SQ Detector Operators Guide
SQ Detector Operators Guide
Operator’s Guide
71500126602/Revision D
Trademarks
ACQUITY UPLC, Connections Insight, ESCi, and Waters are registered
trademarks of Waters Corporation. ACQUITY, Empower, IntelliStart,
IonSABRE, MassLynx, T-Wave, UPLC, and ZSpray and “THE SCIENCE OF
WHAT’S POSSIBLE.” are trademarks of Waters Corporation.
Nalgene is a registered trademark of Nalge Nunc International.
PEEK is a trademark of Victrex Corporation.
snoop and Swagelok are registered trademarks of Swagelok Company.
TORX is a registered trademark of Textron Inc.
Viton is a registered trademark of DuPont Performance Elastomers.
Other trademarks or registered trademarks are the sole property of their
respective owners.
ii
Customer comments
Waters’ Technical Communications department invites you to tell us of any
errors you encounter in this document or to suggest ideas for otherwise
improving it. Please help us better understand what you expect from our
documentation so that we can continuously improve its accuracy and
usability.
We seriously consider every customer comment we receive. You can reach us
at [email protected].
iii
Contacting Waters
®
Contact Waters with enhancement requests or technical questions regarding
the use, transportation, removal, or disposal of any Waters product. You can
reach us via the Internet, telephone, or conventional mail.
Safety considerations
Some reagents and samples used with Waters instruments and devices can
pose chemical, biological, and radiological hazards. You must know the
potentially hazardous effects of all substances you work with. Always follow
Good Laboratory Practice, and consult your organization’s safety
representative for guidance.
When you develop methods, follow the “Protocol for the Adoption of Analytical
Methods in the Clinical Chemistry Laboratory,” American Journal of Medical
Technology, 44, 1, pages 30–37 (1978). This protocol addresses good operating
procedures and the techniques necessary to validate system and method
performance.
iv
Considerations specific to the SQ Detector
Solvent leakage hazard
The source exhaust system is designed to be robust and leak-tight. Waters
recommends you perform a hazard analysis, assuming a maximum leak into
the laboratory atmosphere of 10% LC eluate.
Warning:
• To confirm the integrity of the source exhaust system, renew
the source O-rings at intervals not exceeding one year.
• To avoid chemical degradation of the source O-rings, which
can withstand exposure only to certain solvents (see “Solvents
used to prepare mobile phases” on page C-3), determine
whether any solvents you use that are not listed are
chemically compatible with the composition of the O-rings.
Never let the nitrogen supply pressure fall below 690 kPa (6.9 bar, 100 psi)
during analyses that require flammable solvents. Connect to the LC output
with a gas-fail connector to stop the LC solvent if the nitrogen supply fails.
v
High temperature hazard
PO W ER O PER ATE
DESOLVATION NEBULIZER
HV APPI
PROBE
RP00017
vi
High voltage hazard
Warning:
• To avoid electric shock, do not remove the SQ Detector’s protective
panels. The components they cover are not user-serviceable.
• To avoid non-lethal electric shock, any equipment connected to the
ESI and IonSABRE™ APCI probes must be grounded.
• To avoid nonlethal electric shock when the instrument is in
Operate mode, avoid touching the areas marked with the high
voltage warning symbol. To touch those areas, first put the
instrument in Standby mode.
Safety advisories
Consult Appendix A for a comprehensive list of warning and caution
advisories.
vii
Operating this instrument
When operating this instrument, follow standard quality control procedures
and the guidelines presented in this section.
Applicable symbols
Symbol Definition
Authorized representative of the European
Community
Intended use
Waters designed the Single Quad (SQ) Detector for use as a research tool to
deliver authenticated mass measurement in MS mode.
viii
The Waters SQ Detector can be used for general in vitro diagnostic
applications. However, only professionally trained and qualified laboratory
personnel can use the instrument for those purposes.
The Waters SQ Detector is CE-marked according to the
European Union In Vitro Diagnostic Device Directive 98/79/EC.
Calibrating
To calibrate LC systems, follow acceptable calibration methods using at least
five standards to generate a standard curve. The concentration range for
standards must cover the entire range of quality-control samples, typical
specimens, and atypical specimens.
