the element used into the socket on the turret.
5. Hold the lamp in front of the turret. Then carefully insert the lamp into the
turret. Gently slide the lamp in until it hits the stop. The lamp is now installed
into the instrument.

NOTE: Due to the size of the electrodeless discharge lamps, the lamp
compartment cover must remain open once the EDLs are installed.

6. Next you need to set up the lamp power supply. You’ll find the steps in the
section called Setting Up the EDL Power Supply.
4-46 Installation

Installing the Non-Coded EDL

An Electrodeless Discharge Lamp (EDL) can also be used with the AAnalyst
instrument. As previously mentioned, you can use these older lamps without
coding, if you wish. Refer to the following figure when performing the installation
steps below. Be aware that you must program in the lamp information manually.

Figure 4-27. Installing the non-coded EDL (single mount).

1. Decide which element you want to use for your determination and then select
the EDL for this element.

2. Refer to Figure 4-27. Assemble the lamp by sliding the lamp driver into the
sleeve, being sure to depress the locking pin as the sleeve slides into place.
Check that the locking pin is extended through the locating hole in the sleeve.

3. Locate and open the lamp compartment door on the right side of the instrument
(if it is not already open). Figure 4-18 shows the location.
Assembling the AAnalyst 100 4-47

4. Hold the lamp in front of the mount. Then carefully insert the lamp into the
mount. Gently slide the lamp in until it hits the stop. The lamp is now installed
into the instrument.

NOTE: Due to the size of the electrodeless discharge lamps, the lamp
compartment cover must remain open once the EDLs are installed.

5. Next you need to set up the lamp power supply. You’ll find the steps in the
section called Setting Up the EDL Power Supply.
4-48 Installation

Installing the Non-Coded EDL (Turret Model)

An Electrodeless Discharge Lamp (EDL) can also be used with the AAnalyst
instrument. As previously mentioned, you can use these older lamps without
coding, if you wish. Refer to the following figure when performing the installation
steps below. Be aware that you must program in the lamp information manually.

Figure 4-28. Installing the non-coded EDL (turret model).

1. Decide which element you want to use for your determination and then select
the EDL for this element.

2. Refer to Figure 4-28. Assemble the lamp by sliding the lamp driver into the
sleeve, being sure to depress the locking pin as the sleeve slides into place.
Check that the locking pin is extended through the locating hole in the sleeve.
Assembling the AAnalyst 100 4-49

3. Locate and open the lamp compartment door on the right side of the instrument
(if it is not already open). Figure 4-18 shows the location.

4. Hold the lamp in front of the turret. Then carefully insert the lamp into the
turret mount. Gently slide the lamp in until it hits the stop. The lamp is now
installed into the instrument.

NOTE: Due to the size of the electrodeless discharge lamps, the lamp
compartment cover must remain open once the EDLs are installed.

5. Next you need to set up the lamp power supply. You’ll find the steps in the
section called Setting Up the EDL Power Supply.
4-50 Installation

Setting Up the EDL Power Supply


Continue the installation of the EDL system by setting up the EDL Power Supply.
Basic procedures follow. Refer to the manual that came with your EDL System 2 if
you require more information than is supplied here.

1. Place the EDL power supply near the AAnalyst instrument. Make sure it is
close enough so the cord on the lamp can reach the back of the power supply.
2. Check that the power switch is in the OFF position (see next figure).

Figure 4-29. Wiring the EDL power supply to the AAnalyst instrument.
Assembling the AAnalyst 100 4-51

3. Plug one end of the power supply cable into the receptacle on the rear of the
power supply (Figure 4-29). Plug the other end into an electrical outlet of the
proper voltage and frequency for your instrument.
4. Connect one end of the modulation cable to the receptacle marked “MOD” on
the back of the power supply (Figure 4-29). Connect the other end of the cable
to the receptacle on the far left hand side of the back of the AAnalyst. When
running with EDLs, the power supply must be in the modulation mode.
5. Finally, plug in the cable coming from the EDL in the instrument to the
receptacle on the back of the power supply marked “LAMP1.” Installation of
the EDL power supply is complete.
4-52 Installation

Connecting the Gas Supplies

NOTE:Before connecting the gas supplies, make sure you have read and met
the gas supply conditions stated in the Safety Practices chapter, titled General
Safety Practices - Safe Handling of Gas Cylinders and in the Preparing Your
Laboratory chapter, in the section titled - Gas Supply Requirements.

Perkin-Elmer atomic absorption instruments include the hoses necessary for


connection to gas inlets. It is the responsibility of the user to provide the
appropriate supply, gas hoses, regulators, connectors and valves to which the hoses
are connected.
This section will tell you how to connect the gas hoses from the back of the
AAnalyst 100 (Figure 4-30) to the air, acetylene, and nitrous oxide tanks. The
hoses are dedicated to the following supplies:
• Black hose ⇒ Air
• Red hose ⇒ C2H2 (Acetylene)
• Blue hose ⇒ N2O (Nitrous Oxide-hose is shipped with plug in it)

Figure 4-30. Rear view of the AAnalyst - the gas hoses.


Connecting the Gas Supplies 4-53

Connecting to the Air Supply


Make sure you review the material that discusses the air supply requirements in
Chapter 3, Preparing Your Laboratory. The section called Gas Supply
Requirements - Air Supply Requirements will talk about the air compressor verses
the air cylinder.
You will also find part numbers for the accessories to connect the air supply in
Chapter 3 in the section Gas Supply Requirements - Air Supply Requirements.

Requirements
As mentioned, the burner system requires an air supply that is clean, dry, and oil
free. The air supply should provide a minimum of 28 liters/min (1 cubic foot/min)
at a minimum pressure of 350 kPa (50 psig). Bleed tanks to remove water at least
once a week.

Air Compressor Setup


An air compressor is recommended for the burner system. In general, they are
uncomfortably noisy to have in the immediate vicinity of the instrument. If
possible, locate the compressor at some distance from the lab workers.

Use the following procedure to connect the AAnalyst 100 to an air compressor
supply, using the PE Air Dryer Filter and Regulator assembly (P/N 0047-0652).
If you feel you need further information, refer to the instructions provided with the
Air Dryer Filter Assembly.

Figure 4-31. Air supply connections to the AAnalyst instrument.


4-54 Installation

1. Refer to Figure 4-31. First connect the air dryer filter to your air supply:
a. Connect one end of the black hose included with the air dryer filter to your
air supply. The hose is shipped with 1/4-inch compression fitting end fittings.
b. Connect the other end of the black hose to the valved end of the air dryer
filter as shown in Figure 4-31.
2. Check the pressure on the gauge of the air dryer filter assembly. Make sure the
output pressure is between 350 and 450 kPa (between 51 and 65 psig). Adjust
the pressure regulator if necessary. (See instructions included with assembly.)
3. Connect the black air hose (coming out the back of the AAnalyst 100) to the
other end of the air dryer filter as shown in Figure 4-31 above.

Air Cylinder Setup


Cylinders of compressed air should only be used as an emergency or short term
solution. (An air compressor is recommended.) If you are using compressed air in
cylinders, be sure that the oxygen content is less than 20%. Be sure to read the
cautions in the Safety Practices and Preparing Your Laboratory chapters.

Use the following procedure to connect the AAnalyst 100 to an air cylinder supply,
using the PE Air Dryer Filter Assembly (P/N 0047-0652). If you feel you need
further information, refer to the instructions provided with the Air Dryer Filter
Assembly for additional information

1. First connect the air dryer filter to your air supply:

a. Connect one end of the black hose included with the air dryer filter to your
air supply. The hose is shipped with 1/4-inch compression fitting end fittings.

b. Connect the other end of the black hose to the end of the air dryer filter as
shown in Figure 4-31.
2. Check the pressure of the air dryer filter assembly. Make sure the output
pressure is between 350 and 450 kPa (between 51 and 65 psig).
3. Connect the black air hose (coming out the back of the AAnalyst 100) to the
other end of the air dryer filter as shown in the Figure 4-31.
Connecting the Gas Supplies 4-55

Connecting to the Acetylene Supply


Make sure you review the material that discusses the acetylene supply
requirements in Chapter 3, Preparing Your Laboratory. The section to review is
called Gas Supply Requirements / Acetylene Supply Requirements. It talks about
grade, cylinder specifications, warnings and piping requirements. You will also
find part numbers for the accessories to connect the acetylene supply.

Requirements
The acetylene supply should be of “atomic absorption” or a welding grade (99.6%
pure). The recommended output pressure for the acetylene supply is 83 to 96 kPa
(12-14 psig).

Acetylene Warnings

Acetylene is a flammable gas. Be sure that all connections are gas tight. Check the
connections and gas hose regularly for leaks.

Acetylene line pressure from the tank to the instrument should never exceed
104 kPa (15 psig). At higher pressures, acetylene can spontaneously decompose or
explode. A max. line pressure of 96 kPa (13.7 psig) is strongly recommended.

Use an outlet gauge pressure between 83 and 96 kPa (12 and 14 psig). Never
allow the outlet gauge pressure to exceed 104 kPa (15 psig). At higher
pressures, acetylene can decompose explosively.

Never let the tank pressure drop below 600 kPa (85 psig). Failure to do so may
cause damage to valves or tubing within the burner gas control system due to
acetone contamination.

Air/Acetylene Filter Assembly Setup


This filter system (P/N N0930-1398) is designed for use with AA spectrometers
with microcomputer gas controls. It includes filters for both compressed air and
acetylene. It also includes an acetylene flashback arrestor. Use this “combination”
filter in place of the individual Air Dryer filter and the Acetylene Filter.
4-56 Installation

Recommended Acetylene Supply Setup

Figure 4-32. Acetylene supply connections.

1. Refer to Figure 4-32. Connect an acetylene regulator to your acetylene cylinder


using a CGA No. 510 or 300 adapter.
2. The PE regulator includes a 1/4-inch pipe to 9/16-inch left-hand thread outlet
bushing (P/N 0990-3031). Connect the 1/4-in. end to the regulator end fitting.

If you are not using the Perkin-Elmer regulator and your regulator end fitting
does not match the 1/4-inch end of the outlet bushing, use a female adapter
(P/N 0990-3196).
3. The AAnalyst 100 has a red acetylene hose with a 9/16-inch left-hand thread
connector on the end. Connect the hose to the 9/16-inch end of the outlet
bushing.
4. After all the acetylene connections have been made and the fuel system
pressurized, you must test the connections. Use a solution of water and liquid
soap.

All connections must be leak tested with a solution of water and liquid soap to
insure that no leaks are present.
Connecting the Gas Supplies 4-57

If the smell of acetylene is present at any time and the source of the leak cannot
be determined and corrected, contact a representative at Perkin-Elmer. DO
NOT ATTEMPT TO IGNITE THE FLAME!

Connecting to the Nitrous Oxide Supply


Make sure you review the material that discusses the nitrous oxide supply
requirements in the Preparing Your Laboratory chapter. The section to review is
Chapter 3, Gas Supply Requirements / Nitrous Oxide Supply Requirements. It
talks about cylinder specifications, warnings and the heated regulator requirements.
You will also find part numbers for the accessories to connect the N2O supply.

Requirements
The nitrous oxide supply should be at least 99% pure. A heated regulator
providing an output pressure of 345 to 520 kPa (50-75 psig) is recommended. If
you are not going to use the nitrous oxide gas supply, leave the cap plug fitting
(P/N 0992-0165) on the end of the instrument nitrous oxide hose.

Recommended Nitrous Oxide Supply Setup


Use the procedure below to connect the AAnalyst to your nitrous oxide supply:

Figure 4-33. Nitrous oxide supply connections.

1. Connect a nitrous oxide regulator to your nitrous oxide cylinder as shown in


the figure above.
4-58 Installation

2. Connect the blue AAnalyst 100 nitrous oxide hose to the 5/16-inch male
connector on the regulator.
3. Connect the regulator heater power cord to line power.

Connecting to the Argon Supply


The argon supply is not used with the basic AAnalyst 100. It is used, however,
with some of the accessories (furnace, FIAS, MHS-10). In an effort to dispense
complete information - the argon supply hook-up is included here. Argon gas
never hooks up the AAnalyst instrument; it gets connected to certain accessories.

Make sure you review the material that discusses the argon supply requirements
in Chapter 3, Preparing Your Laboratory. The section to review is called Gas
Supply Requirements / Argon Supply Requirements. It includes details about the
purity criteria. You will also find part numbers for accessories to connection to the
argon.

Requirements

As previously mentioned, a supply of argon meeting the purity criteria listed in the
following table is recommended.

Gas Specified Concentration


Argon > 99.996%
Oxygen < 5 ppm
Nitrogen < 20 ppm
Water < 4 ppm
Connecting the Gas Supplies 4-59

Recommended Argon Supply Setup


The connections at the argon supply are shown below. Refer to Figure 4-34 when
performing the procedures that follow:

Figure 4-34. Argon supply connections (for accessories only).

Use the following procedure to connect your argon gas supply:

1. Connect the argon regulator to your argon supply using a CGA 580 connector
(included with Perkin-Elmer argon regulators).
2. If you are using a Perkin-Elmer regulator, connect the argon hose from your
accessory to the regulator end fitting.
If you are not using a Perkin-Elmer regulator and your regulator end fitting
does not match the 1/4-inch compression fitting connector on the end of the
argon hose, use a female adapter (P/N 0990-3196).
4-60 Installation

Connecting the Electrical Supply

NOTE:All AAnalyst 100 instruments are shipped set for 220 VAC. If the voltage
marked on the instrument does not match your AC line voltage, you must change
the instrument operating voltage. The procedures to do so are in this section.

A Review of the Electrical Specifications


The electrical supply voltage must be one of the following:

•100 VAC ±10% @ 50 Hz ±1% or @ 60Hz ± 1%


•120 VAC ±10% @ 50 Hz ± 1% or @ 60Hz ±1%
•220 VAC ±10% @ 50 Hz ± 1% or @ 60Hz ± 1%
•230 VAC ±10% @ 50 Hz ± 1% or @ 60Hz ± 1%
•240 VAC + 6% / − 10% @ 50 Hz ± 1% or @ 60Hz ± 1%

The electrical supply voltage should be free of line transients in excess of 50V
peak. If the supply voltage produces large AC line voltage fluctuations, install a
voltage regulator between the AC outlet and the instrument.

The spectrometer requires either a 120 VAC standard 15 amp grounded outlet, or a
220 VAC outlet. In addition, the instrument consumes 248 volt amps when
configured for background correction.

The AAnalyst 100 requires a grounded AC outlet providing voltage corresponding to


the voltage marked on the instrument (100, 120, 220 or 230/240 VAC).

Do not remove or alter the ground prong on a three-prong ground cord.


Connecting the Electrical Supply 4-61

How to Find Out the Instrument Voltage Setting


Look for the power entry module on the right side of the instrument (refer to the
figure below). Look for the white pin protruding through one of the four holes on
the power entry module cover plate (marked 100V, 120V, 220V or 240V).That
white pin marks the instrument voltage setting.

For example, the figure below shows that the instrument is set to run at 220 VAC.

Power Entry Module

Power Entry Module


Cover Plate

Voltage Indicator Hole with White


Plastic Pin in 220V position

Figure 4-35. Location of the power entry module and ON/OFF switch.
4-62 Installation

If You Have 220 VAC in Your Lab


If your electrical supply voltage is 220 VAC, then your supply matches what the
instrument was configured for from the factory . To confirm that your instrument has
220V operation, look for the power entry module on the right side of the instrument
(refer to the previous figure). Notice that the voltage selected on the instrument is
220V. (You’ll see a white plastic pin protruding through the hole marked 220V.)

Once you have confirmed the above, you’re ready to connect power to the
instrument. Make sure your instrument is switched OFF (the “o” is depressed).
Next, simply plug one end of the 220 VAC line cord into the power entry module.
Then, plug the other end of the line cord into the 220 VAC power outlet.

Changing the Instrument Operating Voltage


If the operating voltage selected on the instrument does not match the AC line
voltage in your lab, you will need to change the operating voltage on the
instrument.

1. Make sure the instrument is switched OFF (the “o” is depressed). Disconnect
the instrument from the line power (if connected).
2. Refer to the figure below. Locate the power entry module on the right side of
the instrument. Insert a small flat-blade screwdriver or similar tool into the
notch, and carefully pry off the power entry module cover.

Figure 4-36. Pry off the power entry module cover.


Connecting the Electrical Supply 4-63

3a. FUSE BLOCK: Note that the inside of the power entry module cover holds
the fuses necessary to convert the instrument to any of the four operating
voltages. For 100, 120 or 220 VAC labs (single fuse configuration), arrange
the fuse block with the single-fuse side facing up (see the figure below). For
220 and 230/240 VAC labs, arrange the fuse block with the dual-fuse side up.

Figure 4-37. Location of the instrument fuse block and fuses.

3b. To convert your fuse block to a different voltage (when changing the
instrument voltage), hold the fuse block in the position shown above and
remove the phillips head screw that holds the fuse block to the cover. Note
which fuse is facing you before continuing. Now carefully lift the fuse block
away from the cover (wiggle to unhook, if necessary). Flip the fuse block over
so that the OTHER side is now facing you. Carefully place the fuse block
assembly back onto the cover, with the new fuse (or fuses) facing you. Secure
the assembly with the phillips head screw.
4-64 Installation

Changing a Fuse
4. TO CHANGE A FUSE: Perform steps 1 and 2 above. Then, carefully remove
the existing blown fuse and replace it with the correct fuse for your operating
voltage. Refer to Figure 4-38 and use the following tables as a guide when
choosing the correct replacement fuse.

Single Fuse Configuration:

Voltage: Insert the Following Fuse: Part Number:


100 VAC 6.25 amp, slow blow, 250V, 3AG 0998-1761
120 VAC 6.25 amp, slow blow, 250V, 3AG 0998-1761
220 VAC 3.0 amps, slow blow, 250V, 3AG 0998-1626

Dual Fuse Configuration:

Voltage: Insert the Following Fuse: Part Number:


220 VAC 3.15 amps, slow blow, 250V, metric 0999-1675
230/240 VAC 3.15 amps, slow blow, 250V, metric 0999-1675

Figure 4-38. Changing a fuse.


Connecting the Electrical Supply 4-65

Changing the Setting on the Voltage Selector Board


5a. To change the setting on the voltage selector board, locate the voltage selector
board inside the power entry module (see the figure below). Carefully pull the
voltage selector board from the instrument using a long nose pliers (or similar
tool). Take care not to scratch the board cladding or crush the board.

Figure 4-39. Location and removal of the voltage selector board.

5b. Find the printed voltage setting on the board that matches your lab’s voltage.
Notice the arrow next to it. The correct board setup is illustrated in the next
figure. In the end, the white indicator pin should point in the opposite direction
from the arrow next to your chosen lab voltage.

Figure 4-40. Orientation of the indicator pin on the voltage selector board.

To do this, orient the board as in the previous figure, hold the board in one
hand and grasp the white indicator pin in the other. Gently pull the white
voltage indicator pin away from the board, and slide it along each edge of the
board until the pin is pointing in the opposite direction of the arrow. Make
sure the pin seats itself by pushing it snugly into the little notch in the board.
4-66 Installation

6. Reinstall the voltage selector board into the instrument - making sure the side
of the board with writing faces the On/Off switch. Then carefully snap the
power entry module cover back in place.
7. Check to see that the white “pin” can be seen protruding through the module
cover, indicating the correct voltage setting for your lab. If the pin is not
visible, remove the cover and make sure the voltage indicator pin is in the
correct position.

Installing the AC Line Cord

Grounding circuit continuity is vital for safe operation of equipment. Never


operate equipment with grounding conductor disconnected. Do not remove or alter
the ground pin on a three-prong line cord.

The line cord should have the electrical rating and plug appropriate for your
location. See Figure 4-41 for the correct cord.

1. Select the proper line cord for your location.


2. Insure that the power switch is off and insert one side of the line cord plug into
the instrument and the other side into the AC supply.
Connecting the Electrical Supply 4-67

Figure 4-41. The AC line cord selections for the AAnalyst instrument.
4-68 Installation

Setting Up the Okidata 320 Printer


The standard printer for use with the stand-alone AAnalyst 100 is the Okidata
Microline 320 printer. The default printer settings made at the factory are to be
used with the exception of Emulation Mode (which is to be changed to Epson
FXe), and Character Set (which should be changed to Set I). Do the following
before using the Okidata Microline 320 Printer with the AAnalyst 100 instrument
(without a computer).
For a Keypad-Controlled AAnalyst 100
1. Connect the parallel printer cable (0941-0001) between the printer port on the
back of the instrument and the input connector on the back of the printer. (See
figure below.)
2. Connect one end of the printer power cord to the printer and the other end to
the line power.
3. Change the default printer settings per the instructions on the next page.
Setting Up the Okidata 320 Printer 4-69

Figure 4-42. Connecting the printer to the keypad controlled AAnalyst.


Change the Default Settings of the Printer

Using the MODE command on the printer to access the menu selections, change
the printer default settings (settings made at the factory) as described next.

1. Press the MODE button on the front panel of the Okidata Printer. You
will then be able to access the menu selections.
2. Press the GROUP button until you see:
General Control Emulation Control IBM PPR
3. Press the SET button until you see:
General Control Emulation Control Epson FXe
4. Press the PRINT button to print out the menu and the new settings.
5. Press the MODE button on the printer to save the menu changes and
return to the Print mode.
4-70 Installation

Refer to the next table for the printer default settings. If the settings of your
Okidata 320 printer have been changed (for use with another instrument), you must
reset them using the information in this table. Do this before you use the printer
with the key-pad controlled AAnalyst 100.

For the AAnalyst 300 or the PC Controlled AAnalyst 100

Use either an HP Inkjet or LaserJet printer (e.g., the HP Model 660 printer).
Setting Up the Okidata 320 Printer 4-71

Table of Default Settings for the Okidata Microline 320 Printer


Group Item Settings
FONT Print Mode Utility
Draft Mode HSD
Pitch 10 CPI
Style Normal
Size Single
GENERAL Emulation Mode IBM PPR*
Graphics Bi-directional
Max Receive Buffer Full
Paper Out Override No
Print Registration 0
Operator Panel Functions Full Operation
Reset Inhibit No
Print Suppress Effective Yes
CPU Compensation Normal
VERTICAL CONTROL Line Spacing 6 LPI
Form Tear-Off Off
Skip Over Perforation No
Auto LF No
Auto CR No
Auto Feed XT Invalid
Page Length 11"
CUT Sheet Page Length 11"
SYMBOL SETS Character Set Epson**
Language Set American
Zero Character Slashed
* Must be changed to Epson FXe
** Should be changed to Set I

(continued on next page. . . )


4-72 Installation

(Table of Default Settings for the Okidata Microline 320 Printer, cont.)
Group Item Settings
SERIAL INTERFACE Parity None
Serial Data 7 or 8 Bits 8
Protocol Ready/Busy
Diagnostic Test No
Busy Line SSD-
Baud Rate 9600 BPS
DSR Signal Valid
DTR Signal Ready on Power Up
Busy Time 200 Milliseconds
Powering Up the Instrument 4-73

Powering Up the Instrument


This section describes the instrument power up sequence.

