Hardware Guide
Hardware Guide
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Copyright © 1998 The Perkin-Elmer Corporation.
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Manual
Part No. Release Release Date
0993-6088 Rev. E June 1998
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Intensitron is a registered trademark of The Perkin-Elmer Corporation.
GemTip is a trademark of The Perkin-Elmer Corporation.
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AAnalyst is a trademark of The Perkin-Elmer Corporation.
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Contents
Contents......................................................................................i
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
Index
xi
List of Figures
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 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 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.
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
The three different types of warning symbols that appear on the AAnalyst
instrument are reprinted below:
Alternating current.
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.
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.
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.
G J
Serial Number
Norwalk, CT 06859 USA
AAnalyst 100
Part No.
Serial No.
Patents pending
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.
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.
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.
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
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.
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
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
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.
Manual Conventions
In this manual, the following special formats are used to set apart important
information, warnings and notes:
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
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.
This safety chapter is divided into sections that cover both general practices as well
as practices related to specific types of atomic absorption analyses.
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.
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
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.
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.
This section describes potential hazards with any atomic absorption analysis and
recommended safety practices.
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
Electrical Safety
The instrument has been designed to protect the operator from potential electrical
hazards. This section describes some recommended electrical safety practices.
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
Use only fuses with the required current rating and of the specified type for
replacement.
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].
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.
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
• 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.
• 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.
• 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.
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
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.
• Clean up spills immediately using the appropriate equipment and supplies such
as spill cleanup kits.
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.
• 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.
• 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
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.
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.
Air Supply
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
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.
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.
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.
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.
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.
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.
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.
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
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.
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
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
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.
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.
Safety Checks
The following additional potential hazards are associated with furnace analyses.
UV 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
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
This section covers mercury/hydride analyses performed with the MHS-10 or with
Flow Injection (FIAS).
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
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
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.
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.
Magnesium Perchlorate
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.
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.
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.
More information about the behavior of organic solvents with atomic spectroscopy
equipment is given in Reference 12 .
Acid Digestions
Perchloric acid and hydrofluoric acid are particularly hazardous to work with.
1-30 Safety Practices
Perchloric Acid
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.
Performing Digestions
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
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
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.
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
For
For For Flame - FIAS
Flame AA Graphite Furnace AA Manual System
Manual System Manual System
- Burner
- Burner - HGA-800
- FIAS 100/400
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
Removable
Burner Door
Atomizing
Source
(burner)
Drain
Vessel
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 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.
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.
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
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.
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
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 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
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.
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
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.
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.
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
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)
Drain
Vessel
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 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
Access to the lamp compartment in the AAnalyst 300 is from the front of the
spectrometer, allowing for easy lamp installation and removal.
The AAnalyst 300 instrument includes a six-lamp turret as a standard feature. See
the turret details next under Automatic Six-Lamp Turret.
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.
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.
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
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 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.
The AAnalyst 300 system includes a system controller. Its components are
described in the next few sections.
AAnalyst 300 Instrument Details 2-29
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 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 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
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.
Atomizers
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).
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
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.
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 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.
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
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
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.
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:
144 sample vessels 4.5 mL, 6 mL 218 sample vessels 4.5 mL, 6 mL,
8 mL
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
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.
Refer to the section earlier in this manual (Atomizers - Flow Injection Analysis
System) for the full FIAS details.
2-42 System Descriptions
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).
Refer to the section earlier in this chapter for the autosampler details (Autosampler
-Graphite Furnace Autosampler).
Required to mount the optional Quartz Cell Electrical Heating Assembly for the
FIAS-100 or FIAS-400 on the AAnalyst instrument.
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
Allows the coded Intensitron-series hollow cathode lamps to be used with the
AAnalyst instruments. See the figure below.
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.
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.
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
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 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)
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
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.)
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.
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.
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
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.
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).
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 3-2. Dimensions of the AAnalyst 300, HGA-800 Furnace and chiller.
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
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.
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.)
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.
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
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.
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
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
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.
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.
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.
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.
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
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%.
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.
Instructions to hook up the air supply to the instrument are located in the Installation
chapter.
Gas Supply Requirements 3-15
Acetylene is used almost exclusively as the fuel for the flames used in atomic
absorption.
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.
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.
Instructions to hook up the acetylene supply to the instrument are located in the
Installation chapter.
Gas Supply Requirements 3-17
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.
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.
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.
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.
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.
Electrical Requirements
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.
20.5cm
Depth: (8 in.)
51cm
(20 in.) P-E Furnace
Cooling System
35cm Recirculator
(13.75 in.)
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.
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
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.
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).
To collapse and store the carton, follow these instructions and refer to the next
figure.
Unpacking the AAnalyst 100 Instrument 4-7
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.
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
Burner Door
Nebulizer Assembly
Unpacking the AAnalyst 100 Instrument 4-9
Description
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.
The following items are included in the AAnalyst 300 Spares Kit
(P/N N041-0099). The kit is shipped with the instrument.
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.
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.