When calibrating mass spectrometers, consult the calibration section of the
operator’s guide for the instrument you are calibrating. In cases where an
overview and maintenance guide, not operator’s guide, accompanies the
instrument, consult the instrument’s online Help system for calibration
instructions.
Quality control
Routinely run three quality-control samples that represent subnormal,
normal, and above-normal levels of a compound. Ensure that quality-control
sample results fall within an acceptable range, and evaluate precision from
day to day and run to run. Data collected when quality control samples are out
of range might not be valid. Do not report these data until you are certain that
the instrument performs satisfactorily.
When analyzing samples from a complex matrix such as soil, tissue,
serum/plasma, whole blood, and so on, note that the matrix components can
adversely affect LC/MS results, enhancing or suppressing ionization. To
minimize these matrix effects, Waters recommends you adopt the following
measures:
• Prior to the instrumental analysis, use appropriate sample
pretreatment such as protein precipitation, liquid/liquid extraction
(LLE), or solid phase extraction (SPE) to remove matrix interferences.
• Whenever possible, verify method accuracy and precision using
matrix-matched calibrators and QC samples.
• Use one or more internal standard compounds, preferably isotopically
labeled analytes.
ix
IVD authorized representative information
Telephone: +44-161-946-2400
Fax: +44-161-946-2480
Contact: Quality manager
ISM classification
ISM Classification: ISM Group 1 Class A
This classification has been assigned in accordance with CISPR 11 Industrial
Scientific and Medical, (ISM) instruments requirements. Group 1 products
apply to intentionally generated and/or used conductively coupled
radio-frequency energy that is necessary for the internal functioning of the
equipment. Class A products are suitable for use in commercial, (that is,
nonresidential) locations and can be directly connected to a low voltage,
power-supply network.
x
Table of Contents
Copyright notice ................................................................................................... ii
Trademarks ............................................................................................................ ii
Table of Contents xi
MS operating modes ....................................................................................... 1-10
Preparing the instrument for work performed on the source ............... 4-8
Emptying the roughing pump exhaust liquid trap bottle ..................... 4-14
Cleaning the ion block, isolation valve, and extraction cone .............. 4-31
Table of Contents xv
Connecting the oil-free roughing pump ................................................... B-10
Making the electrical connections for an oil-free roughing pump............... B-17
This chapter describes the instrument, including its controls and gas
and plumbing connections.
Contents
Topic Page
Overview 1-2
Ionization techniques and source probes 1-7
Ion optics 1-9
MS operating modes 1-10
Sample inlet 1-10
Leak sensors 1-10
Vacuum system 1-10
Rear panel 1-11
IntelliStart Fluidics system 1-12
System operation 1-13
1-1
Overview
Waters SQ Detector
The Waters® SQ Detector is a single-quadrupole, atmospheric pressure
ionization (API) mass spectrometer. Designed for routine ACQUITY
®
UPLC /MS analyses, it can scan at speeds up to 10,000 Da/s.
Waters provides these ion sources with the instrument as standard
equipment:
• ZSpray™ (dual orthogonal sampling) interface.
®
• Multi-mode ESCi ionization switching for atmospheric pressure
chemical ionization (APCI) and electrospray ionization (ESI).
Optional ionization modes are IonSABRE™ APCI and APPI (atmospheric
pressure photoionization).
For instrument specifications, see the Waters SQ Detector Site Preparation
Guide.
Waters SQ Detector
TP02592
PO W ER O PER ATE
DESOLVATION NEBULIZER
HV APPI
PROBE
RP00016
IntelliStart technology
IntelliStart™ technology monitors LC/MS performance and reports when the
instrument is ready for use.
The software automatically tunes and mass calibrates the instrument and
displays performance readbacks. Integrated with Empower™
chromatography software, MassLynx™ mass spectrometry software, and
ACQUITY UPLC® Console software, it enables simplified setup of the system
for use in routine analytical and open access applications. (See “Software and
data system” on page 1-5).