Switch the power ON (switch on lower right side of instrument, Figure 4-35). The
instrument will automatically run a self test. The following screen is displayed:

SELF TEST MODE

Wait while the instrument goes through its initializing process. The LEDs will all
light as the instrument sequences through its tests. After a few seconds, the
following screen is displayed:

SELF TEST MODE


VERSION X.XX XXXX
The first three numbers (X.XX) refer to the Firmware version

After a few seconds, the following screen is displayed:

PERKIN-ELMER AANALYST

And finally, the following screen is displayed:

RECALL METHOD? (Y/N)


→ N
The instrument power up and initialization procedure is complete and the AAnalyst
is ready for the post installation adjustments and checks next.
4-74 Installation

Post Installation Adjustments and Checks


This section describes how to adjust parts of the instrument after completing the
installation. Adjustments and checks included are listed below:

• Aligning the Lamp(s)


• Adjusting the Burner Height
• Adjusting the Gas Flow for Ignition
• Igniting the Flame
• Adjusting the Burner Position
• Adjusting the Nebulizer
• Sample Introduction System Pre-Conditioning
• Checking the Nitrous Oxide Flame

Aligning the Lamp(s)


Refer to the AAnalyst 100 User’s Guide (P/N 0993-6149) for the lamp alignment
procedures. They are located in Chapter 2, Aligning Lamps. The procedures you
should look for are in the sections called Aligning a Hollow Cathode Lamp or
Aligning an Electrodeless Discharge Lamp - depending on which lamps you are
using.

If you are using an instrument that is under computer control, refer to the AA
WinLab Software Guide (0993-6190). The information is located in Chapter 8,
Setup Windows - Align Lamps Window.

When you are done aligning the lamps, continue on to the next procedures in this
manual to adjust the burner height.
Post Installation Adjustments and Checks 4-75

Adjusting the Burner Height


This section assumes the AAnalyst instrument has been properly installed and
powered up with a lamp in place per the instructions in this chapter. Continue on to
adjust the burner height using the information in this section.

1. Turn on the vent above the instrument.


2. If it is not already on, power up the instrument (as described in the section
Powering Up the Instrument). DO NOT LIGHT THE FLAME.
3. Place a piece of cardboard or a white business card above the burner head
perpendicular to the slot (shown in the next figure). Doing this will enable you
to confirm the presence and general location of the light beam. If you cannot
find a beam, step 4 will give you adjustment instructions.

Figure 4-43. Locating the light beam above the burner.

4. You want to be sure that the burner head is not blocking the beam and that the
beam is centered. Ideally, you want the beam to pass over the length of the
burner head and to be centered over the burner slot (Figure 4-43). If it is not, or
if the burner head is blocking the beam, turn the horizontal adjustment knob
(Figure 4-44) until the light beam is approximately centered directly over the
burner slot.
4-76 Installation

Horizontal
Adjustment Vertical Adjustment
(forward (up and down)
and back) Rotational Adjustment

Figure 4-44. Burner adjustment knobs.

5. Next, you will adjust the height of the burner. Press [Cont] on the instrument
keypad. The Continuous screen appears and displays an arbitrary negative
absorbance value. For example:

CONTINUOUS
ABS = -0.394

6. Lower the burner using the vertical adjustment knob (Figure 4-44) so that the
burner head is well below the light beam.
Post Installation Adjustments and Checks 4-77

7. Next press the [A/Z] key. Autozero is performed and the following display
appears:

CONTINUOUS
ABS = 0.000

8. Raise the burner with the vertical adjustment knob until the display indicates a
slight positive absorbance (0.002 to 0.004 absorbance).
9. Now, slowly turn the vertical adjustment knob clockwise until the absorbance
returns to zero (0.000).
10. Finally, rotate the vertical adjustment knob an additional quarter-turn
clockwise. Your burner height adjustment is now complete.

Adjusting the Gas Flows for Ignition


This section continues with the post installation adjustments and assumes the
AAnalyst instrument has been properly installed and powered up per the
instructions in this chapter. Now you will adjust the gas flows and ignite the flame
using the information in the next two sections.

Do not proceed until all the fuel connections have been leak-tested. Use a
solution of water and liquid soap to check all fuel connections for leaks.
1. Turn on the vent above the instrument (if it is off).
2. If it is not already on, power up the instrument (as described in the section
Powering Up the Instrument). DO NOT LIGHT THE FLAME.
3. Set the pressure regulators on the gas cylinders that you’ll be using as follows:

Tank Output Pressure Settings.

Acetylene 85-100 kPa (12-14 psig)


Air 345-450 kPa (50-65 psig)
Nitrous Oxide 345-520 kPa (50-75 psig)
4-78 Installation

Remember, always monitor the acetylene tank pressure. Change the tank
before the tank pressure drops below 600 kPa (85 psig). If the pressure falls below
this level, acetone may contaminate the burner regulator, valves and tubing. Such
damage is not covered by the instrument warranty.

NOTE: The [Gases On/Off] key will allow the fuel and oxidant to
flow through the gas control system and out the burner head. Make
sure that the vent above the instrument has been turned on.

4. Press [Gases On/Off] on the keypad and observe the flowmeter tube labeled
“Oxidant” on the instrument (Figure 4-45). Using the “Oxidant” control knob,
adjust the oxidant flow until the ball in the flowmeter reads “4” units.

NOTE: The tic marks on both flowmeters are arbitrary units. For the
purposes of this installation, it is sufficient to use the markings on the
tubes as “1” tic mark per line. (The number “4” represents the 4th line up
from the bottom).

Figure 4-45. The gas flowmeters and control knobs.

5. Now observe the flowmeter tube labeled “Fuel.” Using the “Fuel” control
knob, adjust the acetylene flow until the ball in the flowmeter reads about
“2” units.
Post Installation Adjustments and Checks 4-79

Igniting the Flame

Never directly view the flame without protective eye wear. Potentially
hazardous ultraviolet radiation may be emitted from the flame. In general,
ordinary safety glasses will provide sufficient protection, but additional side shields
will insure a further margin of safety. The safety glasses will also provide
mechanical protection for the eyes.

1. Press the [Flame On/Off] key. The ignitor arm will swing over and light the
burner. If the flame does not light on the first try, it may be necessary to press
the [Flame On/Off] key a second time. Note that sometimes when gases are
first turned on, the flame may not ignite the first time due to air in the lines. For
your information, as a safety feature, if the gases do not ignite within
9 seconds, the system will turn off the gas flow and will display an error
message.
If the flame still does not light, an interlock might not be satisfied and an error
message will be displayed. Refer to the Troubleshooting chapter.
2. With the flame on, aspirate the blank and let the flame stabilize for about 30 to
60 seconds.
3. If you see bubbles coming out of the capillary tube, the nebulizer needs an
adjustment. Loosen the nebulizer locking ring and turn the nebulizer adjustment
nut clockwise until the bubbles stop (Figure 4-46). (Note that a full adjustment
is done after you adjust the burner position).
4. Press [A/Z] again. (One should always press the Autozero key when aspirating
the blank.)

Adjusting the Burner Position


This section assumes the AAnalyst instrument is powered up and the flame has
been ignited. Refer to Figure 4-44 when adjusting the burner position.

1. Aspirate a standard that produces a signal of approximately 0.2 absorbance


units. You can use elements such as Cu, Mn, or Mg. These are at wavelengths
where flame gases do not absorb the light.
4-80 Installation

2. Turn the horizontal adjustment knob on the burner assembly (Figure 4-44)
until you obtain maximum absorbance.
3. Turn the rotational adjustment knob until you obtain maximum absorbance.
4. Leave the capillary tube in the standard for the next procedure. Adjusting the
burner position is now complete.

Adjusting the Nebulizer


The next part of the post-installation test is done in order to peak the nebulizer.

Use only an air-acetylene flame while adjusting the nebulizer. Using a nitrous
oxide-acetylene flame for this procedure can cause erratic flame conditions or a
flashback.

1. Loosen the nebulizer locking ring by turning it clockwise (CW) until it is free
of the nebulizer adjustment nut (Figure 4-46).
2. To establish a start point, slowly turn the nebulizer adjustment nut
counterclockwise (CCW) until bubbles begin to appear at the end of the
capillary tube in the standard solution.
3. Slowly turn the nebulizer adjustment nut CW until the absorbance goes to a
maximum and then begins to decrease. The inversion point at which
absorbance changes marks the optimum setting. Slowly turn the nebulizer
adjustment nut CCW to obtain maximum absorbance.
4. Continue to adjust CW or CCW until the maximum absorbance is found.
Post Installation Adjustments and Checks 4-81

Capillary Tube

Nebulizer
Locking
Ring Nebulizer
Adjustment
Nut

Figure 4-46. Adjusting the nebulizer.

5. Finally, lock the nebulizer in this optimum position by firmly holding the
nebulizer adjustment nut in place with one hand while turning the nebulizer
locking ring CCW with the other. Turn it until it is snug against the nut. The
ring will prevent the nut from moving.
Adjusting the nebulizer is now complete.

Sample Introduction System Pre-Conditioning

NOTE: This important procedure MUST be performed at this point of


the installation process.

In order for the sample introduction system to aspirate sample and drain smoothly,
all the internal surfaces need to be prepared. This is easily accomplished by
aspirating a 50/50 solution of water and methanol for approximately 5 minutes.

This procedure should be done directly after installation and repeated if the drain
tube or any of the sample introduction system components are replaced.

Refer to the User’s Guide to check the characteristic concentration (Chapter 5,


Igniting and Optimizing the Flame - 7 Check the Characteristic Concentration).
4-82 Installation

Checking the Nitrous Oxide Flame (for Nitrous Oxide-Acetylene


Analysis)
In this procedure, you will install the nitrous oxide burner head (if it has been
purchased) and check the nitrous oxide flame as described below.

1. Turn OFF the instrument. Allow the burner head to cool.

Allow the burner head in the instrument sufficient time to cool before
proceeding.

2. Once it has cooled, remove the standard burner head and replace it with the
nitrous oxide burner head.
3. Make sure that the burner head is fully seated and secure. (For instructions,
refer to the section Assembling the Quick-Change Burner Mount Assembly -
Installing and Securing the Burner Head earlier in this chapter).
4. Press the [Flame On/Off] key to ignite the flame. Continuously aspirate water
to keep the burner head at a constant temperature when you are not analyzing
samples.
5. Increase the fuel flow until the flame becomes slightly rich. Allow the burner
head to warm up. (Wait approximately 15 seconds.) The red plume should be
1-1/2″ to 1-3/4″ high. If the plume is too high, decrease the fuel. If it is too low,
increase the fuel.
6. Next press the [N2O] key to switch over to a nitrous-oxide/acetylene flame.
Verify that there is a red plume at the base of the flame.
7. To extinguish the flame, press the [Flame On/Off] key once more.

The post installation adjustments and checks are now complete.


Post Installation Adjustments and Checks 4-83
Lamps 5
Introduction to this Chapter.................................................................................. 5-1
General Lamp Information ................................................................................... 5-1
An Explanation: Hollow Cathode Lamps (HCLs) ................................................ 5-3
Lumina Hollow Cathode Lamps .......................................................................... 5-4
Intensitron Hollow Cathode Lamps ..................................................................... 5-4
An Explanation: Electrodeless Discharge Lamps (EDLs) .................................... 5-6
Lamp Installation .................................................................................................. 5-7
Lamp Alignment.................................................................................................... 5-7
Lamp Maintenance and Cleaning......................................................................... 5-7
Lamp Life .............................................................................................................. 5-7
Lamp Troubleshooting .......................................................................................... 5-7
Replacing the Lamps ............................................................................................. 5-8
Lamp Compartment Location .............................................................................. 5-8
Replacing the Lumina HCL................................................................................. 5-9
Replacing the Lumina HCL (Turret Model) ...................................................... 5-10
Replacing the Coded Intensitron HCL ............................................................... 5-11
Replacing the Coded Intensitron HCL (Turret Model) ....................................... 5-13
Replacing the Non-Coded Intensitron HCL ....................................................... 5-14
Replacing the Non-coded Intensitron HCL (Turret Model) ................................ 5-16
5-2 Lamps

Replacing the Coded Electrodeless Discharge Lamp.......................................... 5-18


Replacing the Coded Electrodeless Discharge Lamp (Turret Model) ................. 5-20
Replacing the Non-Coded Electrodeless Discharge Lamp.................................. 5-22
Replacing the Non-Coded Electrodeless Discharge Lamp (Turret) .................... 5-24
The Deuterium Arc Background Corrector ....................................................... 5-26
An Explanation: The Deuterium Arc Background Corrector ........................... 5-26
Replacing the Deuterium Arc Background Corrector Lamp............................. 5-26
Equipment Needed............................................................................................ 5-27
Removing the Deuterium Lamp Assembly......................................................... 5-27
Replacing the Deuterium Lamp ......................................................................... 5-28
Reassembling the Deuterium Lamp Assembly................................................... 5-29
Aligning the Deuterium Arc Lamp Assembly .................................................... 5-30
Lamps 5
Introduction to this Chapter

This chapter contains information on the various light sources (or lamps) that go
into the AAnalyst 100 and AAnalyst 300. You will also find information about the
deuterium arc background corrector lamp.

General Lamp Information

There are a number of different lamps that can be used with the AAnalyst
instruments: the Lumina Hollow Cathode Lamp (HCL); the Intensitron Hollow
Cathode Lamp (coded and non-coded); and the Electrodeless Discharge Lamp
(EDL) (coded and non-coded). The variety exists because many labs are currently
using these lamps in their other Perkin-Elmer AA instruments. All three types of
lamps can also be used in the AAnalyst instrument.

As a point of interest, the Lumina HCL is a new coded cableless lamp design that
plugs directly into the AAnalyst 100 and 300. The older lamps will require adapter
cables. Instructions are included here on how to replace your particular type of
lamp.
5-2 Lamps

The type of primary source lamp required for your instrument depends on the
elements to be determined. Either hollow cathode or electrodeless discharge lamps
may be used. Hollow cathode lamps (HCLs) are excellent for most elements;
however, there are a number of “difficult” elements for which an improved light
source is desirable. Electrodeless discharge lamps (EDLs) are more intense than the
HCLs. Most EDLs provide better lamp life and stability. Some also provide better
sensitivity. EDLs require a separate power supply.

The 5 types of lamps that can be used in the AAnalyst 100 or AAnalyst 300 are
listed:
• the Lumina hollow cathode lamp (HCL)
• the coded Intensitron hollow cathode lamp (HCL)
• the non-coded Intensitron hollow cathode lamp (HCL)
• the coded Electrodeless discharge lamp (EDL)
• the non-coded Electrodeless discharge lamp (EDL)

The basic AAnalyst 100 instrument has a mount for a single lamp. It can, however,
be purchased with an automatic six-lamp turret.

The AAnalyst 300 comes standard with the automatic six-lamp turret.
An Explanation: Hollow Cathode Lamps (HCLs) 5-3

An Explanation: Hollow Cathode Lamps (HCLs)

The specific determination of one element in the presence of others is possible with
the use of special light sources and careful wavelength selection in a spectrometer.
A single-element lamp emits specific wave-lengths of light for the element from
which the cathode is constructed. There are single-element lamps for all elements
commonly measured by atomic absorption. Hollow cathode lamps (HCLs) are ideal
for determining most elements by atomic absorption spectroscopy.

Refer to Figure 5-1. The basic components of an HCL are a glass cylinder filled
with an inert gas (argon or neon) at low pressure, an anode, a cathode, and a quartz
window with a graded seal to be used at wavelengths below 230 nanometers (nm),
or a UV-transmitting glass window for lamps to be used at longer wavelengths.
The cathode is a hollow cylinder of the metal whose spectrum is to be produced.
Both the anode and cathode are sealed in the glass cylinder. The quartz graded seal
or glass window is fused to the glass cylinder.

Figure 5-1. The workings of a hollow cathode lamp (HCL).

Hollow cathode lamps emit light by the following process: the fill gas is ionized
when an electrical potential is applied between the anode and the cathode. The
positively charged ions collide with the negatively charged cathode and dislodge
individual metal atoms in a process known as “sputtering.” These sputtered metal
atoms are excited through impact with fill gas ions. Light of the specific
wavelengths for that element is emitted when the atom “decays” from the excited
state to a more stable state.
5-4 Lamps

Lumina Hollow Cathode Lamps

The Lumina hollow cathode lamps were designed for use with the AAnalyst series
of atomic absorption spectrometers. They are the latest innovation in optimizing
light sources for AA spectrometers. These lamps provide fully automated
wavelength, current and slit selection which results in reduced setup times for easy
and accurate operation.

Figure 5-2. Drawing of a Lumina hollow cathode lamp.

The Lumina HCLs are manufactured without cables. When they are used with the
AAnalyst instrument, they are installed simply by sliding the lamp into the single
lamp mount or turret. Lamp alignment occurs automatically if you have the model
with the automatic six-lamp turret feature.

Each Lumina HCL includes a milliampere-hour timer in its base. This allows you
to monitor the lamp usage easily and accurately for Good Laboratory Practices
compliance as well as lamp replacement scheduling. With a range of 0 to 10,000
milliampere-hours, the meter measures the number of milliampere-hours that your
lamp has operated.

Intensitron Hollow Cathode Lamps

The AAnalyst series spectrometers can also be used with the older Intensitron
hollow cathode lamps (HCLs), either coded or non-coded lamps. The coded HCLs
are used with instruments which can read the lamp coding and automatically set the
An Explanation: Hollow Cathode Lamps (HCLs) 5-5

correct lamp current, wavelength, and slit width. Non-coded HCLs can also
be used with the appropriate adapter; however, lamp and element parameters must
be set manually when non-coded lamps are used.

Figure 5-3. The Intensitron hollow cathode lamps (coded and non-coded).

With the use of the proper adapter cable, the Intensitron HCLs can be used with
AAnalyst instruments. Refer to the figure below. If you have a coded Intensitron
HCL, there is a corresponding coded adapter cable to be used for each of the
lamps. If you have a non-coded Intensitron HCL, there is one adapter cable (N305-
0197) that will connect the plug on any of the non-coded HCLs to the AAnalyst
instrument.

Figure 5-4. The adapter cables necessary to use the Intensitron HCLs.
5-6 Lamps

An Explanation: Electrodeless Discharge Lamps (EDLs)

While hollow cathode lamps are an ideal source for determining most elements by
atomic absorption, for volatile elements, an electrodeless discharge lamp (EDL) is
recommended instead. EDLs provide greater light output for improved detection
limits and precision, along with increased sensitivity and working curve linearity.
EDLs also have a longer life than corresponding hollow cathode lamps. For certain
elements (such as arsenic and selenium), EDLs will also provide improved
sensitivity and lower detection limits.

Figure 5-5. An Electrodeless Discharge Lamp (EDL).

An EDL consists of a quartz bulb under an inert gas atmosphere, containing the
element or a salt of the element for which the lamp is to be used. When an RF field
is applied to the bulb, the inert gas is ionized and the coupled energy excites the
vaporized analyte atoms inside the bulb, causing them to emit their characteristic
spectrum. The emission spectra produced is typically much more intense than that
from hollow cathode lamps, frequently tenfold larger or more.
Lamp Installation 5-7

Lamp Installation

When you first receive your instrument, there is no lamp source installed. For
initial lamp installation details, see Chapter 4, Installation, in this manual. If you
need to replace an existing lamp, the next few sections of this chapter give the
various lamp replacement procedures.

Lamp Alignment

Refer to Chapter 2 of the AAnalyst 100 User’s Guide (0993-6149) for the
procedures to align a lamp in an AAnalyst instrument with a single lamp mount.

Refer to the AA WinLab Software Guide (0993-6190) for the procedures to align
the lamps in an AAnalyst instrument with an automatic six-lamp turret.

Lamp Maintenance and Cleaning

There is really no maintenance procedures for any of the Perkin-Elmer hollow


cathode lamps. If you notice fingerprints on the “window” of your lamp, wipe
them off with a soft, dry, lint free cloth. Use no chemicals or water. See the section
below regarding lamp life and when to replace them.

Lamp Life

Both hollow cathode and electrodeless discharge lamps have a finite lifetime.
Electrodeless discharge lamps typically last longer than hollow cathode lamps for
the same element. If, while aligning a lamp, you are not able to obtain a
satisfactory energy value, this may indicate that the lamp is starting to deteriorate.
As a hollow cathode lamp reaches the end of its useful life, the current on the lamp
may be increased up to the maximum current recommended on the label. Once the
intensity of a lamp begins to deteriorate, it should be replaced.

Lamp Troubleshooting

Refer to Chapter 8, Troubleshooting, in this manual for lamp troubleshooting


information.
5-8 Lamps

Replacing the Lamps

Always wear UV-absorbing safety glasses when installing, replacing or


aligning hollow cathode lamps or electrodeless discharge lamps. The ultraviolet
radiation emitted by these lamps can harm your eyes.

Lamp Compartment Location

The next figure shows where the lamp compartment is located on the instrument.
Access to the lamp compartment is at the front of the spectrometer. This allows for
easy lamp replacement. If you lift the lamp compartment cover (it is hinged on the
top), the lamp compartment can be seen inside.
Lamp Compartment Cover

Figure 5-6. Accessing the lamp compartment.


Replacing the Lamps 5-9

Replacing the Lumina HCL

Always wear UV-absorbing safety glasses when installing, replacing or


aligning hollow cathode lamps. The ultraviolet radiation emitted by these lamps
can harm your eyes.

Refer to the next figure when replacing the Lumina HCL.

Figure 5-7. Replacing the Lumina HCL.

1. Locate and open the lamp compartment door on the right side of the instrument
(if it is not already open). Figure 5-6 shows the location.

2. Remove the old lamp from the lamp mount by carefully grasping it and pulling
it out of the mount.

3. Hold the new lamp in the position shown in Figure 5-7. Make sure the lamp
socket is lined up with the plug on the mount.

4. Carefully insert the new lamp into the mount, gently plugging in the socket to
the plug. Gently push the lamp in until it is fully seated in the mount. Close the
lamp compartment cover.

5. You must now align the lamp. See the procedures in the AAnalyst 100 User’s
Guide (0993-6149) in Chapter 2 - Aligning Lamps.
5-10 Lamps

Replacing the Lumina HCL (Turret Model)

Refer to the next figure when replacing a Lumina HCL in the six-lamp turret.

Figure 5-8. Replacing the Lumina HCL (turret model).

1. Locate and open the lamp compartment door on the right side of the instrument
(if it is not already open). Figure 5-6 shows the location.

2. Remove the old lamp from the turret by carefully grasping it and pulling it out.

3. Hold the new lamp in the position shown in Figure 5-8. Make sure the lamp
socket is lined up with the plug on the turret opening in which the lamp will be
placed.