The next few sections describe the steps necessary to prepare the quick-change
burner mount assembly for installation into the instrument:
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
Burner Chamber
Nebulizer Clamp
O-rings
Nebulizer
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.
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
Burner Chamber
Knurled Screws
(typical 4 places)
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
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
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.
3 Connectors
to be Plugged In
Ignitor Box
PC Board
(Rear of
Sample Compartment)
Tracks (1of 2)
Quick-Disconnect
Release Plate
(Interlock Connector, ref)
Fittings (1 of 3)
Quick Change
Burner Mount Assembly
(Rear of
Sample
Compartment)
Socket
Retainer
Cap
Drain
Trap
Switch
Assembly
Drain
Spiral Wrap Loop
Drain Interlock
Connector
Interlock Cable
Drain Tubing
Drain
Vessel
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.
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
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
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
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
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
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
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
Refer to the next figure when installing the Lumina HCL into the six-lamp turret.
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
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.
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
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.
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
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.
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
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.
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.
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
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.
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
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.
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
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.
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
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
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.
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.
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.
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.
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
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
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.
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!
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.
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.
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.
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
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.
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.
For example, the figure below shows that the instrument is set to run at 220 VAC.
Figure 4-35. Location of the power entry module and ON/OFF switch.
4-62 Installation
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.
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.
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.
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.
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.
The line cord should have the electrical rating and plug appropriate for your
location. See Figure 4-41 for the correct cord.
Figure 4-41. The AC line cord selections for the AAnalyst instrument.
4-68 Installation
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.
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, 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
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:
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:
PERKIN-ELMER AANALYST
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
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
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.
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:
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).
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
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.)
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.
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
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.
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.
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.
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.
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
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.
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
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.
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.
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
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.
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 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
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
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
Refer to the next figure when replacing a Lumina HCL in the six-lamp turret.
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.
Refer to the following figure when replacing the coded Intensitron hollow cathode
lamp.
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.
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
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.
Refer to the following figure when replacing the non-coded Intensitron lamp.
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.
6. You must now align the lamp. See the procedures in the AAnalyst 100 User’s
Guide (0993-6149) in Chapter 2 - Aligning Lamps.
Refer to the following figure when performing the replacement steps below.
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.
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.
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
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).
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.
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
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).
7. You must now align the lamp. See the procedures in the AAnalyst 100 User’s
Guide (0993-6149) in Chapter 2 - Aligning Lamps.
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
Refer to the following figure when performing the replacement steps below. Be
aware that you must program in the lamp information manually.
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).
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 is a standard feature with the AAnalyst
300 and is an option for the AAnalyst 100.
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.
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
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.
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
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.
Next you will put the deuterium lamp assembly back into the instrument.
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
2. Go to BG mode, and after warming the lamp for several minutes, press
[Energy].
Replacing the Deuterium Arc Background Corrector Lamp 5-31
5. Rotate screw Z (which raises and lowers the lamp) 1/4 turn either clockwise or
counterclockwise.
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.
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.
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
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.
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
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)
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.
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
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.
Retaining Ring
Auxiliary Nebulizer
Oxidant Hose
Nebulizer
Oxidant Hose
Fuel Hose
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
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 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 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.
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
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
Interlock Cable
Retainer Cap
Drain
Vessel
Burner Installation
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
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
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.
3 Connectors
to be Plugged In
Ignitor Box
PC Board
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
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
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.
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
Locate the drain interlock connector in the figure below. Make sure that it is
plugged in on your instrument.
Drain
Outlet
Drain Clamp
Drain
Tubing Drain
Interlock
Plug
Spiral Drain
Wrap Interlock
Connector
Drain
Interlock
Cable
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.
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
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
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
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.
(Rear of
Sample
Compartment)
Socket
Figure 7-4. Removing the burner head from the burner chamber.
Cleaning the Burner Head 7-9
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.
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
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.
Burner Head
Magnetic Strip
Retaining Ring
Burner O-Ring
Burner Chamber
Thumbscrew (1 of 2)
Flow Spoiler
Nebulizer
Six O'clock Position
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
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.
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.
Nebulizer
Teflon Tube
Sample Capillary Tube
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).
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).
Nebulizer Clamp
Nebulizer
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.
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
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.
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
Retainer
Cap
Drain
Trap
Switch
Assembly
Drain
Spiral Wrap Loop
Drain Interlock
Connector
Interlock Cable
Drain Tubing
Drain
Vessel
Drain
Outlet
Drain Clamp
Drain
Tubing Drain
Interlock
Plug
Spiral Drain
Wrap Interlock
Connector
Drain
Interlock
Cable
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).
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
Changing a Fuse
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.
Use only fuses with the required current rating and of the specified type for
replacement.
Changing a Fuse 7-29
Lamp Maintenance
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
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
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.
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
FIAS-100/400 Maintenance
Refer to the manual received with the FIAS-100/400 for maintenance information.
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
Drain System
PE Part Number Description
0250-7987 Drain tubing
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
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.
Flame/Burner 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.
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
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
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.
Error Messages
warnings, 4-55
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
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
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
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