4. Carefully insert the new lamp into the turret opening, gently plugging in the
socket to the plug. Gently push the lamp in until it is fully seated.

5. Close the lamp compartment cover. Replacement of a Lumina HCL is


complete.
Replacing the Lamps 5-11

Replacing the Coded Intensitron HCL

Always wear UV-absorbing safety glasses when installing, replacing or


aligning hollow cathode lamps. The ultraviolet radiation emitted by these lamps
can harm your eyes.

Refer to the following figure when replacing the coded Intensitron hollow cathode
lamp.

Figure 5-9. Replacing the coded Intensitron HCL.

1. Locate and open the lamp compartment door on the right side of the instrument
(if it is not already open). Figure 5-6 shows the location.

2. Remove the old lamp from the lamp mount by unplugging the lamp cable from
the adapter cable and then carefully grasping the lamp and pulling it out of the
mount.
5-12 Lamps

3. Hold the new lamp in front of the mount in the position shown in Figure 5-9.
Then carefully insert the lamp into the mount. Gently slide the lamp in until it
hits the stop.

4. Plug the existing adapter cable into the connector on the end of the new lamp.

5. Close the lamp compartment cover. Replacement of the lamp is complete.

6. You must now align the lamp. See the procedures in the AAnalyst 100 User’s
Guide (0993-6149) in Chapter 2 - Aligning Lamps.
Replacing the Lamps 5-13

Replacing the Coded Intensitron HCL (Turret Model)


Refer to the following figure when performing the replacement steps below.

Figure 5-10. Replacing the coded Intensitron HCL (turret model).

1. Locate and open the lamp compartment door on the right side of the instrument
(if it is not already open). Figure 5-6 shows the location.
2. Remove the old lamp from the turret by unplugging the lamp cable from the
adapter cable and then carefully grasping the lamp and pulling it out of the
turret.

3. Hold the new lamp in front of the turret in the position shown in Figure 5-10.
Then carefully insert the lamp into the turret. Gently slide the lamp in until it
hits the stop.

4. Plug the existing adapter cable into the connector on the end of the lamp cable.

5. Close the lamp compartment cover. Replacement of the Intensitron HCL is


complete.
5-14 Lamps

Replacing the Non-Coded Intensitron HCL

Always wear UV-absorbing safety glasses when installing, replacing or


aligning hollow cathode lamps. The ultraviolet radiation emitted by these lamps
can harm your eyes.

Refer to the following figure when replacing the non-coded Intensitron lamp.

Figure 5-11. Replacing the non-coded Intensitron HCL.

1. Locate and open the lamp compartment door on the right side of the instrument
(if it is not already open). Figure 5-6 shows the location.
Replacing the Lamps 5-15

2. Remove the old lamp from the lamp mount by unplugging the lamp
cable from the adapter cable and then carefully grasping the lamp and pulling it
out of the mount.

3. Hold the new lamp in front of the mount in the position shown in Figure 5-11.
Then carefully insert the lamp into the mount. Gently slide the lamp in until it
hits the stop.

4. Plug the existing adapter cable into the connector on the end of the new lamp.

5. Close the lamp compartment cover.

6. You must now align the lamp. See the procedures in the AAnalyst 100 User’s
Guide (0993-6149) in Chapter 2 - Aligning Lamps.

7. Replacement of the lamp is complete.


5-16 Lamps

Replacing the Non-coded Intensitron HCL (Turret Model)

Always wear UV-absorbing safety glasses when installing, replacing or


aligning hollow cathode lamps. The ultraviolet radiation emitted by these lamps
can harm your eyes.

Refer to the following figure when performing the replacement steps below.

Figure 5-12. Replacing the non-coded Intensitron HCL (turret model).

1. Locate and open the lamp compartment door on the right side of the instrument.
Figure 5-6 shows the location.
2. Remove the old lamp from the turret by unplugging the lamp cable from the
adapter cable and then carefully grasping the lamp and pulling it out of the
turret.
Replacing the Lamps 5-17

3. Hold the new lamp in front of the turret in the position shown in Figure
5-12. Then carefully insert the lamp into the turret. Gently slide the lamp in
until it hits the stop.

4. Plug the existing adapter cable into the connector on the end of the lamp cable.

5. Close the lamp compartment cover. Replacement is complete.


5-18 Lamps

Replacing the Coded Electrodeless Discharge Lamp

Always wear UV-absorbing safety glasses when installing, replacing or


aligning electrodeless discharge lamps. The ultraviolet radiation emitted by these
lamps can harm your eyes.

If it is determined that the electrodeless discharge lamp (EDL) needs replacing, it is


the lamp sleeve that is usually replaced. Refer to the following figure when
replacing the coded EDL sleeve.

Figure 5-13. Replacing the coded electrodeless discharge lamp.

1. Turn off the power to the EDL Power Supply.

2. Refer to Figure 5-13. Remove the old lamp from the lamp mount by carefully
grasping the lamp around the sleeve and pulling the assembly out of the mount.

3. Push in on the locking pin and slide the lamp sleeve off the driver.
Replacing the Lamps 5-19

4. Slide the new lamp sleeve onto the lamp driver, being sure to depress
the locking pin as the sleeve slides into place. Check that the locking pin is
extended through the locating hole in the sleeve.

5. Hold the assembly in front of the mount in the position shown in Figure 5-13.
Then carefully insert the lamp into the mount. Gently slide the lamp in until it
hits the stop. The lamp cable should already be plugged into the receptacle on
the back of the EDL power supply (check that is still is).

6. If the new EDL is of a different element from the old one, you’ll need to change
the coding plug, too. Remove the old coding plug from the lamp mount. Plug in
the proper coding plug for the new element into the socket on the lamp mount.
7. Turn on the power switch to the EDL Power Supply.

8. You must now align the lamp. See the procedures in the AAnalyst 100 User’s
Guide (0993-6149) in Chapter 2 - Aligning Lamps.

9. Replacement of the lamp is complete.

NOTE: Due to the size of the electrodeless discharge lamps, the lamp
compartment cover must remain open once the EDLs are installed.
5-20 Lamps

Replacing the Coded Electrodeless Discharge Lamp (Turret Model)

Always wear UV-absorbing safety glasses when installing, replacing or


aligning electrodeless discharge lamps. The ultraviolet radiation emitted by these
lamps can harm your eyes.

If it is determined that the electrodeless discharge lamp (EDL) needs replacing, it is


the lamp sleeve that is usually replaced. Refer to the following figure when
replacing the coded EDL sleeve. .

Figure 5-14. Replacing the coded EDL (turret model).

1. Turn off the power to the EDL Power Supply.


Replacing the Lamps 5-21

2. Refer to Figure 5-14. Remove the old lamp from the lamp mount by
carefully grasping the lamp around the sleeve and pulling the assembly out of
the mount.

3. Push in on the locking pin and slide the lamp sleeve off the driver.

4. Slide the new lamp sleeve onto the lamp driver, being sure to depress the
locking pin as the sleeve slides into place. Check that the locking pin is
extended through the locating hole in the sleeve.

5. Hold the assembly in front of the turret in the position shown in Figure 5-14.
Gently slide the lamp in until it hits the stop. The lamp cable should already be
plugged into the receptacle on the back of the EDL power supply (check that is
still is).

6. Turn on the power switch to the EDL Power Supply.

7. If the new EDL is of a different element from the old one, you’ll need to change
the coding plug, too. Remove the old coding plug from the turret. Plug in the
proper coding plug for the new element into the socket on the lamp turret.
Replacement of the lamp is complete.

8. Replacement of the lamp is complete.

NOTE: Due to the size of the electrodeless discharge lamps, the lamp
compartment cover must remain open once the EDLs are installed.
5-22 Lamps

Replacing the Non-Coded Electrodeless Discharge Lamp

Always wear UV-absorbing safety glasses when installing, replacing or


aligning electrodeless discharge lamps. The ultraviolet radiation emitted by these
lamps can harm your eyes.

If it is determined that the electrodeless discharge lamp (EDL) needs replacing, it is


the lamp sleeve that is usually replaced. Refer to the following figure when
replacing the EDL sleeve.

Figure 5-15. Replacing the non-coded electrodeless discharge lamp.

1. Turn off the power to the EDL Power Supply.

2. Refer to Figure 5-15. Remove the old lamp from the lamp mount by carefully
grasping the lamp around the sleeve and pulling the assembly out of the mount.

3. Push in on the locking pin and slide the lamp sleeve off the driver.
Replacing the Lamps 5-23

4. Slide the new lamp sleeve onto the lamp driver, being sure to depress
the locking pin as the sleeve slides into place. Check that the locking pin is
extended through the locating hole in the sleeve.

5. Hold the assembly in front of the mount in the position shown in Figure 5-15.
Then carefully insert the lamp into the mount. Gently slide the lamp in until it
hits the stop. The lamp cable should already be plugged into the receptacle on
the back of the EDL power supply (check that is still is).

6. Turn on the power switch to the EDL Power Supply.

7. You must now align the lamp. See the procedures in the AAnalyst 100 User’s
Guide (0993-6149) in Chapter 2 - Aligning Lamps.

8. Replacement of the lamp is complete.

NOTE: Due to the size of the electrodeless discharge lamps, the lamp
compartment cover must remain open once the EDLs are installed.
5-24 Lamps

Replacing the Non-Coded Electrodeless Discharge Lamp (Turret)

Always wear UV-absorbing safety glasses when installing, replacing or


aligning electrodeless discharge lamps. The ultraviolet radiation emitted by these
lamps can harm your eyes.

Refer to the following figure when performing the replacement steps below. Be
aware that you must program in the lamp information manually.

Figure 5-16. Replacing the non-coded EDL (turret model).

1. Turn off the power to the EDL Power Supply.


Replacing the Lamps 5-25

2. Refer to Figure 5-16. Remove the old lamp from the turret by carefully
grasping the lamp around the sleeve and pulling the assembly out.

3. Push in on the locking pin and slide the lamp sleeve off the driver.

4. Slide the new lamp sleeve onto the lamp driver, being sure to depress the
locking pin as the sleeve slides into place. Check that the locking pin is
extended through the locating hole in the sleeve.

5. Hold the assembly in front of the turret in the position shown in Figure 5-16.
Then carefully insert the lamp into the turret. Gently slide the lamp in until it
hits the stop. The lamp cable should already be plugged into the receptacle on
the back of the EDL power supply (check that is still is).

6. Turn on the power switch to the EDL Power Supply.

7. Replacement of the lamp is complete.

NOTE: Due to the size of the electrodeless discharge lamps, the lamp
compartment cover must remain open once the EDLs are installed.
5-26 Lamps

The Deuterium Arc Background Corrector

The Deuterium Arc Background Corrector is a standard feature with the AAnalyst
300 and is an option for the AAnalyst 100.

An Explanation: The Deuterium Arc Background Corrector

The Deuterium Arc Background Corrector is an internally mounted assembly that


provides simultaneous correction for molecular absorption and light-scattering. The
spectrometer uses a deuterium arc lamp to correct for background absorbance
caused by non-atomic species in the atom cloud.

When the deuterium arc background corrector is used, two alternating sets
of measurements are made: one with the primary source and a second with
the background corrector source. The primary source measures a combination
of background and atomic absorption. The continuum source measures only the
background. The difference between the two measurements yields the atomic
absorption.

A deuterium arc source is used for maximum wavelength coverage and intensity.
The AAnalyst can accurately handle combined atomic plus background absorption
signals as large as 3 absorbance units.
The background corrector is internally installed, with its power supplied from the
instrument. Power to the source is automatically and continuously adjusted to be in
the optimum range for operation. The deuterium arc lamp is easily accessible,
allowing convenient replacement of the lamp by the users. Instructions to replace
the lamp are included in this chapter.

Replacing the Deuterium Arc Background Corrector Lamp

Since the instrument cover will be removed, this procedure should be done by
a skilled person who is trained in the servicing of optical and electrical
components and is aware of the hazards of high voltage electronics.
Replacing the Deuterium Arc Background Corrector Lamp 5-27

Equipment Needed

You’ll need to gather the following items in order to replace the deuterium lamp:
• the deuterium arc lamp - P/N N037-0119
• Ultraviolet-absorbing safety glasses
• phillips head screwdriver

Removing the Deuterium Lamp Assembly

1. Turn OFF the switch and unplug the power cord on the instrument.

Wait a sufficient amount of time for the background corrector lamp to cool
before replacing it. The lamp is very hot after use.

2. Lift up the top cover of the instrument by grasping the front edge on the center
of the cover and lifting. (The cover is hinged in the back and held by magnets
along the front edge of the cover.) Lift it up until it hits the stops at the hinge.

3. Locate the deuterium lamp assembly in the instrument (it is inside the large
triangle block to the left of the lamp compartment).

4. Unscrew the 3 phillips screws that hold the deuterium lamp plate in place.
Don’t let any of the 3 screws drop into the instrument.

5. Carefully lift the assembly away from the housing.

6. Unplug the 3 pin cable from the instrument and feed the connector out through
the opening in the housing.

7. Turn the plate upside down and place it on a workbench (see the next figure).
5-28 Lamps

Figure 5-17. Underside view of the deuterium lamp assembly.

Replacing the Deuterium Lamp

Use great care when handling the deuterium lamp, it is fragile.

Caution When handling the new lamp, do not handle the glass - only the metal lamp
bracket. You don’t want to get fingerprints on the viewing area of the lamp, as this
will decrease the UV performance and damage the lamp.

1. Loosen and remove the thumbscrew and lockwasher that holds the lamp
bracket to the mounting plate (Figure 5-17). The thumbscrew and lockwasher
are not captive, so be careful not to drop them into the instrument. Put them in
a safe place.

2. Remove the old deuterium lamp by grasping the lamp and bracket off of the
mounting plate. You may have to wiggle it while pulling it up and away from
the mounting plate in order to free it from the lower screw.

3. With your other hand, feed the lamp cable and plug through the opening in the
mounting plate to free the lamp from the plate.

NOTE: Remember, when handling the new lamp, do not handle the
glass - only the metal lamp bracket.

4. You are ready to put in the new lamp. Feed the cable of the new lamp through
the opening in the mounting plate, being careful not to touch the glass.
Replacing the Deuterium Arc Background Corrector Lamp 5-29

5. Slide the lamp assembly down over captive screw on the lower part of
the mounting plate as far as it will go.

6. Reinstall the thumbscrew and lockwasher and tighten it hand tight.

Reassembling the Deuterium Lamp Assembly

Next you will put the deuterium lamp assembly back into the instrument.

1. Plug in the lamp cable.

2. Gently set the deuterium lamp plate assembly back into place in the instrument.

3. Reinstall the 3 phillips head screws into the plate and tighten down the cover.

Reassembly is complete. Next you may have to align the deuterium lamp.
Instructions follow.
5-30 Lamps

Aligning the Deuterium Arc Lamp Assembly

Refer to Figure 5-18 when aligning the deuterium lamp.

Figure 5-18. Location of the alignment screws of the deuterium lamp.

1. Set up the standard conditions for copper (including slit).

2. Go to BG mode, and after warming the lamp for several minutes, press
[Energy].
Replacing the Deuterium Arc Background Corrector Lamp 5-31

3. Adjust the X, Y, and Z alignment screws (see Figure 5-18) to obtain


maximum energy/counts as described next in steps 4 - 10. The lock nuts are
self locking - do not loosen.

4. Tweak screws X and Y to obtain the maximum energy.

5. Rotate screw Z (which raises and lowers the lamp) 1/4 turn either clockwise or
counterclockwise.

6. Rotate screw X to obtain maximum energy.

7. Rotate screw Y to "tweak up" the energy.

8. Again observe the counts/energy. If you have a higher number of counts than
you did before you rotated screw Z, repeat steps 5 - 7, rotating screw Z
another 1/4 turn in the same direction.

NOTE: If you have less energy than you did before you first rotated screw Z
1/4 turn, rotate screw Z 1/2 turn in the opposite direction, and repeat steps
6 - 8.

9. Repeat steps 5 - 7 until the energy/counts begins to decrease. Then turn screw
Z a slight amount (∼ 1/8 turn) in the opposite direction that you used to
maximize counts/energy.

(continued on next page)


5-32 Lamps

10. Place a white card in the center of the sample compartment and note the
positions of the beams from the deuterium lamp and the Hollow Cathode Lamp
(Figure 5-19). To complete the peaking procedure, if the beams are not
coincident (the same centers), tweak screws X, Y and Z to center the Hollow
Cathode Lamp beam inside the deuterium arc lamp beam. The next figure
illustrates the “ideal” appearance of the two beams.

Figure 5-19. Centering of the two lamp beams.

The alignment procedure is now complete.


Burner System 6
Introduction to this Chapter.................................................................................. 6-1
Burner System Details........................................................................................... 6-2
How the Burner System Works............................................................................ 6-4
Burner Part Details .............................................................................................6-6
The Nebulizer ................................................................................................. 6-6
The Burner Chamber and End Cap ................................................................. 6-6
The Burner Head ............................................................................................6-7
The Burner Mount ..........................................................................................6-8
The Ignitor Assembly ......................................................................................6-8
The Gas Controls ............................................................................................6-9
The Drain System ......................................................................................... 6-10
Burner Installation .............................................................................................. 6-12
Burner Pre-Ignition Checklist ............................................................................ 6-12
Check: Burner Head is Securely Latched ........................................................... 6-13
Check: Ignitor Box Connectors are Plugged In .................................................. 6-14
Check: Burner End Cap is Tightened Securely .................................................. 6-15
Check: AUX Oxidant, NEB Oxidant and Fuel Hoses are Secure........................ 6-15
Check: Nebulizer is Securely Clamped to the Burner End Cap .......................... 6-16
Check: Main Interlock Connector is Plugged in ................................................ 6-17
Check: Drain Interlock is Plugged In ................................................................ 6-18
Check: Drain Hose is Securely Attached to the Burner End Cap ........................ 6-18
Check: Water is Present in the Drain System Float Assembly ............................ 6-19
6-2 Burner System

Lighting the Burner............................................................................................. 6-20


Burner System Maintenance............................................................................... 6-20
Burner System Troubleshooting.......................................................................... 6-20
Burner Spare Parts and Accessories................................................................... 6-20
Burner System 6
Introduction to this Chapter

The AAnalyst instrument burner system is one of the atomization systems available
for the spectrometer. In general terms, the heat produced by the burner converts the
sample into free atoms that can absorb the light from the source lamp for the
element(s).

This chapter describes in more detail the burner system and includes information on
how to make necessary adjustments and perform routine maintenance.

The purpose of this chapter is to discuss all the hardware related information
pertaining to the burner system. See Chapter 4, Installation, for instructions on
installing the burner assembly and connecting the gas supplies to the instrument.
See the Chapter 7, Maintenance for the burner system maintenance procedures and
when to perform them.

For the step by step procedures to perform analyses using the AAnalyst 100, refer
to the AAnalyst 100 User's Guide (P/N 0993-6149).

For the step by step procedures to perform analyses using the AAnalyst 300, refer
to the AA WinLab Software Guide (P/N 0993-6190).
6-2 Burner System

Burner System Details

The Perkin-Elmer burner system includes all the parts that are assembled onto the
quick change burner mount. The burner assembly is standard equipment on both
the AAnalyst 100 and 300 instruments. It resides in the sample area in the front of
the instrument. The entire burner assembly is shown in the figure below.

Flame Sensor Notch


Burner
Head

Burner (Mixing) Chamber

NEB Side Arm


Ignitor
Burner End Cap Assembly

AUX
Oxidant Hose

FUEL
Inlet Hose Main Interlock
Connector
Mechanical
Nebulizer Interlock
Knob

Capillary
Tube

Drain
Tube Burner Mount
Horizontal
Adjustment Knob NEB Oxidant Hose

Vertical Adjustment Knob Rotational Adjustment Knob

Figure 6-1. The burner assembly and its parts.


Burner System Details 6-3

The major parts of the burner system are listed below and shown in the
simplified figure that follows:
l nebulizer
l burner chamber (including the flow spoiler and end cap)
l burner head
l drain system (not shown)
l gas supply and controls (with a safety interlock system,
all not shown)

Figure 6-2. The major parts of the burner.


6-4 Burner System

How the Burner System Works

The basic AAnalyst instrument includes a burner system for flame sampling
operation. A system block diagram is shown in Figure 6-3. As previously
mentioned, the heat produced by the burner converts the sample into free atoms that
can absorb the light from the source lamp for the element(s).

A sample solution is aspirated through the nebulizer and sprayed as a fine aerosol
mist into the burner chamber. Here, the sample mist is thoroughly mixed with the
fuel and either air or nitrous oxide gases. Fuel gas enters the chamber through the
fuel inlet hose while the oxidant enters through the nebulizer side-arm and the AUX
oxidant inlet.

To prevent incomplete sample atomization, a plastic flow spoiler is placed inside


the chamber directly in front of the nebulizer. Larger sample droplets not carried
around the flow spoiler by the gas flow are forced by the spoiler to the bottom of
the chamber. This, in turn, allows only the finer sample droplets to be carried into
the chamber. The larger droplets are removed through the drain.

Once the sample mist is thoroughly mixed in the chamber, it is carried to the burner
head. Once there, the flame causes dislocation and atomization.

The gas control system monitors and controls fuel and oxidant flows. Burner
operation, including flame ignition, flame shutoff and gas flow settings, is
controlled through the instrument keypad (AAnalyst 100). The AAnalyst 300
burner system is controlled through the computer and the WinLab software.

Figure 6-3 on the next page shows a “block diagram” of how the AAnalyst burner
system flows, from the gas supplies, to the gas box, to the burner hardware itself
and out to the drain vessel.
Burner System Details 6-5

Figure 6-3. Block diagram of the complete burner system.


6-6 Burner System

Burner Part Details

The burner system consists of a nebulizer, chamber, burner head, ignitor, burner
mount, drain system, and built-in gas controls with a safety interlock system. A
premix burner system design is used. Refer to Figure 6-2 while reading about the
burner details to follow.

The Nebulizer

The part of the burner system called the nebulizer (Figure 6-2) is a pneumatic
device used to aspirate the sample solution, creating a fine mist in the burner
chamber. An adjustable Universal GemTip corrosion-resistant, plastic nebulizer
is used. It is ideal for general, all around use when a wide variety of sample types
will be analyzed. The optional High Sensitivity GemTip nebulizer is available for
those applications requiring the utmost in sensitivity and detection limits.

The Burner Chamber and End Cap

Retaining Ring

Burner (Mixing) Chamber

Burner End Cap

Auxiliary Nebulizer
Oxidant Hose
Nebulizer
Oxidant Hose

Fuel Hose

Drain Capillary Tubing

Figure 6-4. Details of the Burner (Mixing) Chamber.


Burner System Details 6-7

The burner system also includes a chemical resistant high-strength plastic


burner (mixing) chamber (Figure 6-4). The chamber is angled to ensure proper
drainage. An impact device (flow spoiler) allows only the finer sample droplets to
be carried into the chamber, removing larger droplets through the drain. In the
chamber, the sample mist is thoroughly mixed with the oxidant-fuel mixture before
ignition takes place. Separate fuel and nebulizer-oxidant hoses connected to the
burner end cap are used to limit combustible gas mixtures to those areas
specifically designed to accommodate them. A separate auxiliary oxidant hose is
included to allow variation of fuel:oxidant flow ratios without varying nebulizer
oxidant flow, thereby maintaining constant, optimum solution aspiration rates.

The Burner Head

All the burner heads are made from titanium. The 10-cm, air-acetylene burner head
is standard with the AAnalyst instruments. All the available burner heads are listed
next in numerical order. Refer to 6-4.
• N040-0100: 5-cm, single-slot burner head (for nitrous oxide-
acetylene operation)
• N040-0101: 5-cm, single-slot burner head (for air-acetylene
operation). It features a wider slot than the nitrous oxide burner head.
• N040-0102: 10-cm, single-slot burner head (for air-acetylene
operation - standard with all burners)
• N040-0103: 10-cm, three-slot burner head (for analysis of high dissolved
solids content solutions with air-acetylene flames).
The 5-cm single-slot air-acetylene burner head is rotatable to 90 degrees.
6-8 Burner System

Figure 6-5. The four available burner heads.

The Burner Mount

The quick change burner mount provides horizontal, vertical, and rotational
adjustment. The quick-disconnect release lever simplifies removal of the burner
assembly. This enables an easy changeover to the HGA-800 Graphite Furnace
operation. Here, the furnace and optional autosampler are mounted on a sampling
arm attached to the side of the instrument that can be easily rotated into place.

The Ignitor Assembly

The ignitor assembly includes the glow plug, the ignitor solenoid and ignitor arm,
the burner head interface circuit, and the flame detect circuit. When the ignitor is
activated (either manually or automatically), the glow plug is energized and heats
up. The ignitor solenoid, which is also energized, swings the ignitor arm into place.
The ignitor arm is a gas-capture tube through which the gases flow from the burner
Burner System Details 6-9

to the glow plug. The gases in the tube are ignited by the heat of the glow
plug, which, in turn, ignite the flame at the burner head slot.

The Gas Controls


AAnalyst 100: The AAnalyst 100 gas controls include flow control for air or
nitrous oxide, and acetylene as well as automatic flame ignition. Automatic, safe
sequencing of gases when lighting or extinguishing a nitrous oxide-acetylene flame
(even in the event of a power failure) is also provided. fuel,

The gas is controlled by the keypad on the instrument. There are three pertinent
keys: [Gases On\Off], [Flame On\Off], and the [N2O] key. Air or N 2O flows to
the nebulizer as well as the AUX supply. If fuel pressure drops too low, the fuel
pressure switch will open, and the flame will shut down in a safe sequence. If the
air pressure drops too low, the air pressure switch will open, and the flame will
shut down in a safe sequence.

Figure 6-6. The gas adjustment knobs on the AAnalyst 100.

AAnalyst 300: The computer provides user friendly control of the gas flows.
Automatic sequencing of gases when lighting or extinguishing a nitrous-oxide-
acetylene flame (even in the event of a power failure) is provided.
6-10 Burner System

The Drain System

Refer to Figure 6-7. During instrument operation, unused sample is drained from
the burner assembly down to a 15-liter (4 gallon) polyethylene bottle through the
drain tube. One end of the drain tube is clamped to the burner end cap, and the
other end to the drain bottle cap.

The drain bottle (vessel) includes an internal trap to make certain that there is back
pressure for the burner chamber. This insures that the air\acetylene mixture does
not enter the bottle. There are two magnetically activated, hermetically sealed reed
float switches in the drain bottle that shut down the AAnalyst flame if the drain
system is not functioning properly. One of the float switches makes certain that
there is enough liquid inside the trap, and the other indicates that the drain bottle is
full, (i.e., they indicate if the liquid level is too high or too low).

The drain is one of the safety interlocks of the AAnalyst. If either of the reed float
switches is activated, an interlock signal shuts down the gases, extinguishing the
flame.
Burner System Details 6-11

Spiral Wrap

Drain Interlock Cable


Connector at Burner
Drain Tubing

Interlock Cable

Retainer Cap

Drain Interlock Float


Switch Assembly

Drain
Vessel

Figure 6-7. The burner drain system and its parts.


6-12 Burner System

Burner Installation

The entire installation of the burner is covered in Chapter 4, Installation of this


manual. The basic steps are bulleted below for your reference. Directions on how
to perform each step are discussed in detail during installation.
• unpacking the instrument (and burner assembly)
• installing the nebulizer on the burner
• checking that the burner end cap is secure
• connecting and securing the gas hoses to the burner
• installing and securing the burner head
• check that the ignitor box connectors are plugged in
• installing the quick-change burner mount assembly into the
instrument
• installing and connecting the burner drain system

Burner Pre-Ignition Checklist

Check all the following items before igniting the flame on the burner. The steps are
listed below and the procedures follow.
• check that the burner head is securely latched
• check that the ignitor box connectors are plugged in
• check that the burner end cap is tightened securely
• check that the auxiliary oxidant, the nebulizer oxidant and the fuel hoses
are securely attached to the burner end cap
• check that the nebulizer is securely clamped to the burner end cap
• check that the main interlock connector is p lugged in
• check that the drain interlock is plugged in
• check that the drain hose is securely attached to the burner end cap
• check that water is present in the drain system float assembly
Burner Pre-Ignition Checklist 6-13

Check: Burner Head is Securely Latched

Refer to the figure below while performing the following steps:

1. Press the tab on the safety latch while lowering the burner head into place.

2. Confirm that the magnetic strip on the burner head ring is positioned around
back and “facing” the ignitor box. (See the left-most drawing below.)

3. Refer to the right-most drawing below. Be sure the burner head is securely
seated in the o-ring. You will know that it is fully seated because the ignitor
arm will swing over the burner.

4. Then release the safety latch. Look at it closely to confirm that the safety latch
“hook” is positioned over the burner head, thereby capturing the ring.

Figure 6-8. Secure the burner head in place with the safety latch.
6-14 Burner System

Check: Ignitor Box Connectors are Plugged In

Refer to the next figure. Locate the three sensor wire connectors inside the rear of
the Ignitor Assembly. Confirm that all three connectors are plugged into the PC
Board.

Rear View of the


Ignitor Box Assembly

3 Connectors
to be Plugged In

Ignitor Box
PC Board

Figure 6-9. Location of the ignitor box connectors.


Burner Pre-Ignition Checklist 6-15

Check: Burner End Cap is Tightened Securely

Make sure the four knurled screws holding the burner end cap to the burner
chamber are tight. See the figure below for the location of the screws.
Nebulizer Clamp
Burner End Cap
Nebulizer
Auxiliary
Oxidant Hose Nebulizer Side Arm

Connector Nut

Nebulizer
Compression Fittings Oxidant Hose

Fuel Hose

Knurled Screws
(typical - 4 places)
Drain Clamp Drain Tube

Figure 6-10. Things to check on the burner end cap.

Check: AUX Oxidant, NEB Oxidant and Fuel Hoses are Secure
Refer to Figure 6-10 above. Make sure the compression fittings holding the
auxiliary oxidant hose and the fuel hose to the burner end cap are tight. If they are
not, tighten the compression fittings hand tight plus a 1/4 turn using two wrenches:
one wrench to hold the nebulizer fitting and the other to turn the compression
fitting.

Confirm that the connector nut holding the nebulizer oxidant hose to the nebulizer
side arm is tight. If it is not, tighten the nut just finger tight.
6-16 Burner System

Check: Nebulizer is Securely Clamped to the Burner End Cap


Refer to the next figure. Make sure that the nebulizer clamp is tightly holding the
nebulizer in place.

1. Locate the nebulizer clamp (Figure 6-11, Detail A) and slide it up while
pushing the nebulizer into the burner end cap. Be sure to orient the nebulizer
side arm so that it will lay in the slot provided. (A gentle twisting and pushing
motion might be necessary to fully seat the nebulizer in the burner end cap.)

2. Lower the nebulizer clamp until it presses against the barrel and flange of the
nebulizer (shaded area). Ensure that the nebulizer is pushed in all the way and
clamped in correctly. Warning, the nebulizer clamp must be lowered and
locked OVER the nebulizer flange. Figure 6-11, Detail B, shows the clamp
lowered and locked correctly over the nebulizer flange.

Figure 6-11. Nebulizer clamp securing the nebulizer flange in place.


Burner Pre-Ignition Checklist 6-17

Check: Main Interlock Connector is Plugged in

Connect the main interlock by inserting the plug into the socket. See the figure
below.

1. Grasp the body of the main interlock connector with your right hand and place
your thumb on the “clear rubber button.”

2. Next, plug the interlock connector into the socket on the back wall of the
sample compartment. You must push it in until the connector mechanically
snaps into place. While doing so, use the main interlock connector body to
press down on the black mechanical interlock knob. When the interlock
connector is completely plugged into the socket (there by pressing down on the
mechanical interlock knob), the burner assembly will be locked in place.
(Rear of
Sample
Compartment)

Socket

Quick-Disconnect Release Plate


Clear Rubber Button
Main Interlock Connector
Mechanical Interlock Knob

Quick-Change Burner Mount Assembly

Figure 6-12. Plugging in the main interlock connector.


6-18 Burner System

Check: Drain Interlock is Plugged In

Locate the drain interlock connector in the figure below. Make sure that it is
plugged in on your instrument.

Burner End Cap Burner Assembly

Drain
Outlet
Drain Clamp

Drain
Tubing Drain
Interlock
Plug
Spiral Drain
Wrap Interlock
Connector
Drain
Interlock
Cable

Figure 6-13. Location of the drain interlock connector.

Check: Drain Hose is Securely Attached to the Burner End Cap


Refer to the figure above. Make sure the drain clamp is securely holding the drain
tubing to the burner end cap.
Burner Pre-Ignition Checklist 6-19

Check: Water is Present in the Drain System Float Assembly

Enough water must be present in the drain system to activate the drain float
assembly. If not, carry out the following procedure. Loosen the drain clamp and
remove the drain tube from the drain outlet of the burner end cap (see Figure
6-13). Pour about 250 mL of water into the drain tube. Reconnect the drain tube to
the burner end cap. Replace the drain hose clamp and tighten securely.

Figure 6-14. The drain system float assembly.


6-20 Burner System

Lighting the Burner

When you are ready to ignite the flame in the burner, you will find the procedures
in Chapter 4, Installation. The information is located in the sections called Post
Installation Adjustments and Checks - Adjusting the Gas Flow for Ignition and
Igniting the Flame. Other flame related procedures can be found in the User’s
Guide (P/N 0993-6149). See the chapter on Igniting and Optimizing the Flame.
Remember, be sure that all the steps listed above have been completed before
attempting to light the burner

Burner System Maintenance

Refer to Chapter 7, Maintenance, in this manual for extensive burner system


maintenance information.

Burner System Troubleshooting

We recommend that you consult the troubleshooting information included in this


manual before you call a Perkin-Elmer service engineer. Refer to Chapter 8,
Troubleshooting, for burner system troubleshooting information. Included are
suggestions to help you determine systematically whether instrument problems are
due to improper analytical techniques, improper selection of instrument parameters,
or a malfunction of the instrument.

Burner Spare Parts and Accessories

Refer to the end of Chapter 7, Maintenance, for burner system spare parts
information.
Maintenance 7
Introduction to this Chapter.................................................................................. 7-1
General Maintenance Checklist............................................................................ 7-2
Instrument Maintenance Checklist....................................................................... 7-2
Cleaning the Instrument........................................................................................ 7-3
Burner System Maintenance Checklist ................................................................ 7-4
Removing the Burner Door ................................................................................... 7-5
Replacing the Burner Door ................................................................................... 7-6
Removing the Burner Assembly from the Instrument.......................................... 7-7
Removing the Burner Head................................................................................... 7-8
Cleaning the Burner Head .................................................................................... 7-9
Frequency ........................................................................................................... 7-9
Quick Cleaning Procedure................................................................................... 7-9
Complete Cleaning Procedure ............................................................................. 7-9
Cleaning the Burner Chamber............................................................................ 7-11
Cleaning the Burner Chamber After Use with Organic Solvents ........................ 7-11
Cleaning the Burner after Aspirating Cu, Ag, or Hg Samples ............................ 7-12
Disassembling the Burner Chamber ................................................................... 7-12
Thoroughly Cleaning the Burner Chamber Parts ............................................... 7-14
Reassembling the Burner .................................................................................... 7-15
Pre-Conditioning a New Burner or Drain Tube................................................. 7-16
7-2 Maintenance

Cleaning the Nebulizer........................................................................................ 7-17


To Clear an Obstruction in the Capillary or Teflon Tubes ................................. 7-17
To Clear an Obstruction in the Nebulizer .......................................................... 7-17
Removing the Nebulizer ...................................................................................... 7-18
Disassembling the Nebulizer............................................................................. 7-19
Cleaning the Disassembled Nebulizer ............................................................... 7-20
Reassembling the Nebulizer ................................................................................ 7-20
Cleaning the High-Sensitivity Nebulizer ........................................................... 7-22
Drain System Maintenance ................................................................................. 7-23
Cleaning (or Flushing) the Drain System .......................................................... 7-24
Replacing the Drain Tubing .............................................................................. 7-24
Preparing the New Drain Tubing for Use .......................................................... 7-25
Cleaning the Drain Float Assembly ................................................................... 7-26
Adding Water to the Drain Float Assembly ....................................................... 7-27
Changing a Fuse .................................................................................................. 7-28
Ordering Supplies and Accessories..................................................................... 7-30
Lamp Maintenance.............................................................................................. 7-30
Primary Source Lamps ...................................................................................... 7-30
Deuterium Arc Lamps ....................................................................................... 7-30
Acetylene Gas Tank Maintenance ...................................................................... 7-31
AS-90 and AS-91 Autosampler Maintenance ..................................................... 7-32
Routine Maintenance ........................................................................................ 7-32
Spare Parts........................................................................................................ 7-32
Servicing........................................................................................................... 7-32
MHS-10 Mercury/Hydride System Maintenance............................................... 7-33
Replacing or Installing the MHS-10 Quartz Cell Holder ................................... 7-33
Replacing or Installing the MHS-10 Quartz Cell onto the Holder ...................... 7-34
HGA-800 Graphite Furnace Maintenance ......................................................... 7-36
Routine Maintenance Checklist......................................................................... 7-36
FIAS-100/400 Maintenance................................................................................. 7-36
Routine Maintenance Checklist......................................................................... 7-36
Spare Parts and Accessories................................................................................ 7-37
Burner and Accessories ..................................................................................... 7-37
Burner Gasket Kit (0047-0988)......................................................................... 7-37
Burner Heads .................................................................................................... 7-37
Nebulizers and Accessories ............................................................................... 7-38
Drain System .................................................................................................... 7-38
Deuterium Arc Background Correction Lamp ................................................... 7-38
Maintenance 7
Introduction to this Chapter
This chapter contains routine maintenance procedures for the AAnalyst instrument
that you can do yourself. Additional maintenance information may be found in the
manuals shipped with the accessories you are using. All other maintenance and
service should be performed by a trained Perkin–Elmer Service Representative.

To reduce the chance of electrical shock, do not remove covers that require
tool access. No user serviceable parts are inside (except for the deuterium arc
background corrector. Refer all other servicing to the Perkin-Elmer qualified
service personnel.

Caution Before using any cleaning or decontamination methods except those specified by
the manufacturer, users should check with the manufacturer that the proposed
method will not damage the equipment.
7-2 Maintenance

General Maintenance Checklist


The following checklist describes general maintenance procedures.
q For safety reasons, and to avoid contaminating new samples, you should
ensure that the work area is kept absolutely clean. This is especially important
when working with toxic substances and when measuring trace amounts of
any elements.
q Clean up spills immediately, using a spill clean-up kit approved by your
organization.

In accordance with safe laboratory practices, spilled material should be cleaned up


and disposed of properly, taking into consideration the following:

l location and size of the spill;


l chemical and physical properties of the material;
l hazardous properties of the material; and
l types of personal protective equipment that might be needed.

Instrument Maintenance Checklist


To properly maintain the spectrometer instrument, do the following as required:
q Clean the exterior of the instrument.
q Inspect and clean any fans and filters.
q Monitor Tank Pressures
q Inspect the burner assembly (see checklist later in this chapter).
q Inspect the drain system.
q Optical: Check the window surfaces in the sample compartment for
fingerprints, dirt, lint, etc. Clean the windows with a tuft of cotton moistened
with a dilute solution of a mild liquid detergent followed by several rinsings
with deionized water.
q If the energy of the primary source lamp is too low, refer to the lamp
troubleshooting information in the Troubleshooting chapter of this manual
(Chapter 8). The lamp may need to be realigned, or replaced if it is old.
Cleaning the Instrument 7-3

Realignment information is in the User’s Guide and replacement information


is in Chapter 5 of this manual.
q If the intensity of the deuterium arc background corrector source is too low,
refer to the troubleshooting information in the Troubleshooting chapter of this
manual. The source lamp may need to be realigned or replaced. Instructions
to do so are in the Lamps chapter of this manual (Chapter 5).
q Normally, the spectrometer optics will require little or no maintenance.
However, low energy lamp readings, or noisy or erratic results may indicate
that the optics require cleaning or alignment. This should only be done by a
Perkin-Elmer service engineer.
A service technician may clean the mirrors by careful use of a clean cotton
cloth moistened with a clean solvent such as alcohol. Quick drying of the
surfaces is important. Do not rub optical surfaces.

Caution If mirror surfaces become dirty (e.g., from exposure to laboratory vapors),
cleaning should be done only by a Perkin-Elmer service engineer. If a service
engineer is not available, a skilled technician may clean the surfaces as described
below. Special care must be taken to avoid scratches, which would require
resurfacing of the mirrors.

Caution Never touch or clean the grating surfaces. Fingerprints or scratches will
adversely affect the dispersion characteristics of the grating and impair the
operation of the instrument.

Caution Before using any cleaning or decontamination methods except those specified by
the manufacturer, users should check with the manufacturer that the proposed
method will not damage the equipment.

Cleaning the Instrument


Exterior surfaces may be cleaned with a soft cloth, dampened with a mild detergent
and water solution. Do not use abrasive cleaners or solvents.
Use the same technique to clean the sample compartment windows, too.
7-4 Maintenance

Burner System Maintenance Checklist


Do the following as required. The procedures are located in this chapter.
q Inspect the condition of the burner head, burner chamber, and nebulizer.
Clean if necessary.
q Clear an obstruction in the nebulizer or capillary tubing using the copper
cleaning wire provided. Only if necessary, disassemble and clean the
nebulizer and o-rings.
q Check the condition of the o-rings, specifically:
the end cap o-ring (or cork gasket) (Figure 7-5)
the burner head o-ring (Figure 7-5) and
the 3 o-rings on the nebulizer (Figure 7-9).
q Visually check for proper flame conditions when igniting the acetylene and
nitrous-oxide flames.
q Clean the burner head whenever the flame becomes uneven.
q Check the drain system regularly for signs of wear and replace if necessary.
Empty the drain vessel before it becomes full. Dispose of hazardous solutions
properly.
q Check the gas hoses for leaks. Call a Perkin-Elmer service engineer if a leak
is detected.
q If analyzing samples with high solids content: Clean the chamber at least
once daily using the cleaning procedure described in this chapter.
q If using organic solvents: When switching from organic to aqueous solvents,
examine the burner chamber for sample deposits and clean if necessary. Flush
the drain tube and empty the vessel. Dispose of hazardous solutions properly.
q If analyzing samples with high concentrations of silver, copper, or mercury:
As previously mentioned, unstable acetylides, which are especially likely to
explode when permitted to dry, may be formed with these sample types when
using an air-acetylene flame. Thoroughly flush the chamber and waste drain
tube with water immediately after this kind of analysis. Inspect the chamber
to be sure that all traces of residue have been removed.
q To avoid acetone carryover which can cause potential damage to the
instrument and an explosion hazard, change the acetylene cylinder when the
cylinder pressure falls below 600 kPa (85 psig).
Removing the Burner Door 7-5

Removing the Burner Door


Refer to the figure below when removing the burner door.

Figure 7-1. Removing the burner door.

1. Swing the door open to about the 45°position.


2. Exert enough upward pressure on the lower left corner of the door to tilt the top
of the door away from the upper door bracket.
3. Lower the door free of the bottom bracket. Removal is complete.
7-6 Maintenance

Replacing the Burner Door


Refer to the figure below when re-installing the burner door.

Figure 7-2. Replacing the burner door.


1. Hold the door in place next to the burner compartment shown in Figure 7-2.
2. Swing the door to the open position. Tilt the top of the door away from the
upper door pin while you push the lower pin up into the hole in the door mount.
3. Drop the top pin down into the upper hole in the door mount while holding the
bottom pin in place. Swing the door while letting it drop down and lock into
place on the hinges.
4. Close the door. Re-installation is complete.
Removing the Burner Assembly from the Instrument 7-7

Removing the Burner Assembly from the Instrument


1. Extinguish the flame, turn off the gases, and power down the instrument. Let
the burner head cool. Open the burner door.
2. Disconnect the drain tube, unplug the drain interlock connector (Figure 7-12).
3. To unplug the main interlock connector (see Figure 7-3), grasp the body of the
connector with your right hand, put your thumb on the clear rubber button,
push the button down and pull the connector out of the socket.

(Rear of
Sample
Compartment)

Socket

Quick-Disconnect Release Plate


Clear Rubber Button
Main Interlock Connector
Mechanical Interlock Knob

Quick-Change Burner Mount Assembly

Figure 7-3. Removing the burner assembly from the instrument.


4. Lift up on the black mechanical interlock knob to free up the burner mount.
5. To take the burner assembly out of the instrument, press down firmly on the
quick-disconnect release plate with one hand while pulling on the quick-change
burner mount assembly with the other. Slide the burner assembly out.
6. Place the burner assembly on a bench, for it is ready for servicing.
7-8 Maintenance

Removing the Burner Head


To remove the burner head, press the tab on the safety latch found on the ignitor
box (Figure 7-4). At the same time, gently pull and twist the burner head in an
upward direction until it comes off the chamber (right most drawing below).

Figure 7-4. Removing the burner head from the burner chamber.
Cleaning the Burner Head 7-9

Cleaning the Burner Head

Frequency
The nature of the samples aspirated determines the burner head cleaning interval.
In ordinary operation, the burner head will need infrequent cleaning.
The burner head should provide an even flame over the length of the burner slot.
An uneven flame may indicate the slot needs cleaning.

Quick Cleaning Procedure


If the instrument is running, extinguish the flame, turn off the gases, and let the
burner head cool. Open the burner door. Carefully work along and between the
burner head slot using the burner head cleaning tool (P/N 0303-1573) provided in
the Spares Kit. Be sure not to nick the edges of the burner slot. (It is strongly
recommended that you use the cleaning tool provided. It looks like a piece of shim
stock and is shipped with the Spares Kit. Other cleaning items may have burrs that
could nick the burner.)

Complete Cleaning Procedure


Cleaning stubborn deposits from the burner head slot may require that you first
remove the burner head from the burner chamber, and then clean it.
1. If the instrument is running, extinguish the flame, turn off the gases, and
power down the instrument. Let the burner head cool. Open the burner door.
2. Remove the burner head. To do so, press the safety latch tab on the ignitor box
while gently pulling and twisting the burner head until it comes off the chamber
(see procedure above).
3. Once the head is removed, carefully work through the slot with the burner head
cleaning tool provided. (Again, it is strongly recommended that you use the
cleaning tool shipped with the instrument to clean the burner head slot.) Do not
nick the edges of the slot. Remove scrapings from inside and outside of the
burner head.
7-10 Maintenance

4. If more cleaning is necessary, the burner head can also be soaked overnight in a
detergent solution and then rinsed with deionized water and blown dry with a
clean air supply.
5. Put the burner head back onto the burner chamber while pressing the safety
latch tab. Position the magnetic strip on the burner head ring around the back
of the assembly - it should face the ignitor box. Release the safety latch. Be
sure the burner head is fully seated on the chamber. A gentle twisting and
pushing may be necessary. You will know that the burner head is fully seated
because the ignitor will swing over the burner.
6. Close the burner door.
Cleaning the Burner Chamber 7-11

Cleaning the Burner Chamber


Again, the nature of the samples aspirated determines the burner chamber cleaning
interval. If only dilute aqueous solutions are routinely analyzed, the burner will not
need frequent cleanings. When samples with high solids content are aspirated, clean
the burner at least daily.
When switching from aqueous to organic solutions, the burner chamber should
always be inspected for deposits and cleaned if necessary.
Be sure to clean the burner chamber after working with organic samples as
described in the section Cleaning the Burner After Use with Organic Solvents.

Unstable acetylides, which are likely to explode when dry, may be formed
when aspirating high concentrations of silver, copper, or mercury salts into an
acetylene flame

Caution If high concentrations of Cu, Ag, or Hg have been aspirated into an acetylene
flame, clean the burner chamber immediately after use by following the
procedures in this section called Cleaning the Burner after Aspirating Cu, Ag, or
Hg Sample.

Cleaning the Burner Chamber After Use with Organic Solvents


If aqueous samples are aspirated right after aspirating organic samples (such as oil
or MIBK extracts), the absorption signal produced can be noisy and erratic. After
aspirating organic samples, use the following procedure to prevent contamination
of subsequent aqueous samples.
1. Aspirate for 5 minutes with an organic solvent miscible with the samples that
have just been aspirated.
2. Aspirate methanol or another solvent miscible with both the organic solvent and
water, for 5 minutes.
3. Aspirate 1% HNO3 for 5 minutes.
4. Flush the drain tube thoroughly with water. Empty the collection vessel and
refill with water. Dispose of hazardous or corrosive solutions properly and
observe local codes concerning the effect of the waste on the environment.
7-12 Maintenance

Cleaning the Burner after Aspirating Cu, Ag, or Hg Samples


As previously mentioned, unstable acetylides (which are likely to explode when
dry), may be formed when aspirating high concentrations of copper, silver, or
mercury salts into an acetylene flame. To help keep the burner chamber clean and
to prevent the buildup of these unstable acetylides, do the following:
1. Aspirate dilute acid (1% HCl) for five minutes before turning off the flame.
2. Extinguish the flame and let the burner head cool.
3. Remove the burner head.
4. Continue to flush the system by slowly pouring about 500 mL of water into the
burner chamber.

Disassembling the Burner Chamber


These procedures assume that you have removed the burner assembly from the
instrument and placed it on a workbench. Next you will disassemble it.
1. Press the safety latch tab on the ignitor box (Figure 7-4) while gently pulling
and twisting the burner head until it comes off the chamber.
2. Unscrew the retaining ring (Figure 7-5) and pull out the burner o-ring.
Disassembling the Burner Chamber 7-13

Burner Head

Magnetic Strip

Retaining Ring

Burner O-Ring
Burner Chamber

End Cap O-Ring/Gasket Plate


Guide Pin
Burner End Cap
Cut-outs
Nebulizer Clamp
Thumbscrews

Thumbscrew (1 of 2)

Flow Spoiler

Nebulizer
Six O'clock Position

Figure 7-5. Exploded view of the burner chamber assembly.


3. Lift the nebulizer clamp and carefully slide out the nebulizer. Put it to the side.
4. If you feel you’ll need to completely remove the end cap from the chamber,
jump down to steps 5 - 7. Otherwise, unscrew the four thumbscrews holding
the burner end cap and carefully let the end cap hang down (you don’t have to
disconnect any of the hoses). Now skip down to step 8.
5. (Optional) To completely remove the burner end cap, perform steps 5 - 7 and
refer to Figure 7-6. Disconnect the auxiliary oxidant hose and the fuel hose
7-14 Maintenance

from the burner end cap using the “double wrench” method (one wrench to
hold the nebulizer fitting and the other to turn the compression fitting).
Burner End Cap
Auxiliary
Oxidant Line

Compression
Fittings
Fuel Line

Drain Clamp
Knurled Screws
(typical - 4 places)
Drain Tube

Figure 7-6. Removing the burner end cap.


6. (Optional) Disconnect the drain tube and clamp (if they are in place).
7. (Optional) Unscrew the four knurled screws holding the end cap to the burner
chamber and carefully remove the end cap.
8. Remove the flow spoiler from inside the burner chamber (Figure 7-5).
9. Unscrew the two thumbscrews holding the burner chamber and plate to the
burner assembly (one thumbscrew can be seen under the burner chamber in
Figure 7-5). Lift the burner chamber and plate from the assembly.
10. Clean the chamber and various parts by following the cleaning procedures
described next.

Thoroughly Cleaning the Burner Chamber Parts


Refer to Figure 7-5 while cleaning the burner parts. All of the o-rings used in the
burner assembly are available in the Spares Kit. The part numbers for the burner
replacement parts can be found at the end of this chapter.
1. If it is not already done, remove and disassemble the burner chamber according
the procedures - Removing the Burner Assembly from the Instrument and
Disassembling the Burner Chamber. Both of these procedures are found
previous to this section.
Reassembling the Burner 7-15

2. To remove the stubborn deposits from inside the burner chamber, from the end
cap, from the flow spoiler and on the burner head, gently scrub them with a
bottle brush and a detergent solution. Be careful not to scratch the inner
surfaces. Be sure to clean the drain outlet thoroughly.
Caution
Do not soak the burner parts in acid or use kitchen-type cleaners. Do not use
abrasive tools. Such chemicals or tools could damage the inner surfaces.

3. Rinse the chamber, end cap, flow spoiler and head thoroughly with deionized
water and allow to dry.
4. If step 2 and 3 did not completely remove the deposits, you should put the parts
in an ultrasonic cleaner. Let them soak in a detergent solution in the machine
until they are completely clean. Remove, rinse with deionized water and allow
to dry.
5. Reassemble the burner chamber according the procedures in this chapter -
Reassembling the Burner.

Reassembling the Burner


Reassemble the burner chamber onto the burner assembly after you have cleaned it
according to the cleaning procedures above.
1. Place the burner chamber and plate back on the burner assembly (be careful
not to hit the nebulizer). Make sure the two guide pins (Figure 7-5) are
protruding through the guide pin cut-outs on the end of the plate before starting
the screws. Tighten down the two thumbscrews.
2. Put the cleaned flow spoiler back into the burner chamber - being sure that one
of the blades is in the six o’clock position (see Figure 7-5).
3. Check that the burner end cap o-ring (or gasket) is properly seated on the inside
groove of the cap and is in good condition. If it is not, replace the rubber o-ring
(0990-2147) or cork gasket (0047-2014), both found in the Spares Kit. Apply
a little Apiezon grease to the rubber o-ring in order to form a good seal with the
chamber. Take care not to let any of the grease get near the insides of the
chamber. If you do, wipe the chamber surface clean with a dry cloth.
4. Place the burner end cap back onto the chamber and tighten the four knurled
screws in an alternate pattern until finger tight. Snug them down by hand one
more time in an alternating pattern.
7-16 Maintenance

5. If they were removed, reconnect the auxiliary oxidant hose and the fuel hose to
the burner end cap. Tighten the compression fittings hand tight plus a 1/4 turn
using two wrenches, one wrench to hold the nebulizer fitting and the other to
turn the compression fitting.
6. Check that the burner o-ring is properly seated on the inside of the burner
chamber (Figure 7-5) and is in good condition. If it is not, replace the o-ring
(0990-2219). Apply a little Apiezon grease to the inner surface of the o-ring to
help form a good seal with the burner head. Take care not to let any of the
grease get near the insides of the chamber.
7. Place the retaining ring back on the burner (Figure 7-5) and hand tighten.
8. Put the burner head back onto the burner chamber while pressing the safety
latch tab. Position the magnetic strip on the burner head ring around the back
of the assembly - it should face the ignitor box. Release the safety latch. Be
sure the burner head is fully seated on the chamber. A gentle twisting and
pushing may be necessary. You will know that the burner head is fully seated
because the ignitor will swing over the burner.
9. Put the burner assembly back into the instrument.
10. Check the burner alignment. You should readjust the burner any time the
burner is cleaned or the burner head is replaced. If necessary, see the section in
the Installation chapter called Post Installation Adjustments and Checks -
Adjusting the Burner Height as well as Adjusting the Burner Position.

Pre-Conditioning a New Burner or Drain Tube


NOTE: This important procedure MUST be performed when a NEW
burner or drain tubing is installed.
This procedure should be done directly after installation of a new burner and
repeated if the drain tube or any of the sample introduction system components are
replaced.
In order for a new sample introduction system to aspirate sample and drain
smoothly, all the internal surfaces need to be prepared. This is easily accomplished
by aspirating a 50/50 solution of water and methanol for approximately 5 minutes.
Refer to the User’s Guide to check the characteristic concentration (Chapter 5,
Igniting and Optimizing the Flame - 7 Check the Characteristic Concentration).
Cleaning the Nebulizer 7-17

Cleaning the Nebulizer


A low absorbance reading may indicate that the burner head or the nebulizer and
sample capillary tube require cleaning. If you find that the burner slot is clean, the
problem is probably due to an obstruction in the capillary tube or nebulizer.

To Clear an Obstruction in the Capillary or Teflon Tubes


1. Aspirate pure solvent with the flame on until the absorbance reading is
satisfactory for a standard.
2. If solvent aspiration fails to clear the sample capillary or Teflon tubes, go on to
the next procedure - To Clear an Obstruction in the Nebulizer.

To Clear an Obstruction in the Nebulizer


1. Remove the sample capillary tube from the Teflon tube protruding out of the
end of the nebulizer (Figure 7-7).

Nebulizer

Teflon Tube
Sample Capillary Tube

Figure 7-7. A close up of the nebulizer.


2. Push the copper cleaning wire (0303-0135, provided with the nebulizer kit)
through the Teflon tube, all the way through the nebulizer and out the sapphire
tip. Move the wire in and out to dislodge any solid particles (it may take
several attempts). Take care not to scratch the nebulizer.

Caution Use only the copper cleaning wire provided with the nebulizer (0303- 0135) to
clean the capillary. Other wire may be burred and can damage the nebulizer.

3. Next, attach a new piece of the sample capillary tube to the nebulizer.
4. Run several standards to determine if the nebulizer has been cleared.
7-18 Maintenance

5. If the absorbance values are still not acceptable, (i.e., deposits have not been
removed using these measures), remove the nebulizer so you can disassemble
and thoroughly clean it (next few sections).

Removing the Nebulizer


The cleaning procedures just described usually suffices enough to restore the
nebulizer to satisfactory working order. The disassembly instructions provided are
seldom needed. However, for deposits which do not yield to either of the cleaning
procedures in the previous 2 sections, it will be necessary to disassemble the
nebulizer and clean it. First, remove the nebulizer according to the steps below.

Caution Do not disassemble the nebulizer unless you are sure that the cleaning
procedure did not sufficiently restore the nebulizers performance. The
performance characteristics of the nebulizer might be modified by disassembly.

1. Extinguish the flame and turn off the gases (if on). Open the burner door.
2. Remove the sample capillary tube (Figure 7-8).

Burner End Cap

Nebulizer Clamp

Nebulizer

Nebulizer Side Arm


Ridges
Side Arm Nut

Black Nebulizer Oxidant Tubing


Sample
Capillary Tube

Figure 7-8. Removing the nebulizer from the burner end cap.
Removing the Nebulizer 7-19

3. Locate the nebulizer clamp, slide it up and hold it there while you carefully pull
the nebulizer out of the burner end cap.
4. Carefully remove the black nebulizer oxidant tubing (NEB) from the nebulizer
side arm. Do this by first loosening the side arm nut. Then, hold the nebulizer
in one hand and with the other hand, gently coax the tubing off the ridges on
the end of the side arm. Removal of the nebulizer is complete.

Disassembling the Nebulizer


This procedure assumes that the nebulizer has been removed from the burner (see
Removing the Nebulizer). Refer to the next figure while doing the following:
1. Unscrew and remove the adjustment nut on the nebulizer body (Figure 7-8).

Figure 7-9. Exploded view of the nebulizer.

2. Next, remove the capillary holder by holding the nebulizer body in your right
hand and pulling the capillary holder out with the left hand.
3. Unscrew and remove the gland nut from the capillary holder.
7-20 Maintenance

Cleaning the Disassembled Nebulizer


1. With the piece of the nebulizer assembly called the capillary holder in one
hand, take the copper cleaning wire (0303-0135) in the other and push it all the
way through the threaded side of the capillary holder and out the sapphire tip.
Move the wire in and out to dislodge any solid particles (it may take several
attempts). Take care not to scratch the insides.

Caution Use only the copper cleaning wire provided with the nebulizer (0303- 0135) to
clean the nebulizer. Other wire may be burred and can damage the nebulizer.

2. Next, gently pull the Teflon tubing out of the gland nut (it may be necessary to
use a needle-nose pliers). Clean the capillary holder, Teflon tubing and gland
nut in an ultrasonic cleaner with distilled water. If they still look dirty, discard
the Teflon tubing and gland nut. Replace them with new ones from the
nebulizer kit. Replacement details are described in the next section.
3. It may be necessary to clean all the parts of the nebulizer in an ultrasonic
cleaner - user’s discretion.
4. Inspect the 3 o-rings (1 on the capillary holder and 2 on the nebulizer body, see
Figure 7-9). They can be cleaned with detergent and water. If they look
damaged, replace them.

Reassembling the Nebulizer


1. Cut a 2.3 cm (0.95 in.) length of the Teflon tubing. Cut a 20 cm (8 in.) length
of the capillary tubing at a 45°angle for ease of insertion (put it aside).
2. Insert the Teflon tubing piece into the threaded end of the gland nut until it is
flush with the knurled edge surface (Figure 7-9).
3. Screw the threaded end of the gland nut onto the capillary holder until it
becomes hard to turn, thereby forcing the tubing back out the other end of the
nut. Doing this will insure that the tubing seats completely inside the capillary
holder.
4. Slide the spring back onto the capillary holder (if it was removed).
5. If you didn’t already do it, inspect the tiny o-ring on the capillary holder for
damage (Figure 7-9). Replace it if necessary. Lightly lubricate the surface of
the o-ring with Apiezon grease. Be sure to keep it off the sapphire tip.
Reassembling the Nebulizer 7-21

6. Slide the assembled capillary holder into the nebulizer body. Line up the
alignment key with the slot in the nebulizer body (see detail - Nebulizer End
View, Figure 7-9). Push the capillary holder in until it bottoms out in the
nebulizer. The spring will take care of the spacing. If you inserted the capillary
holder correctly, it should move freely in and out of the nebulizer. If it does not,
remove and reinstall, paying particular attention to the alignment key.
7. Screw the locking ring onto the nebulizer threads (if it was removed).
8. Screw the adjustment nut onto the nebulizer threads.
9. If you didn’t already do it, inspect the two o-rings on the end of the nebulizer
for damage (Figure 7-9). Replace them if necessary.
10. Lightly lubricate the two o-rings on the end of the nebulizer body with a bit of
Apiezon grease (supplied with the nebulizer).
11. Install the nebulizer onto the burner by lifting up the nebulizer clamp and
sliding the nebulizer in.
12. Connect the black nebulizer oxidant tubing onto the ridges on the nebulizer side
arm. Slide the plastic nut up the black tubing and gently thread it over the
ridges on the side arm. Tighten the plastic nut just finger tight.
13. Connect the new sample capillary tubing to the nebulizer. To ease the job,
expand the opening in the Teflon tubing by pressing and rotating a push-pin
into the tubing protruding out of the nebulizer (refer to Figure 7-10).

Figure 7-10. Attaching new capillary tubing to the nebulizer Teflon tubing.
14. Now that the nebulizer is in place, adjust the aspiration rate as described in the
Installation chapter in the section called - Post Installation Adjustments and
Checks - Adjusting the Nebulizer. Lock the setting by turning the locking ring
counterclockwise (CCW) against the adjustment knob. The procedure is now
complete.
7-22 Maintenance

Cleaning the High-Sensitivity Nebulizer


The same procedures just given for the standard nebulizer can also be used for
removing, disassembling, cleaning and reassembling the high-sensitivity nebulizer.
The only difference is that you have to first carefully remove the impact bead. The
impact bead can also be cleaned using an ultrasonic cleaner. Be sure to handle the
impact bead with care, for it is very fragile.
Refer to the Operating Instructions booklet (0993-6025) that came with your
nebulizer if you feel you need more information.
Drain System Maintenance 7-23

Drain System Maintenance


Drain system maintenance includes cleaning (or flushing) the drain system,
replacing the drain tubing and emptying the drain vessel when full. Replacing the
drain trap and switch assembly must be done by trained service personnel only.
Figure 7-11 shows all the parts of the AAnalyst drain system. It is the same for the
AAnalyst 100 and the AAnalyst 300.
The drain hose and vessel must be checked periodically for wear and/or chemical
attack. The drain tubing should be clear with as few bends as possible. The drain
system should be replaced if it has deteriorated

Retainer
Cap

Drain
Trap
Switch
Assembly

Drain
Spiral Wrap Loop

Drain Interlock
Connector
Interlock Cable
Drain Tubing

Drain
Vessel

Figure 7-11. The burner drain system.


7-24 Maintenance

Cleaning (or Flushing) the Drain System


It is recommended that the drain system be flushed thoroughly with water at the end
of each working day to remove caustic, corrosive, or organic waste materials that
could otherwise damage the burner chamber or drain tubing.
To flush the system, remove the burner head then slowly pour about 500 mL of
water into the burner chamber. Allow the water to drain into the drain vessel.

Replacing the Drain Tubing


If the drain tubing (P/N 0250-7987) is damaged or extremely dirty and needs to be
replaced, refer to the next figure and proceed as described next.

Burner End Cap Burner Assembly

Drain
Outlet
Drain Clamp

Drain
Tubing Drain
Interlock
Plug
Spiral Drain
Wrap Interlock
Connector
Drain
Interlock
Cable

Figure 7-12. Replacing the drain tubing.

1. Turn off the AAnalyst power switch.


2. Remove all effluent from the drain vessel.
Drain System Maintenance 7-25

Dispose of drain vessel waste in accordance with the regulations applicable to


your locality, state, and/or country..

3. Unplug the drain interlock connector from the burner (see Figure 7-12).
4. Disconnect the drain tubing from both the drain vessel and the drain outlet on
the burner end cap by loosening the clamps on each end of the tubing. Once
the clamps are loosened, the tubing should easily pull out.
5. Remove the spiral wrap from the drain tubing by unwrapping it. This will
release the drain interlock cable.
6. Place the new piece of drain tubing (P/N 0250-7987) next to the drain interlock
cable and carefully rewrap the spiral wrap around them both.
7. Place the drain clamp on the upper end of the new drain tubing. Then attach the
tubing to the drain outlet on the burner end cap. Tighten the clamp securely.
8. Place the other drain clamp on the lower end of the drain tubing. Then attach
the tubing to the drain trap switch assembly. Tighten the clamp securely.
9. Plug the drain interlock connector into the receptacle under the burner. Make
sure the interlock connector is plugged in all the way.
10. Go to “Preparing the New Drain Tubing for Use” (next).

Preparing the New Drain Tubing for Use

NOTE: This important procedure MUST be performed at this


point of the drain tube replacement process.
In order for the sample introduction system to drain smoothly, the internal surface
of the new drain tube needs to be prepared. This is easily accomplished when you:
1. Aspirate a 50/50 solution of water and methanol for approximately 5 minutes.
2. Replacement and preparation is now complete.
7-26 Maintenance

Cleaning the Drain Float Assembly


1. Extinguish the flame, turn off the gases (if on) and power down the instrument.
2. Have a bucket or a container of water large enough in which to dip the drain
trap assembly up to the water line. The drain trap (Figure 7-13) is found in the
drain vessel.
3. Unscrew the retainer cap from the drain vessel. Slide out the drain trap
assembly and the drain loop (leaving the tube and wire attached).

Figure 7-13. The drain trap assembly.

4. Clean the drain trap assembly with soap and water using a test tube brush.
5. Rinse with water.
6. Reassemble the system in reverse order.
Drain System Maintenance 7-27

Adding Water to the Drain Float Assembly


Enough water must be present in the drain system to fill the drain loop and to
activate the drain float assembly. If not, carry out the following procedure:
1. Loosen the drain clamp and remove the drain tubing from the drain outlet on
the burner end cap (see Figure 7-12).
2. Pour about 250 mL of water into the drain tubing.
3. Reconnect the drain tubing to the burner end cap. Replace the drain clamp and
tighten securely. Installation of the burner drain is complete.
7-28 Maintenance

Changing a Fuse

To avoid electrical shock, disconnect power supply before changing a fuse.


Disconnect supply whenever cover is removed.

1. Make sure the instrument is switched OFF (the “o” is depressed). Disconnect
the instrument from the line power (if connected).
2. Refer to the figure below. Locate the power entry module on the right side of
the instrument. Insert a small flat-blade screwdriver or similar tool into the
notch, and carefully pry off the power entry module cover. Flip it over to see
the fuses.

Figure 7-14. Pry off the power entry module cover.


3. Carefully remove the existing blown fuse and replace it with the correct fuse
for your operating voltage. Refer to Figure 7-15 and use the following two
tables as a guide when choosing the correct replacement fuse.

Use only fuses with the required current rating and of the specified type for
replacement.
Changing a Fuse 7-29

Single Fuse Configuration:

Voltage: Insert the Following Fuse: Part Number:


100 VAC 6.25 amp, slow blow, 250V, 3AG 0998-1761
120 VAC 6.25 amp, slow blow, 250V, 3AG 0998-1761
220 VAC 3.0 amps, slow blow, 250V, 3AG 0998-1626

Dual Fuse Configuration:

Voltage: Insert the Following Fuse: Part Number:


220 VAC 3.15 amps, slow blow, 250V, metric 0999-1675
230/240 VAC 3.15 amps, slow blow, 250V, metric 0999-1675

Figure 7-15. Changing a fuse.


7-30 Maintenance

Ordering Supplies and Accessories


Supplies, accessories, and replacement parts can be ordered directly from Perkin-
Elmer. Perkin-Elmer offers a full selection of high-quality atomic spectroscopy
supplies through the Atomic Spectroscopy Supplies Catalog.
To place an order for supplies and many replacement parts, to request a free
catalog, or to ask for information, call your local Perkin-Elmer representative.

Lamp Maintenance

Primary Source Lamps


There is really no maintenance procedures for any of the Perkin-Elmer hollow
cathode lamps or the EDLs. If you notice fingerprints on the “window” of your
lamp, wipe them off with a soft, dry, lint free cloth. Use no chemicals or water.
Refer to Chapter 5, Lamps in this manual for information regarding lamp life and
when to replace them.

Deuterium Arc Lamps


There is no maintenance procedures for the deuterium arc background corrector
lamps. Refer to the information at the end of Chapter 5, Lamps (in this manual) if
you need to replace the lamp.
Acetylene Gas Tank Maintenance 7-31

Acetylene Gas Tank Maintenance


Both fuel and oxidant gas hoses should be depressurized at the end of the working
day or if the instrument will not be used for an extended period. Cylinder valves
should be closed to avoid the possibility of pressure regulators failing and gas
hoses being subjected to the full cylinder pressure.
Acetylene is supplied dissolved in acetone, and a small amount of acetone
carryover with the acetylene is normal. However, as tank pressure falls, the relative
amount of acetone entering the gas stream increases and can give erratic results,
particularly for elements such as calcium, tin, chromium, molybdenum and others
whose sensitivity is highly dependent on the fuel/oxidant ratio. For this reason,
acetylene tanks should be replaced when the cylinder pressure drops to about 600
kPa (85 psig). Since the acetylene is dissolved in acetone, the pressure drop is not
linear with gas removal, and a pressure of 600 kPa indicates that the cylinder is
nearly empty, assuming the cylinder is at room temperature.

Change the acetylene cylinder before the cylinder pressure drops below
600 kPa (85 psig). Failure to do so may cause damage to valves or tubing within
the burner gas control system due to high acetone carryover. Such damage can lead
to a serious explosion.

Carefully monitor the cylinder pressure and replace the cylinder as needed. Should
acetone carryover occur, the external gas hoses and tubing should be replaced and
the gas control system should be inspected by a Perkin-Elmer Service Engineer.
Acetylene tanks should always be stored and operated vertically, rather than
horizontally, to prevent liquid acetone from reaching the cylinder valve.
The practice of "cracking the valve" of an acetylene tank (that is, opening the valve
slightly for a very short period previous to attaching the regulator) is not
recommended. While such an action will clear the valve opening of dust or dirt
particles and may remove acetone from the cylinder valve, it is a potentially
hazardous practice and one which should never be attempted in the presence of an
open flame, sparks or other possible sources of ignition.
7-32 Maintenance

AS-90 and AS-91 Autosampler Maintenance


Routine Maintenance
Minimal routine maintenance is required. Keep the carousel clean and try to avoid
spills. Do not use abrasives to clean the clear plastic carousel cover. Do not use
organic solvents to clean the carousel cover.
For more information, refer to the manuals received with the Autosamplers. For the
AS-90, see manual B050-3858 and for the AS-91, see manual B050-9569..

Spare Parts
If corrosive solutions are being routinely analyzed, a corrosion-resistant, platinum-
rhodium probe is available to replace the standard stainless-steel version on the
AS-90 and AS-91 Autosamplers. You may find it convenient to purchase
additional sample carousels, so that samples may be loaded into a second carousel
while the first is still in use. For spare parts, refer to the AS90 or AS91 manuals
provided with the Autosamplers.

Servicing
Servicing of the Autosamplers may only be performed by a trained Perkin-Elmer
Service Representative. Contact your local Perkin-Elmer representative to schedule
a service call.
MHS-10 Mercury/Hydride System Maintenance 7-33

MHS-10 Mercury/Hydride System Maintenance


Refer to the MHS-10 Operator's Manual (B009-8670) for maintenance details.

Replacing or Installing the MHS-10 Quartz Cell Holder


This section describes how to install the quartz cell holder onto the burner head.
The following section describes how to then install the quartz cell.
1. Extinguish the flame (if lit) and allow adequate time for the burner head to
cool.
2. Refer to Figure 7-16. Make sure the two adjusting screws in each clamp are
loose. Place the securing clamps of the cell holder bracket over the ends of the
burner head.

Figure 7-16. Mounting the quartz cell-holder onto the burner head.
7-34 Maintenance

3. Refer to Figure 7-17, and align the "V" in the cell holder with the slot in the
burner head.

Figure 7-17. Adjusting the position of the cell-holder bracket.


4. Tighten the four clamp-adjusting screws.

Replacing or Installing the MHS-10 Quartz Cell onto the Holder


After installing the cell holder, refer to Figures 7-17 and 7-18, and install the
quartz cell as follows:
1. Rotate the cell-holder bracket to the "up" position
2. Place the quartz cell in the cell holder as shown in Figure 7-18.

Be certain that the transfer hose (Figure 7-18) cannot become pinched or
kinked in any way. A restriction in the hose may lead to a pressure buildup in the
system which can cause an explosion.
MHS-10 Mercury/Hydride System Maintenance 7-35

Figure 7-18. Installing the quartz cell onto the holder.


3. Carefully lower the cell-holder bracket to the "down" position.
7-36 Maintenance

HGA-800 Graphite Furnace Maintenance


Refer to the HGA-800 Hardware Guide (0993-5242) for furnace and Graphite
Furnace Autosampler maintenance information.

Routine Maintenance Checklist


q Clean the furnace windows
q Check the graphite tube and contact cylinders.
q Check the pump head, plunger and check valves.
q Check the cooling system water level.
q Maintain the separator trap, filter cartridge, pump, graphite nozzle and nozzle
holder on ZL instruments.

FIAS-100/400 Maintenance
Refer to the manual received with the FIAS-100/400 for maintenance information.

Routine Maintenance Checklist


q Clean the cell and cell windows.
q Check the tubing and connections.
q Rinse and dry the system.
Spare Parts and Accessories 7-37

Spare Parts and Accessories


Following is a partial list of common consumable parts and accessories.

Burner and Accessories


PE Part Number Description
0057-0948 Burner Chamber
N037-0392 End Cap Assembly for 0057-0948
0057-2561 Flow Spoiler
0303-1573 Burner Head Cleaning Tool
0047-0988 Burner Gasket Kit for 0057-0948

Burner Gasket Kit (0047-0988)


PE Part Number Description
0990-2147 Viton O-ring for end cap (general use)
0047-2014 Corpreen Gasket for end cap (organic use)
0990-2219 O-ring on burner chamber (for burner head)
0990-2236 O-ring 1\8 I.D. (impact bead o-ring)
0990-2240 O-ring (end cap/ impact bead o-ring)

Burner Heads
PE Part Number Description
N040-0100 5-cm, single-slot, N 20 / acetylene
N040-0101 5-cm, single-slot, air / acetylene
N040-0102 10-cm, single-slot, air / acetylene (standard)
N040-0103 10-cm, three-slot, air / acetylene
7-38 Maintenance

Nebulizers and Accessories


PE Part Number Description
N037-0394 Standard GemTip Nebulizer Kit
N037-0393 High-Sensitivity GemTip Nebulizer Kit
0303-0405 Apiezon Grease (1 tube)
0998-5708 30 cm (12 in.) length of 0.84-mm I.D. Teflon Tubing
N037-1505 Gland Nut
0303-0135 Cleaning Wires (1 package of 5)
0993-6025 Operating Instructions Booklet, GemTip Nebulizers
0990-8265 Capillary Tubing, 3 meter (10 ft.) length of
0.6-mm I.D.
B050-5086 Impact Bead Structure (for High-Sensitivity GemTip
Nebulizer)

Drain System
PE Part Number Description
0250-7987 Drain tubing

Deuterium Arc Background Correction Lamp


PE Part Number Description
N037-0119 Deuterium Arc Assembly Replacement Lamp
Troubleshooting 8
Introduction to this Chapter.................................................................................. 8-1
Flame Analysis Troubleshooting ........................................................................... 8-2
Flame/Burner Troubleshooting............................................................................. 8-7
Lamp Troubleshooting ........................................................................................ 8-10
Troubleshooting Deuterium Background Corrector Problems .......................... 8-13
Error Messages.................................................................................................... 8-14
Troubleshooting 8
Introduction to this Chapter

The AAnalyst instruments were designed for routine, trouble-free operation.


Although the system is relatively simple to operate, occasional problems may
occur.

We include this chapter of troubleshooting suggestions to help you determine


systematically whether instrument problems are due to improper analytical
techniques, improper selection of instrument parameters, or a malfunction of the
instrument. We recommend that you consult the troubleshooting information
included in this chapter before you call a Perkin-Elmer service engineer.

If, after checking the instrument against the symptoms described in this chapter, the
problem appears to be due to malfunctioning of the instrument, we strongly
recommend that you contact your local Perkin-Elmer Service Representative.
Servicing of the instrument by a person other than a Perkin-Elmer Service
Representative will render the warranty null and void.
8-2 Troubleshooting

Flame Analysis Troubleshooting

Some possible problems associated with flame analyses are listed below along with
probable causes and suggested remedies. It is suggested that you use this checklist
to diagnose possible problems before contacting Perkin-Elmer service for
assistance.

Possible Cause of Problem Check and/or Remedy


Results Corrections may not have been made for Zero the instrument while aspirating
erroneously reagent blank. a reagent blank.
high
Ionization enhancement may be present Add approximately 1000 mg/L of an
in sample or blank. easily ionized salt (such as
potassium, lithium, or lanthanum) to
samples, standards, and blank.
Standard solutions may have deteriorated Restandardize with a proven
or may have been improperly made. standard.
Background absorption (molecular Use a background corrector or, if
absorption, light scattering, etc.) may be applicable, use a nitrous oxide-
present. This is especially likely to occur acetylene flame.
below 330 nm or where a high
concentration of a refractory matrix is
encountered.
The sample matrix may be less viscous Remake the standards in the same
than the standards. matrix as the samples or use the
method of additions.
Flame Analysis Troubleshooting 8-3

Possible Cause of Problem Check and/or Remedy


Results Matrix interferences (chemical, Separate the interferent, match the sample
erroneously low bulk, viscosity) may be present. matrix in your standards, or use the
method of additions. Add matrix modifiers
required to control chemical interferences.
Ionization enhancement may be Add approximately 1000 mg/L of an
present in the standard but not easily ionized salt (such as potassium,
the sample. lithium, or lanthanum) to samples,
standards, and blank.
Standard solutions may have Rerun proven standards.
been improperly made.
Blank solution may be Change blank.
contaminated.
The flame may have been too Refer to the recommended flame
rich or too lean for the element conditions in the Standard Conditions
being determined. window for the element or theAnalytical
Methods manual.
Cannot get You may not be comparing the Recheck the characteristic concentration
close to characteristic concentration for the wavelength.
suggested specified for the wavelength you
characteristic are using.
concentration
Instrument under keypad Use the [Param Entry] key to change the
control: The instrument may not wavelength by ±0.4 nm increments until
be using the correct wavelength. the correct line is found. If a problem is
found, contact a Perkin-Elmer service
engineer for assistance.
Instrument using WinLab: The Use the wavelength scanning function in
instrument may not be using the the software to check the wavelength. If a
correct wavelength. problem is found, contact a Perkin-Elmer
service engineer for assistance.
8-4 Troubleshooting

Possible Cause of Problem Check and/or Remedy


Cannot get If the element is easily ionized, Add approximately 1000 mg/L of an
close to ionization suppressant may be easily ionized salt (such as potassium,
suggested required. lithium, or lanthanum) to samples,
characteristic standards, and blank.
concentration
(continued)
The fuel and oxidant flows may Adjust the gas flows or change to a
not be set properly or the wrong nitrous oxide-acetylene flame if
type of flame may be being used. appropriate.
Slit width may be too wide. Check recommended settings in the
Standard Conditions window for the
element being determined.
Instrument under keypad Adjust the nebulizer using the information
control: Nebulizer may not be given in Chapter 4 in the section:Post
adjusted properly. Installation Adjustments and Checks -
Adjusting the Nebulizer.
Instrument using WinLab: Adjust the nebulizer using the information
Nebulizer may not be adjusted given in Chapter 4 in the section: Post
properly. Installation Adjustments and Checks -
Adjusting the Nebulizer. Also see the AA
WinLab Software Guide (0993-6190).
The nebulizer may be clogged. Clean the nebulizer using the procedure
given in this chapter.
Lamp current may be improperly Reset lamp current.
set (too high).
Too much liquid may be building Check for proper drainage.
up in the burner chamber.
The burner head may be skewed Position the burner head so that it is
in the light path. parallel to the light beam.
Flame Analysis Troubleshooting 8-5

Possible Cause of Problem Check and/or Remedy


The burner position may be Adjust the horizontal, vertical, and
Cannot get close incorrect. rotational position using the information in
to suggested Chapter 4 in the sections: Post
characteristic Installation Adjustments and Checks -
concentration Adjusting the Burner Height and Fine
(continued) Tuning the Burner Position. Also, see the
AA WinLab Software Guide (0993-6190).
The instrument may have been Autozero the instrument while aspirating a
autozeroed while a sample was blank.
being aspirated.
Cannot get Characteristic concentration may Check to make sure the characteristic
suggested not be within 20% of the concentration is within 20% of the
detection limits standard conditions value. specified value. If it is not, refer to the
information on characteristic
concentration above before performing the
following checks.

Instrument under keypad Try higher expansion factor with longer


control: Expansion factor and integration using the [Expand] key.
integration time may be
insufficient.
Instrument using WinLab: Try higher expansion factor with longer
Expansion factor and integration integration using theFixed Expansion
time may be insufficient. window.
Incorrect wavelength may have Use the most sensitive wavelength listed in
been selected. the Standard Conditions window for the
element being determined.
Lamp current may be too low or Increase lamp current or replace lamp.
the lamp may be at the end of its
useful life.
8-6 Troubleshooting

Possible Cause of Problem Check and/or Remedy


Data noisy with Instrument under keypad Check expansion factor and reset if
flame off control: Expansion factor may necessary using the [Expand] key.
be set too high.
Instrument using WinLab: Check expansion factor and reset
Expansion factor may be set too if necessary using the Fixed Expansion
high. window.
Lamp may be unstable or weak. Replace lamp or increase the lamp
current. Or try using the next widest slit
setting. See Chapter 5, Lamps. You can
also refer to the User’s Guide
If noise is more prominent in far Contact a Perkin-Elmer service
ultraviolet range, may indicate representative.
that the optics require cleaning.
Data noisy Burner may be contaminated. Clean the burner head and burner chamber
when aspirating as described in theMaintenance chapter.
blank Check for proper drainage.
Noise may be due to a highly Use background correction or vary the gas
absorbing flame in far ultraviolet flows to minimize flame absorption or
range. maximize flame stability.
Noise may be due to a weak - increase the lamp current to the max rating
lamp coupled with a highly - replace the lamp
absorbing flame. - use the next widest slit setting (although
this may affect the sensitivity)
- select a different wavelength or
- separate analyte element from a highly
emissive matrix by chemical means.
Noise may also be due to acetone Check the acetylene cylinder pressure. For
carryover from the acetylene more information, refer to thePreparing
supply. Your Laboratory chapter in this manual.
Background Background corrector source Refer to the troubleshooting information
correction not lamp may need replacement or on the deuterium arc background corrector
producing alignment. later in this chapter.
expected results
Flame/Burner Troubleshooting 8-7

Flame/Burner Troubleshooting

Possible Cause of Problem Check and/or Remedy


Flame does not Instrument under keypad control: Check the interlock points. The
ignite The interlocks may not be satisfied alpha/numeric display will
(for one or more of the possible prompt you as to which
reasons listed below). interlock is tripped. Refer to the
possible causes listed below.
Instrument using WinLab: The Check to see if the Safety
interlocks may not be satisfied (for one Interlock box in the Flame
or more of the possible reasons listed Control window has a red “X”.
below). If so, check the status of the
interlocks to determine the
specific cause(s). Refer to the
possible causes listed below.
Fuel or oxidant may not be on or at the Check fuel and oxidant. Check
proper pressures. that the pressure is maintained
during the ignition cycle.
The proper burner head may not be Check to make sure the correct
installed or fully seated. The 5-cm burner head is installed, fully
N2O burner head must be used for all seated and secured.
nitrous oxide-acetylene analyses.
(N20/C2H2)
The drain interlock may not be Make sure the drain interlock
connected. connection has been made.
The level of liquid in the drain vessel Pour about 200-300 mL of
may be too low. deionized water into the neck of
the burner or directly into the
top of the drain hose.
The level of liquid in the drain vessel Empty the drain vessel.
may be too high.
The fuel/oxidant flow stopped after 15 Try igniting the flame again.
seconds.
8-8 Troubleshooting

Possible Cause of Problem Check and/or Remedy


Flame does not ignite The thermal shield is too hot. Wait for the shield to cool,
(continued) retry.
The thermal shield interlock is Call PE for service.
defective.
The nebulizer interlock may not be Check that the nebulizer
connected. interlock (on the nebulizer side-
arm) is making contact.
The flame may not ignite if the ignitor Try igniting the flame a second
tube is not positioned directly above or third time.
the burner slot.
Burner flashes back Flashbacks can be caused by any of the Carefully inspect the burner
reasons listed below. system for possible causes,
referring to the ones listed
below. Reignite the flame only
after the problem has been
corrected. Contact a Perkin-
Elmer service representative for
assistance.
Fuel and oxidant gas lines may have Check the connections at the
been inadvertently switched. burner and at the gas supplies.
The burner system may leak. Check the condition of all
O-rings (burner head, end cap,
O-ring on nebulizer front end
cap). Replace O-rings that show
signs of wear (cracking,
swelling). Inspect the inner
surface of the burner chamber
for pitting and replace if
necessary. Check drain
connections for leaks.
Flame/Burner Troubleshooting 8-9

Possible Cause of Problem Check and/or Remedy


Burner flashes back There may be a break or leak in the Inspect tubing and replace if
(continued) drain tubing. necessary.
The burner head may be clogged. Check the burner head and
clean with the shim stock
provided.
Gas flows may be set incorrectly. If running samples in organic
solvents, a flame that is too lean
can cause a flashback. If a lean
flame is required, adjust the
nebulizer uptake rate.
Gas connections may be loose or a leak If you suspect a leak in the gas
may have occurred. lines, immediately close the
cylinder valve. If you need
assistance, contact the gas
supplier or a Perkin-Elmer
service representative. Gas
hoses and connections can be
checked for leaks by applying a
soapy solution and checking to
see if bubbles appear.
The air supply may contain excess Be sure the air supply contains
oxygen. less than 20% oxygen.
The wrong gas supplies may be in use. Check the source of the gases.
8-10 Troubleshooting

Lamp Troubleshooting

Some possible problems are listed below along with probable causes and suggested
remedies. It is suggested that you use this checklist before contacting Perkin-Elmer.

Possible Cause of Problem Check and/or Remedy


Lamp will not fit in If the lamp diameter is smaller than 2 Use the Small Lamp Adapter
the turret inches, it needs a special adapter. Kit (P/N 0303-0870).
Lamp connector If the lamp is non-coded (has a small, Connect the lamp to the turret
will not fit the plug blue or black connector), it needs an using the non-coded lamp
on the instrument adapter. adapter (P/N N305-0198).
If the lamp is not manufactured by Contact the lamp manufacturer
Perkin-Elmer, it may need a special for further information.
adapter cable.
The lamp may not be plugged into the Connect the lamp using an
lamp compartment. adapter cable if necessary.
Lamp is an EDL. EDLs require a special power
supply (see below).
Hollow cathode Instrument is off or not plugged in. Turn instrument on or plug into
lamp will not light line power.
Lamp not plugged in. Connect lamp.
Lamp worn out or damaged. Try another lamp.
Instrument under keypad control: Use [Param Entry] to set the
Insufficient lamp current. proper current.
Instrument under WinLab control: Set current in Align Lamps or
Insufficient lamp current. in Method.
EDL (Electrodeless The lamp may not be connected to the Check the lamp cable; plug it in
Discharge Lamp) EDL power supply. if it is not already.
will not light
EDL power supply not on. Turn on the power supply.
Lamp Troubleshooting 8-11

Possible Causes of Problem Check and/or Remedy

EDL (Electrodeless If the EDL power supply is set to Be sure the modulation cable
Discharge amp) will external modulation, the lamp will not from the EDL power supply is
not light light unless the modulation cable is connected to the plug labeled
(continued) plugged in. "EDL MOD" on the rear of the
instrument.
Lamp energy value The lamp may not be properly aligned. Single lamp unit: Adjust the
is too low position of the lamp. Refer to
the User’s Guide (0993-6149).
Instrument with Turret: the
turret is self aligning (WinLab).
The lamp may be starting to It may be possible to continue
deteriorate. using a hollow cathode lamp for
a short period of time by
increasing the lamp current up
to the maximum value listed on
the label on the lamp.
Otherwise, it may be necessary
to replace the lamp.
The hollow cathode lamp current may Instrument under keypad
be too low. control: Refer to the User’s
Guide (0993-6149) to adjust
the lamp current using the
[Param Entry] key.
Instrument under WinLab
control: Refer to the AA
WinLab Software Guide (0993-
6190) to adjust the lamp current
BOTH: Use the recommended
value for continuous operation
listed on the lamp label.
8-12 Troubleshooting

Possible Causes of Problem Check and/or Remedy

Lamp energy value Instrument under keypad control: Set the instrument lamp current
is too low The electrodeless discharge lamp to 5 mA using [Param Entry]
(continued) current setting may be too low. on the keypad or Align Lamps
in WinLab. Then set the EDL
power supply to the appropriate
current for the mode of
operation (AA or AA-BG). Plug
in the modulation cable between
the back of the instrument and
the EDL power supply. Select
the Modulated mode on the
EDL power supply. Let the
EDL warm up for 20-30 min.
before peaking the lamp.
The slit width may be too small. Check the recommended
settings for the element in the
Standard Conditions window
(or in Analytical Methods for
Atomic Absorption
Spectrometry).
Instrument under keypad control: Using the [Param Entry] key,
The wrong wavelength for the element refer to the Standard Conditions
may be specified. window for the element.
Instrument using WinLab: The Refer to the Standard
wrong wavelength for the element may Conditions window for the
be specified in the method file. element or the manual
Analytical Methods for Atomic
Absorption Spectrometry
(0303-0152, the AA Cookbook)
Troubleshooting Deuterium Background Corrector Problems 8-13

Troubleshooting Deuterium Background Corrector Problems

Background correction requires the use of both the primary and the continuum
source. It is important that these sources be of similar intensity and pass through
exactly the same area of the sample cell. There are three possible problems that
may be observed when the background corrector source lamp is not aligned or
needs replacing:
• Measurements are excessively noisy.
• The intensity of the background source may be much less than the intensit
y of
the primary source. With the AAnalyst using a computer, this error is indicated
by a message that appears either in the Align Lamps window or during the
automatic setup procedure.
• Background absorbance may not be properly corrected. You can check this by
measuring a sample containing only matrix components with no analyte.
These problems indicate that the background corrector source is either not properly
aligned or should be replaced. Refer to the section calledReplacing the Deuterium
Arc Background Corrector in Chapter 5 - Lamps if it needs replacing.

Possible Cause of Problem Check and/or Remedy


Background source May not need to use the Determine if the background corrector
intensity is much background corrector. should be used. It is useful up to about
lower than the 400 nm.
primary source
The intensity is not matched. 1). Reduce the source lamp current or
the EDL current in order to reduce the
primary source intensity. This may
increase the noise for the
determination.
2). In addition (or alternatively)
increase the slit width (this may
increase the possibility of spectral
interferences or increase the calibration
curvature).
The deuterium lamp may need Replace the lamp (see the procedure in
replacing (P/N 0037-0119). Chapter 5, Lamps).
8-14 Troubleshooting

Error Messages

ERR:1 RESULT > THAN ALLOWED FORMAT

ERR:2 EXPANSION > THAN 100

ERR:3 STANDARD IS NOT IN ORDER

ERR:4 STANDARD NOT IN SEQUENCE

ERR:5 RESLOPE STD > THAN HIGH STD

ERR:6 ABS/EM&CONC SIGNS DO NOT MATCH

ERR:7 INVALID CONCENTRATION CURVE

ERR:8 S SHAPED CURVE - 2 COEF USED

ERR:9 SAMPLE CONC > THAN HIGHEST STD

ERR:10 CALIBRATION RANGE EXCEEDED

ERR:11 SAMPLE CONC > MAXIMUM STD

ERR:12 NO CONC VAL. ENTERED FOR STD

ERR:13 RSLP STD > 20% IN ERROR

ERR:14 CORR COEF ERROR

ERR:15 NO CALIB. CURVE FOR RESLOPE

ERR:16 CURVE FIT PROBLEM

ERR:17 CALIB CURVE MAY NOT BE LINEAR

ERR:18 At SIGNAL TOO BIG FOR A/D

ERR:19 BG SIGNAL TOO BIG FOR A/D

ERR:20 MofADD ADDITIONS TOO SMALL


Error Messages 8-15
ERR:21 SIGNAL CHANGES DURING BOC

ERR:22 HI STD > THAN 2 COEF ASYMP.

ERR:23 CAN’T RESLOPE WITH MOFA

ERR:24 RAM ERROR (DEPRESS CE KEY)

ERR:25 ROM ERR (DEPRESS CE KEY)

ERR:26 CHOPPER MTR (DEPRESS CE KEY)

ERR:27 NO A/D IRQ (DEPRESS CE KEY)

ERR:29 MPU ERROR (DEPRESS CE KEY)

ERR:30 LINE FREQ (DEPRESS CE KEY)

ERR:32 BRAM ERROR (DEPRESS CE KEY)

ERR:33 TOO MANY DIGITS

ERR:34 ENTRY MUST BE AN INTEGER

ERR:35 VALUE OUT OF RANGE

ERR:36 TOO MANY DECIMAL PLACES

ERR:38 TOO MANY SIGNIFICANT DIGITS

ERR:39 D2 CURRENT RANGE IS 0 - 255

ERR:40 PMT VOLTAGE RANGE IS 250 - 850 V.

ERR:42 SELECT GAIN WITH ENERGY OR EM

ERR:43 AGC CANNOT ASSIGN CORRECT GAIN

ERR:44 AIC CANNOT ASSIGN CORRECT GAIN

ERR:45 IEEE 488 BUS TIMEOUT

ERR:46 DATA KEY MUST BE SELECTED


8-16 Troubleshooting

ERR:47 AUTOSAMPLER NOT SELECTED

ERR:48 D2 OPTION NOT AVAILABLE

ERR:49 CAN’T SELECT EM WITH ENERGY

ERR:50 CAN'T A/Z IN PARAM ENTRY/ENERGY

ERR:51 PRINTER NOT SELECTED

ERR:52 EMISSION TOO HIGH FOR PMT

ERR:53 AUTOSAMPLER TRAY TYPE ERROR

ERR:54 AUTOSAMPLER FLUSH ERROR

ERR:55 AUTOSAMPLEFR TIME OUT ERROR

ERR:56 REPS HAVE NOT BEEN COMPLETED

ERR:57 CAN’T RECAL. WITH METH OF ADD

ERR:58 SELECT MOFA FOR A/Z FREQ

ERR:59 CAN’T USE A/S FOR PEAK AREA/HT

ERR:60 TOO MANY STD FOR LAST SAMPLE POS

ERR:61 YES/NO ENTRY IS NOT VALID

ERR:62 YES/NO ENTRY IS REQUIRED

ERR:63 STEPS BEFORE ATOM. MUST BE >4 SEC

ERR:64 AUTOSAMPLER NOT AVAILABLE

ERR:65 SAMPLE LOC. MUST BE > LAST STD

ERR:66 SAMPLE LOC. MUST BE < LAST SMP

ERR:67 SELECT NO (0) ON MENU 488

ERR:144 MAX. POWER TEMP TOO LOW <1000


Error Messages 8-17
ERR:145 CHECK HGA POWER. NO COMM.

ERR:146 HGA POWER FAILURE

ERR:147 TOTAL VOLUME MUST BE <100 µL

ERR:148 IEEE CAN’T ACCESS FURNACE

ERR:149 IEEE CAN’T ACCESS FIAS

ERR:150 PARAM ENTRY MUST BE SELECTED

ERR:151 READ PULSE MISSING. CHECK CABLE

ERR:152 PRINTER OUT OF PAPER

ERR:153 PRINTER NOT ONLINE

ERR:154 PRINTER NOT SELECTED

ERR:155 PRINTER TIMEOUT

ERR:156 HGA FURNACE IS OPEN

ERR:157 VALVE AT UNKNOWN POSITION

ERR:158 LAMP NOT FOUND

ERR:159 MENU UNAVAILABLE

ERR:301 AS72 MISSING AUTOSAMPLER

ERR:302 AS72 TAKEUP RANGE ERROR

ERR:303 AS72 NOT READY FOR TAKEUP

ERR:304 AS72 TAKEUP POSITION ERROR

ERR:305 AS72 TAKEUP VOLUME ERROR

ERR:306 AS72 PIPET RANGE ERROR

ERR:307 AS72 NOT READY FOR PIPET


8-18 Troubleshooting

ERR:308 AS72 ROTATE POSITION ERROR

ERR:309 AS72 FLASH RANGE ERROR

ERR:310 AS72 PIPET TEMPERATURE ERROR

ERR:311 AS72 NO FLUSH SOLUTION

ERR:312 AS72 NO PIPET TIMEOUT

ERR:313 AS72 RINSE TIMEOUT

ERR:314 AS72 ET RINSE TIMEOUT

ERR:315 AS72 PIPET TUBE TIMEOUT

ERR:316 AS72 RINSE PUMP UP TIMEOUT

ERR:317 AS72 RINSE PUMP DOWN TIMEOUT

ERR:318 AS72 SAMPLE PUMP UP TIMEOUT

ERR:319 AS72 SAMPLE PUMP LOAD TIMEOUT

ERR:320 AS72 PUMP PREPARATION

ERR:321 AS72 TAKE SAMPLE TIMEOUT

ERR:322 AS72 ROTATE TIMEOUT

ERR:323 AS72 SWING TIMEOUT

ERR:324 AS72 TASK COMMAND ERROR

ERR:325 AS72 POWER ON NOT READY

ERR:326 AS72 BUSY

ERR:327 AS72 RINSE PUMP LOAD TIMEOUT

ERR:401 HGA PAGE PROGRAMMING ERROR

ERR:402 HGA GAS FLOW RANGE ERROR


Error Messages 8-19
ERR:403 HGA GAS TYPE ERROR

ERR:404 HGA TEMP. RANGE ERROR

ERR:405 HGA TEMP. SEQUENCE ERROR

ERR:406 HGA CALIB. TEMP. ERROR

ERR:407 HGA TEMP. CALIB. TIMEOUT

ERR:408: HGA TEMP. CALIB. FAIL ERROR

ERR:409 HGA TEMP. CALIB. SENSOR TIMEOUT

ERR:410 HGA FURNACE OPEN ERROR

ERR:411 HGA RAMP RANGE ERROR

ERR:412 HGA RAMP KIND ERROR

ERR:413 HGA HOLDTIME ERROR

ERR:414 HGA MAXIMUM POWER ERROR

ERR:415 HGA FAST RAMP ERROR

ERR:416 HGA NORMAL RAMP ERROR

ERR:417 HGA READ VALUE ERROR

ERR:418 HGA STEP SEQUENCE ERROR

ERR:419 HGA NOT CALIBRATED

ERR:420 HGA GAS FLOW ERROR

ERR:421 HGA NORMAL GAS ALARM

ERR:422 HGA ALTERNATE GAS ALARM

ERR:423 HGA HIGH TRAFO TEMPERATURE

ERR:424 HGA POWER FAIL


8-20 Troubleshooting

ERR:425 HGA TUBE BREAK ALARM

ERR:426 HGA TUBE ABSENCE ALARM

ERR:427 HGA HIGH FURNACE TEMPERATURE

ERR:428 HGA HIGH MAGNET TEMPERATURE

ERR:429 HGA MAGNET POWER SUPPLY ERROR

ERR:430 HGA MULTI READ ERROR

ERR:431 HGA READ STEP MISSING

ERR:432 HGA MAX. POWER RAMP TIMEOUT

ERR:433 HGA FAST RAMP TIMEOUT

ERR:434 HGA MAGNET POWER ALARM

ERR:435 HGA MAGNET TEMP. ALARM

ERR:436 HGA MANUAL TEMP. ABORTED

ERR:437 HGA NO PAGE LOADED

ERR:438 HGA NO PAGE RUNNING

ERR:439 HGA LAST TASK COMMAND ERROR

ERR:440 HGA POWER ON NOT READY

ERR:441 HGA BUSY

ERR:442 HGA HIGH WATER TEMP.

ERR:443 HGA MANUAL TEMP. RUNNING

ERR:501 HGA/AS72 ALARM ERROR

ERR:502 HGA/AS72 POWER ON NOT READY

ERR:503 HGA/AS72 ILLEGAL PASSWORD


Error Messages 8-21
ERR:504 HGA/AS72 COMMAND DISABLED

ERR:505 HGA/AS72 UNKNOWN PROBLEM

ERR:506 HGA/AS72 INVALID PARAMETER

ERR:507 HGA/AS72 ILLEGAL COMMAND

ERR:508 HGA ALARM NORMAL GAS PRESSURE

ERR:509 HGA ALARM ALTERNATE GAS PRES.

ERR:510 HGA ALARM XFMR. TEMP.

ERR:511 HGA ALARM PWR. CIRCUIT BREAKER

ERR:512 HGA ALARM HIGH FURNACE TEMP.

ERR:513 HGA ALARM MAGNET TEMP. FAIL

ERR:514 HGA ALARM MAGNET POWER FAIL

ERR:515 HGA ALARM GRAPHITE TUBE BREAK (currently not available)

ERR:516 HGA ALARM MANUAL TEMP. RUNNING


8-22 Troubleshooting
Index
A
AA WinLab
controller upgrade, 2-45 lamps, (see Lamp)
kit upgrade, 2-47 manuals, xxviii
software kit, 2-46 optics, 2-8
software, AAnalyst 300, 2-30 options, 2-41
system controller, AAnalyst 100, 2-17 overview, 2-1, 2-2
part numbers, 4-3
AAnalyst 100 post installation adjustments and checks, 4-73
AA WinLab system controller, 2-17 powering up instrument, 4-72
accessory manuals, xxix primary light source, 2-8
assembling, 4-12 printer, 4-68
burner system description, 2-12 sample area, 2-11
carton recycling, 4-6 shipping list, 4-8
data handling, 2-17 spares kit, 4-10
details, 2-6 spectrometer, 2-8
detector, 2-8 system block diagram, 2-4
deuterium arc background corrector, 2-11 system configurations diagram, 2-5
deuterium arc background corrector description, system information, 2-3
5-26 troubleshooting, 8-1
dimensions, 3-3 unpacking, 4-4
documents, xxviii user interface, 2-16
gas control description, 2-14, 6-9
inspecting shipment, 4-3
installation summary, 4-2
interlocks, 2-14 AAnalyst 300
introduction, xxvii AA WinLab software, 2-30
keypad, 2-16 accessory manuals, xxix
lamp compartment, 2-10 automatic six-lamp turret description, 2-26
burner system description, 2-27
carton recycling, 4-6
I-2 Index

warnings, 4-55

AAnalyst 300 (continued) Acid Digestions


description, 2-19 at elevated pressure, 1-31
detector, 2-24 hydrofluoric acid, 1-30
deuterium arc background corrector, 2-26 perchloric acid, 1-30
deuterium arc background corrector description, safety practices, 1-29, 1-31
5-26 Adjustments
dimensions, 3-4 burner height, 4-74
documents, xxviii burner position, 4-78
features, 2-19 gas flow, 4-76
gas control description, 2-28, 6-9 lamp, 4-73
instrument details, 2-23 nebulizer, 4-79
interlocks, 2-28 post installation, 4-73
introduction, xxvii
lamp compartment, 2-26 Air Compressor (see Air Supply)
lamps, (see Lamp)
Air Supply
manuals, xxviii accessories for, 3-13
optics, 2-24 compressor requirements, 3-12
options, 2-41 compressor setup, 4-53
overview, 2-1 connecting, 4-53
part numbers, 4-3 connections diagram, 4-53
primary light source, 2-24 cylinder info, 3-12
sample area, 2-27 cylinder setup, 4-54
spares kit, 4-11 filter part numbers, 4-53
spectrometer, 2-24 requirements, 3-12, 4-53
system information, 2-20 safety practices, 1-14
troubleshooting, 8-1 warning, 3-12
unpacking, 4-4
user interface, 2-28 Air/Acetylene
burner head, 10-cm, 2-44
Acetone burner head, 10-cm, three-slot, 2-44
carryover hazards, 1-19 burner head, 5-cm, 2-44
Acetylene filter assembly, 4-55
accessories for gas supply, 3-15 flame, high temperature use, 3-11
copper warning, 1-14
Aligning
cylinder maintenance, 7-31 lamp assembly, deuterium arc, 5-30
cylinder specifications, 3-14
flash arrestor, 3-14 Argon
grade, 3-14 accessories for gas supply, 3-18
handling, 1-15 graphite furnace use, 1-21
hazards, 1-8 hazards, 1-8
piping, 1-14 liquid, 1-22
requirements, 3-14, 4-55 purity, 3-18, 4-58
safety practices, 1-14 requirements, 3-18, 4-58
storage, 1-15 suffocation, 1-21
supply setup, 4-56 supply setup, 4-58, 4-59
tubing, 3-15
warning, copper, 3-15
warning, gauge pressure, 3-14
warning, leak testing, 4-56
Index I-3
AS-90 or AS-91 (see Autosampler) Blower
dimensions, 3-9
Assembling the Instrument, (see Installation) information, 3-7
kit, 3-7
vent installation, 3-8
Burner
adjusting the height, 4-74
Atomic Absorption
adjusting the position, 4-78
description, xxv
burner head, 2-13
flame AA description, xxvi
graphite furnace AA description, xxvi Burner (continued)
burner mount, 2-13
Atomizers
chamber cleaning, 7-11
description, 2-32
chamber description, 2-13, 6-7
flow injection analysis system, 2-36
chamber disassembling, 7-12
graphite furnace system, 2-32
chamber reassembling, 7-15
mercury/hydride determination system, 2-34
chamber thorough cleaning, 7-14
safety practices, 1-10
checklist, pre-ignition, 6-12
Automatic Six-Lamp Turret description, 6-4
description, 2-26 description, AAnalyst 100, 2-12
electrodeless discharge, installation, 4-48 description, AAnalyst 300, 2-27
lamp installation, EDL, 4-44 door, installing, 4-28
lamp installation, Intensitron HCL, 4-36, 4-40 door, removing, 7-5
lamp installation, Lumina HCL, 4-34 door, replacing, 7-6
lamp replacement, EDL, 5-20, 5-24 drain system description, 6-10
lamp replacement, Intensitron HCL, 5-16 end cap hoses secure, 6-15
lamp replacement, Lumina HCL, 5-10 end cap installation, 4-18
lamp, when to replace, 5-7 end cap o-ring/gasket, replacing, 7-15
lamps, types of, 5-2 end cap tightened securely, 6-15
flow spoiler description, 2-13, 6-7
Autosampler fuel (inlet) hose purpose, 2-13
description, 2-38
gas control description, automatic, 6-9
flame, 2-38
gas hoses, connecting, 4-19
flow injection analysis system, 2-38
gasket kit, 7-37
graphite furnace, 2-40
head description, 6-7
maintenance, 7-32
head, removing, 7-8
manual, AS-90, 7-32
height adjustments, 4-74
manual, AS91, 7-32
ignitor description, 2-13, 6-9
option, 2-42
installation, 4-23
servicing, 7-32
lighting, 4-78, 6-20
spare parts, 7-32
mount description, 6-8
nebulizer clamped securely, 6-16
B nebulizer description, 2-13, 6-6
overview, 6-1
Background Correction Lamp (see Deuterium pre-conditioning, 4-80
Arc Background Corrector) quick-change burner mount, assembling, 4-15
quick-change burner mount, installing, 4-23
Bench
removing from instrument, 7-7
requirements, 3-2
spare parts, 7-37
system layout, 3-3
system details, 6-2
system, how it works, 6-4
I-4 Index

troubleshooting, 6-20, 8-7


Burner Drain System (see Drain System)
Index I-5

Chemical Reagents
Burner Head, 2-13 data sheets, 1-11
air/acetylene, 10-cm, 2-44
definitions of warning, 1-7
air/acetylene, 5-cm, 2-44
disposal, 1-11
air/acetylene, three-slot, 10-cm, 2-44
hydrofluoric acid, 1-26, 1-30
cleaning procedure, complete, 7-9
magnesium perchlorate, 1-27
cleaning procedure, quick, 7-9
mercury/hydride systems, 1-25
description, 6-7
perchloric acid, 1-30
installation, 4-21
protective equipment, 1-11
nitrous oxide, 2-44
safety practices, 1-11
part numbers, 2-44, 6-7
sodium tetrahydroborate, 1-25
removing, 7-8
storage, 1-11
securely latched, 6-13
tin (II) chloride, 1-26
types, 2-44
use, 1-11
warning, burn hazard, 4-81
Cleaning
burner chamber, 7-11
C burner head, 7-9
capillary tubes, 7-17
Cables
drain float assembly, 7-26
drain interlock, 6-18
lamps, 5-7
ignitor box, 6-14
nebulizer, 7-17, 7-20
lamp adapter, 2-43, 4-35, 4-37, 5-5
teflon tube, 7-17
main interlock, plugged in, 6-17
parallel printer, 2-48 Computer System
description, AAnalyst 100, 2-17
Capillary Tubes
cleaning, 7-17 description, AAnalyst 300, 2-29
placement of, 3-3
Carton Recycling upgrade, 2-45
AAnalyst instrument, 4-6
Connecting
Changing acetylene supply, 4-56
fuse, 4-64, 7-28 air compressor, 4-53
air cylinder, 4-54
Checks
air supply, 4-53
burner end cap tightened securely, 6-15
argon supply, 4-59
burner head securely latched, 6-13
drain system, 4-25
burner, pre-ignition, 6-12
EDL power supply, 4-50
drain hose secure, 6-18
electrical supply, 4-60
drain interlock plugged in, 6-18
gas hoses to burner, 4-19
fuel hose secure, 6-15
gas supplies to instrument, 4-52
graphite furnace analysis, 1-22
nitrous oxide, 4-57
ignitor connectors plugged in, 6-14
printer, 4-68
interlock, main, plugged in, 6-17
mercury/hydride systems, 1-24 Conventions Used
nebulizer clamped securely, 6-16 cautions, xxxi
nitrous oxide flame, 4-81 notes, xxxi
oxidant hoses secure, 6-15 warnings, xxxi
post installation, 4-73
pre-ignition, 1-16
water present in drain system, 6-19
I-6 Index

Cooling Accessories, 3-20 water in float, check, 6-19


Corpreen Gasket, 7-15
Customer Service, xxi E
Cyanide Solutions EDL (see Lamp, electrodeless discharge)
hazards, 1-20 EDL Power Supply
installation, 4-50
D Electrical Heater Assembly Adapter
option, 2-42
Data Handling
AAnalyst 100, 2-17 Electrical Safety
AAnalyst 300, 2-30 electrical protection compliance, xvi
FCC compliance, xvi
Detector installation category, xvi
spectrometer, 2-8, 2-24
insulation, xvi
Deuterium Arc Background Corrector pollution degree, xvi
AAnalyst 100, 2-11 safe practices, 1-4
AAnalyst 300, 2-26
Electrical Supply
aligning lamp, 5-30
100/110V operation, 4-62
description, 5-26
220/230V operation, 4-62
lamp, spare, 7-38
240V operation, 4-62
option, 2-42
connecting, 4-60
reassembling, 5-29
fuse block, 4-63
removing lamp assembly, 5-27
fuse block, converting, 4-63
replacing lamp, 5-26, 5-27, 5-28
fuse, changing, 4-64, 7-28
troubleshooting, 8-13
grounded outlet, 4-60
warning about lamp, 5-28
instrument voltage, changing, 4-62
Documents (see Manuals) instrument voltage, setting, 4-61
line cords, 4-66
Door (see Burner) powering up instrument, 4-72
Drain System requirements, 3-19
adding water, 4-27 specifications, 4-60
cleaning the system, 7-24 supply voltage, 4-60
connecting, 4-25 volt amps rating, 4-60
description, 6-10 voltage indicator pin, 4-65
drain float, adding water, 7-27 voltage regulator, 4-60
drain float, cleaning the, 7-26 voltage setting, changing, 4-65
drain float, description, 6-10 warning, altering ground cord, 4-60
drain hose secure, 6-18 Electrodeless Discharge Lamp (see Lamp,
flushing the system, 7-24 electrodeless discharge)
installing, 4-25
interlock, connector location, 4-26 End Cap (see Burner)
interlock, float switches, 6-10
Environmental
interlock, plugged in, 6-18
requirements, 3-2
maintenance, 7-23
safety conditions, 1-2
tubing, flushing the, 7-24
storage requirements, 3-2
tubing, prepare new for use, 7-25
tubing, replacing the drain, 7-24
waste disposal, drain vessel, 1-12
Index I-7
option, 2-41

Exhaust Vent
dimensions, 3-8 Flow Spoiler
installation, 3-8 impact device, 6-7
kit, 3-7 picture, 6-3
requirements, 3-5 purpose, 2-13
sources for tubing, 3-8
Fuel Hose
tubing, 3-8
attached securely, 6-15
purpose, 2-13, 6-7
F Fuse
FCC Compliance, xvi changing, 4-64, 7-28
location diagram, 4-63
FIAS-100 or FIAS-400 see (Flow Injection warning, disconnect power, 7-28
Analysis System)
Fuse Block
Fittings converting the, 4-63
acetylene supply, 3-15 location diagram, 4-63
setting up, 4-63
Flame
autosampler, 2-38 Fusion Mixtures
description, xxvi used for sample preparation, 1-31
igniting, 4-78, 6-20
troubleshooting, 8-7
Flame Analysis
G
acetone carryover, 1-19 Gas
acetylides, 1-20 acetone carryover, 1-19
cyanide solutions, 1-20 acetylene, 1-14
flashbacks, 1-18 air supply, 1-14
hazards, 1-18 cyanide solutions, 1-20
high temperature, 1-19 cylinder handling, 1-10
organic solvents, 1-20 cylinder identification, 1-9
safety interlocks, 1-13 cylinder maintenance, 7-31
safety practices, 1-13 cylinder safety practices, 1-8
troubleshooting, 8-2 cylinder storage, 1-9
flashbacks, 1-18
Flame Gas Controls flow adjustments, 4-76
AAnalyst 100, 2-14, 6-9 flowmeter diagram, 4-77
AAnalyst 300, 2-28, 6-9
hazards, 1-18
automatic, 6-9
hoses, connecting, 4-19
keypad, 6-9
ignition, 1-16
Flashbacks nitrous oxide, 1-15
definition, 1-18 organic solvents, 1-20
possible causes, 8-9 safety practices, 1-13
what to do, 1-18 supply hazards, 1-8
supply requirements, 3-11
Flow Injection Analysis System (FIAS) supply, connecting, 4-52
atomizers, 2-36
autosampler, 2-38 Gas Controls (see Flame Gas Controls)
heater option, 2-42
maintenance, 7-36
I-8 Index

Graphite Furnace I
argon requirements, 3-18
argon, safe use, 1-21 IEC Compliance, xvi
atomizers, 2-32 Igniting the Flame, 4-78, 6-20
description, xxvi, 2-41
dimensions, 3-4 Ignitor
HGA-800, 2-32 connectors plugged in, 4-22, 6-14
interlocks, 1-21 description, 2-13, 6-9
maintenance, 7-36
Inert Gas Supply
safety checks, 1-22 graphite furnace, 1-21
system, 2-32 mercury/hydride system, 1-24
Graphite Furnace Analysis Installation
hazards, 1-22 AAnalyst 100, 4-2
high temperatures, 1-23 acetylene supply, 4-56
inert gas supply, 1-21 air compressor, 4-53
safety practices, 1-21 air cylinder, 4-54
Graphite Furnace Autosampler air/acetylene filter, 4-55
description, 2-40 argon supply, 4-58
option, 2-42 assembling the AAnalyst 100, 4-12
blower, 3-8
burner, 4-23
H burner door, 4-28
burner end cap, 4-18
Hazards burner head, 4-21
chemicals, 1-11
cell holder, MHS-10 quartz, 7-33
compressed gases, 1-8
drain system, 4-25
graphite furnace analysis, 1-22
EDL power supply, 4-50
high temperatures, 1-23, 1-25
fuse block, 4-63
mercury/hydride systems, 1-25
fuse, changing, 4-64, 7-28
ultraviolet radiation, 1-22
gas hoses, connecting, 4-19
HCL (see Lamp, hollow cathode) gas supplies, 4-52
ignitor box connectors, 4-22
Heated Regulator inspecting shipment, 4-3
for nitrous oxide, 3-16 lamp compartment cover, 4-29
HGA-800 (see Graphite Furnace) lamp turret, EDL, 4-44, 4-48
lamp turret, Intensitron HCL, 4-36, 4-40
High Temperatures lamp turret, Lumina HCL, 4-34
warning, burner head, 1-19 lamp, EDL, 4-42, 4-46
warning, graphite furnace analysis, 1-23 lamp, general information, 4-31
warning, mercury/hydride analysis, 1-25 lamp, Intensitron HCL, 4-35, 4-38
Hoses lamp, Lumina HCL, 4-33
drain, securely attached, 6-18 nebulizer, 4-15
fuel, securely attached, 6-15 nitrous oxide supply, 4-57
oxidant, securely attached, 6-15 post installation adjustments, 4-73
powering up instrument, 4-72
Hydrofluoric Acid printer, Okidata 320, 4-68
used in acid digestions, 1-30 quartz cell, 7-34
used with mercury/hydride systems, 1-26 quick-change burner mount, assembling, 4-15
quick-change burner mount, installation, 4-23
sample trays, 4-30
Index I-9
Service Engineer, 4-1, 4-12
Lamp
Installation (continued) adapter cables, 2-43, 5-5
unpacking the AAnalyst 100, 4-3 alignment, 5-7
unpacking the AAnalyst 300, 4-3 cable options, 2-43
vent system, 3-8 cleaning, 5-7
voltage selector board, 4-65 coding plugs, 2-44
water in drain float, 4-27 compartment access and location, 4-32, 5-8
deuterium lamp, aligning, 5-30
Instrument deuterium lamp, description, 5-26
details, AAnalyst 100, 2-6
deuterium lamp, reassembling, 5-29
details, AAnalyst 300, 2-23
deuterium lamp, replacing, 5-28
handling safely, 1-3
disposal, hazardous waste, 1-12
servicing warning, 1-5
EDL, 5-6
warning, proper lifting posture, 4-5
EDL, replacing, 5-18, 5-22
Instrument Setting electrodeless discharge, description, 5-6
changing operating voltage, 4-62 electrodeless discharge, installation, 4-42, 4-44,
voltage, 4-61 4-46
general information, 5-1
Intensitron HCL (see Lamp, Intensitron HCL) HCL, 5-3
Interlock Sensors hollow cathode, description, 5-3
AAnalyst 100, 2-14 installation, general, 4-31
AAnalyst 300, 2-28 Intensitron HCL, description, 5-5
complete listing, 4-22 Intensitron HCL, replacing, 5-11, 5-14
drain float switches, 6-10 Intensitron hollow cathode, installation, 4-35,
drain interlock, plugged in, 4-26, 6-18 4-38, 4-40
flame analysis, 1-13 life, 5-7
graphite furnace, 1-21 Lumina HCL, description, 5-4
ignitor interlock, plugged in, 4-22 Lumina HCL, replacing, 5-9
main interlock, plugged in, 4-24, 6-17 Lumina hollow cathode, installation, 4-33
maintenance, 5-7, 7-30
power supply, EDL, installation, 4-50
replace, when to, 5-7
replacing (see lamp types)
troubleshooting, 8-10
K turret, (see Automatic Six-Lamp Turret)
types used, 5-1
Keypad
warning, eye protection, 4-31
AAnalyst 100, 2-16
warning, UV, 5-8, 5-9
gas control, 6-9
Lamp Adapter Cables, 2-43, 5-5
Lamp Coding Plugs, 2-44
Lamp Compartment
AAnalyst 100, 2-10
L AAnalyst 300, 2-26
Labels on the Instrument, xvii access, 4-32
back, xix cover remains open for EDLs, 4-47, 4-49
inside, xx features, 2-26
right side, xviii installing cover, 4-29
three different types, xvii location, 4-32
I-10 Index

Lamp Turret (see Automatic Six-Lamp who should perform, 7-1


Turret)
Manuals
Lighting the Burner, 4-78, 6-20 accessory, xxix
conventions used, xxxi
Lumina HCL (see Lamp, Lumina HCL) list of manuals, xxviii
Mercury/Hydride Analysis
M hydrofluoric acid, 1-26
Magnesium Perchlorate Mercury/Hydride Determination System
used with amalgam system, 1-27 argon requirements, 3-18
atomizers, 2-34
Main Interlock Connector, (see Interlock
cell holder, installation, 7-33
Sensors)
cell holder, replacing, 7-33
Maintenance chemical hazards, 1-25
acetylene gas tank, 7-31 high temperatures, 1-25
autosampler, 7-32 inert gas supply, 1-24
burner chamber, cleaning, 7-11, 7-14 maintenance, 7-33
burner chamber, disassembling, 7-12 manual P/N, 7-33
burner chamber, reassembling, 7-15 option, 2-41
burner head, complete cleaning procedure, 7-9 quartz cell, installation, 7-34
burner head, quick cleaning procedure, 7-9 quartz cell, replacing, 7-34
burner pre-conditioning, 4-80 safety checks, 1-24
burner, removing for, 7-7 safety practices, 1-24
capillary tubes, 7-17 sodium tetrahydroborate, 1-25
checklist, burner system, 7-4 tin (II) chloride, 1-26
checklist, general, 7-2
checklist, instrument, 7-2 MHS-10 (see Mercury/Hydride Determination
cleaning spills, 7-2 System)
cleaning, instrument, 7-3 Monochromator Optics
cleaning, sample compartment windows, 7-3 spectrometer, 2-8, 2-24
drain float, adding water, 4-27
drain system, 7-23
FIAS, 7-36 N
flushing the drain system, 7-24
Nebulizer
fuse, changing a, 4-64, 7-28
accessories, 7-38
general information, 7-1
adjustment, 4-79
lamp, 5-7
clamped securely, 6-16
lamp, when to replace, 5-7
cleaning, 7-17, 7-20
Mercury/Hydride Determination System, 7-33
cleaning caution, 7-20
nebulizer, cleaning, 7-17, 7-20
cleaning high-sensitivity, 7-22
nebulizer, disassembling, 7-19
description, 2-13, 6-6
nebulizer, reassembling, 7-20
disassembling, 7-19
nebulizer, removing, 7-18
fuel hose attached, 6-15
optical system, 7-2
installation, 4-15
ordering parts, 7-1
oxidant hose attached, 6-15
pre-conditioning, burner, 4-80
reassembling, 7-20
pre-conditioning, burner, new, 7-16
removing, 7-18
pre-conditioning, drain tube, new, 7-16
spare parts, 7-38
replacing drain tubing, 7-24
service engineer, 7-3
teflon tubes, 7-17
Index I-11
Nitrogen Organic Solvents
hazards, 1-8 hazards, 1-20
safety practices, 1-28
Oxidant Hose
Nitrous Oxide attached securely, 6-15
accessories for gas supply, 3-17
burner head, 2-44 Oxygen Use
cap, hose, 4-57 warning, 3-13
connecting, 4-57
cylinder specifications, 3-16
flame, checking, 4-81 P
hazards, 1-8 Parallel Printer Cable, 2-48
heated regulator, 3-16
hose cap P/N, 4-57 Part Numbers
requirements, 3-16 AAnalyst 100, 4-3
safety practices, 1-15 AAnalyst 300, 4-3
supply setup, 4-57 acetylene hose, 4-56
warnings, 3-16 acetylene regulator, 4-56
air dryer filter and regulator, 4-53
Nitrous Oxide/Acetylene Flame air/acetylene filter, 4-53
high temperature use, 3-11 Apiezon grease, 7-38
argon regulator, 4-59
O blower assembly, 3-7
burner end cap, 7-37
Operating Voltage, 4-62 burner gasket kit, 7-37
burner head cleaning tool, 7-9
Options burner heads, 2-44, 6-7, 7-37
burner heads, 2-44 burner o-ring, 7-16
computer system upgrade, 2-45 burner parts, 7-37
deuterium arc corrector, 2-42 cap, nitrous oxide hose, 4-57
electrical heater assembly adapter, 2-42 capillary tubing, 7-38
flame or FIAS autosampler, 2-42 cleaning wires, nebulizer, 7-38
flow injection analysis system, 2-41 computer worktable, 3-3
graphite furnace, 2-41 drain tubing, 7-24
graphite furnace autosampler, 2-42 exhaust vent kit, 3-7
lamp, 2-47 flash arrestor, 4-56
lamp adapter cable, 2-43 fuses, 4-64, 7-28
lamp coding plugs, 2-44 graphite furnace, 2-41
mercury/hydride determination system, 2-41 lamp, adapter cables, 2-43, 4-35
printer cable, parallel, 2-48 lamp, coding plug, 2-44
printer, HP DeskJet 660C, 2-47 lamp, deuterium arc, 7-38
printer, HP LaserJet IV, 2-47 manuals, xxviii
printer, Okidata Microline, 2-47 nebulizer parts, 7-19, 7-38
quartz cell holder, 2-42 ordering parts, 7-1
water cooling system, 2-41 printer cable, parallel, 4-68
Winlab controller kit, 2-45 spare parts, 7-37
WinLab software kit, 2-46 spares kit, 4-10, 4-11
WinLab upgrade kit, 2-47
Perchloric Acid
Ordering used in acid digestions, 1-30
parts, xxi, 7-1
supplies/accessories, xxi, 7-1
I-12 Index

Perkin-Elmer Quick-Change Burner Mount Assembly (see


contacting, xxi Burner)
Plugs
lamp coding, 2-44 R
Post Installation Reagents (see Chemical Reagents)
adjusting the burner position, 4-78
adjusting the lamps, 4-73 Reassembling
adjustments and checks, 4-73 lamp assembly, deuterium arc, 5-29
burner height adjustments, 4-74
Recirculator
burner pre-conditioning, 4-80 cooling system dimensions, 3-20
checking the nitrous oxide flame, 4-81
gas flow adjustments, 4-76 Recycling Carton, 4-6
igniting the flame, 4-78
Removing
nebulizer adjustment, 4-79
burner assembly, 7-7
Powering Up the Instrument, 4-72 burner door, 7-5
burner head, 7-8
Pre-Ignition Checklist deuterium arc lamp assembly, 5-27
burner, 6-12 nebulizer, 7-18
Primary Light Source, 2-8 Replacing
Printer burner door, 7-6
change default settings, 4-69 burner end cap o-ring/gasket, 7-15
connecting, 4-68 burner o-ring, 7-16
HP DeskJet 660C, 2-47 drain tubing, 7-24
HP LaserJet IV, 2-47 fuse, 4-64, 7-28
installation, 4-68 lamp, deuterium arc, 5-26, 5-27, 5-28
Microline, 2-47 lamp, EDL , coded, 5-18
Microline default settings, 4-70, 4-71 lamp, EDL, non-coded, 5-22
Okidata Microline 320, 2-47 lamp, Intensitron HCL, coded, 5-11
parallel cable, 2-48 lamp, Intensitron HCL, non-coded, 5-14
lamp, Lumina HCL, 5-9
Protective Equipment lamp, when to, 5-7
hydrofluoric acid use, 1-27, 1-30 nebulizer capillary holder o-ring, 7-20
safety practices, 1-11 nebulizer o-rings, 7-20
ultraviolet radiation, 1-4 quartz cell holder, MHS-10, 7-33
quartz cell, MHS-10, 7-34
Q turret lamp, EDL, 5-20, 5-24
turret lamp, Intensitron HCL, 5-16
Quartz Cells turret lamp, Lumina HCL, 5-10
cell holder, installing, 7-33
Requirements
for MHS and FIAS systems, 1-24
acetylene supply, 3-14, 4-55
holder option, 2-42
air supply, 3-12, 4-53
installing, 7-34
argon supply, 3-18, 4-58
replacing, 7-34
bench space, 3-2
electrical, 4-60
electrical supply, 3-19
environemental, 3-2
exhaust vent, 3-5
gas supply, 3-11
Index I-13
nitrous oxide requirements, 3-16
storage environement, 3-2
system layout, 3-3
work area, 3-4
I-14 Index

Sample Area
AAnalyst 100, 2-11
S AAnalyst 300, 2-27
Safety Checks (see Checks) Sample Introduction System
pre-conditioning, 4-80
Safety Interlocks (see Interlock Sensors)
Sample Trays
Safety Practices installation, 4-30
acetone carryover, 1-19
acetylene, 1-14 Samples
acetylides, 1-20 safety practices in preparation, 1-28
acid digestions, 1-29, 1-31
Service Engineer
air supply, 1-14
installation, 4-1
argon, 1-21
installation), 4-12
atomizers, 1-10
servicing warning, 1-5
burner gases, 1-13
chemical reagents, 1-11 Servicing
cyanide solutions, 1-20 autosampler, 7-32
drain vessel, 1-12
electrical safety, 1-4 Setup
environmental conditions, 1-2 acetylene supply, 4-56
flame analysis, 1-13 air compressor, 4-53
flame analysis hazards, 1-18 air cylinder, 4-54
flashbacks, 1-18 air/acetylene filter assembly, 4-55
furnace analyses, 1-21 argon supply, 4-58, 4-59
fusion mixtures, 1-31 nitrous oxide supply, 4-57
gas cylinders, 1-8 Shim Stock
guidelines, 1-2 burner cleaning tool, 7-9
handling the instrument, 1-3
high temperature, 1-19 Shipping List
hydroflouric acid, 1-30 AAnalyst 100, 4-8
ignition, 1-16 Sodium Borohydride (see Sodium
inert gas supply, 1-21 Tetrahydroborate)
interlocks, 1-13, 1-21
introduction, 1-1 Sodium Tetrahydroborate
laboratory ventilation, 1-3 used with mercury/hydride systems, 1-25
lamps, primary source, 1-12 Solid Samples
lifting posture, proper, 4-5 dissolving in aqueous solutions, 1-29
mercury/hydride analyses, 1-24 dissolving in organics, 1-28
nitrous oxide, 1-15
organic solvents, 1-20, 1-28 Spare Parts
perchloric acid, 1-30 accessories, 7-37
protective equipment, 1-11 autosampler, 7-32
reagent disposal, 1-11 burner, 7-37
reagent storage, 1-11 burner gasket kit, 7-37
reagent use, 1-11 burner heads, 7-37
sample preparation, 1-28 deuterium arc background correction lamp, 7-38
ultraviolet radiation, 1-3 drain tubing, 7-38
waste disposal, 1-12 nebulizer, 7-38
nebulizer accessories, 7-38
Index I-15
ordering, xxi, 7-1 Tubing
acetylene supply, 3-15
Spares Kit exhaust vent, 3-8
AAnalyst 100, 4-10
AAnalyst 300, 4-11 Turret (see Automatic Six-Lamp Turret)
burner head cleaning tool, 4-10, 4-11
shim stock, 7-9
U
Specifications
(also see Requirements) Ultraviolet Radiation
acetylene, 3-14 explanation, 1-3
argon, 3-18 hazards, 1-22
electrical supply, 4-60 hazards with flame, 1-19
environmental, 3-2 safety practices, 1-3
nitrous oxide, 3-16 warning, eye protection, 4-31
water supply, 3-20 Unpacking
Spectrometer AAnalyst 100, 4-4
AAnalyst 100, 2-8 AAnalyst 300, 4-4
AAnalyst 300, 2-24 User Interface
detector, 2-8, 2-24 AAnalyst 100, 2-16
monochromator optics, 2-8, 2-24 AAnalyst 300, 2-28
primary light source, 2-8, 2-24
Stannous Chloride (see Tin (II) Chloride)
V
Supplies
ordering, xxi, 7-1 Ventilation
(see Exhaust Vent)
Symbols
graphics on the instrument, xvii Voltage Selector Board
labels on the instrument, xviii, xix, xx change setting, 4-65
warnings on the instrument, xvii location diagram, 4-65

System Information Voltage Setting, 4-61


AAnalyst 100, 2-3
AAnalyst 300, 2-20
W
System Layout, 3-3
Warnings
acetone carryover, 1-19
T acetylene, 1-14, 4-55
acetylene and copper, 1-14, 3-15
Tin (II) Chloride acetylene cylinder pressure drop, 7-31
used with mercury/hydride systems, 1-26 acetylene gauge pressure, 3-14
acetylene tank pressure, 4-77
Troubleshooting
burner problems, 8-7 acetylides, 1-20
deuterium arc background corrector, 8-13 air supply, 3-12
error messages, 8-14 argon safety data sheet, 1-21
flame analysis problems, 8-2 burn hazard, 1-25, 4-81, 5-27
flame problems, 8-7 burns, how to avoid, 1-10
interlock not satisfied, 4-78 chemical reagents, 1-11
introduction, 8-1 covers, don’t remove, 7-1
lamp problems, 8-10 covers, if removed, 5-26
covers, off instrument, 1-4
I-16 Index

cyanide solutions, 1-20 ultraviolet radiation protection, 1-4


cyanogen gas (C2N2), 1-21 volatile organic solvents, 1-20
definition of a caution, xxxi waste disposal, 1-12, 7-25
definition of a note, xxxi

Waste Disposal
Warnings (continued)
drain vessel, 1-12, 7-25
definition of a warning, xxxi
primary source lamps, 1-12
deuterium arc lamp, handling, 5-28
procedues, 1-12
don’t view flame, 1-19
warning, 1-12
electrical shock, avoid, 1-5
exhaust system, 3-5 Water Cooling System, 2-41
explosion hazard, FIAS quartz cell, 1-24
explosion hazards, 1-20 WinLab (see AA WinLab)
eye protection, 1-28, 4-31, 4-78 Work Area Location, 3-4
flashbacks, 1-18
follow instructions in manual, xv, xxx
fuses, disconnect power, 7-28
fuses, proper, 1-5, 7-28
gas cylinders, 1-8
gas supply, 1-13
graphite furnace, let cool, 1-23
ground connection, protective, 1-4
ground cord, altering, 4-60
grounding circuit, 1-4, 3-19
handling deuterium arc lamp, 5-28
hazardous chemicals, 1-7
high temperatures, 1-19, 5-27
hot burner head, 4-81
hot lamp, 5-27
hydrofluoric acid, 1-27, 1-30
interlocks, defeating, 1-13
labels on the instrument, xviii, xix, xx
leak testing, 4-56
lethal voltages, 1-5
lifting posture, proper, 4-5
magnesium perchlorate, 1-27
make no adjustments-except..., 1-5
MSDS’s, 1-7
nebulizer, adjusting, 4-79
nitrous oxide, 1-15, 3-16
no chemical hoods, 3-5
oxygen use, 1-14, 3-13
perchloric acid, 1-30
pressure digestions, 1-31
quartz cell hose kink, 7-34
safety interlocks, 1-21
servicing instrument, 1-5
sodium tetrahydroborate (NaBH4), 1-25
symbols used on instrument, xvii
tin (II) chloride (SnCl2), 1-26
ultraviolet radiation, 1-22

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