The IntelliStart Fluidics system is built into the instrument. It delivers
sample directly to the MS probe from the LC column or from two integral
reservoirs. The integral reservoirs can also deliver sample through direct or
combined infusion so that you can optimize instrument performance at
analytical flow rates. See the instrument’s online Help for further details of
IntelliStart.
Overview 1-3
ACQUITY SQD UPLC/MS system
The ACQUITY SQD UPLC/MS system includes an ACQUITY UPLC system
and the Waters SQ Detector.
If you are not using your instrument as part of an ACQUITY UPLC system,
refer to the documentation for your LC system.
Solvent tray
Column heater
SQ Detector
TP02597
Binary solvent Sample manager
manager
Overview 1-5
• Processing data.
• Reviewing data.
• Printing data.
See Empower and MassLynx 4.1 user documentation and online Help for more
information on installing and using Empower or MassLynx software.
ESCi mode
RP00029 ESI probe tip
Corona pin
Isolation valve
Sample inlet
Either of two methods delivers solvent and sample to the installed probe:
• An LC system, which delivers the eluent from an LC analysis.
• IntelliStart Fluidics system, which uses onboard solutions to automate
instrument optimization. You can deliver solutions by direct or
combined infusion.
Leak sensors
Where fitted, leak sensors in the drip trays of the ACQUITY UPLC system
and the SQ Detector continuously monitor system components for leaks. A
leak sensor stops system flow when its optical sensor detects about 1.5 mL of
accumulated, leaked liquid in its surrounding reservoir. At the same time, the
ACQUITY UPLC Console displays an error message alerting you that a leak
has developed.
Tip: If you are using MassLynx software, refer to the software release notes
provided at installation to confirm whether the leak sensors are enabled.
See Waters ACQUITY UPLC Leak Sensor maintenance instructions for
complete details.
Vacuum system
An external roughing (rotary vane) pump and an internal split-flow
turbomolecular pump combine to create the source vacuum. The
turbomolecular pump evacuates the analyzer and ion transfer region.
Rear panel
The following figure shows the rear panel locations of the connectors used to
operate the instrument with external devices.
!
Event inputs
and outputs
RS 232
1 1
Analog O ut InjectS tart In
2 2
3 G round 3 G round
4 4
N otused Event In
5
6
Stop Flow O ut
5
6
Sw itch 3 O ut
ETHERNET
7 7
ACN 065444751 8 G round 8 G round
9 9
Shielded
Sw itch 2 O ut Sw itch 4 O ut
10 10
Serial Number
Source vent
VACUUM
Source
vacuum
RP00001
Overview
The IntelliStart Fluidics system is built into the instrument. The system
delivers sample directly to the MS probe in one of two ways:
• From the LC column.
• From two integral reservoirs.
Tip: The integral reservoirs can also deliver sample through direct or
combined infusion to enable optimization at analytical flow rates.
The system incorporates a multi-position valve with these attributes:
• An input connection from an external LC column.
• An input connection from the instrument’s infusion syringe. (The
infusion syringe is also connected to two reservoirs, A and B. In the
software, you specify which reservoir to draw from.)
• An output connection to the probe.
• An output connection to a waste line.
Probe
B
LC Idle Off
A
Off
Column
Syringe
Topic Page
Starting the instrument 2-2
Preparing the IntelliStart Fluidics system 2-6
Rebooting the instrument 2-11
Leaving the mass spectrometer ready for operation 2-12
2-1
Starting the instrument
The Waters SQ Detector is designed for compatibility with the ACQUITY
UPLC system. If you are not using an ACQUITY UPLC system, refer to the
documentation relevant to the system being used.
To access IntelliStart
1. In the ACQUITY UPLC Console system tree, expand SQ Detector.
2. Click IntelliStart.
Note: Under low ambient temperature, high moisture, and high flow rate
conditions, condensation can occur in the instrument’s source.
Power LED
The power LED, to the top, left-hand side of the instrument’s front panel,
indicates when the instrument is powered-on or powered-off.
Operate LED
The Operate LED, on the right-hand side of the power LED, indicates the
operating condition.
See the instrument’s online Help topic “Monitoring the detector LEDs” for
details of the Operate LED indications.
TP02685
TP02630
TP02630
Probe
B
Waste Idle Off
A
Off
Column
Syringe
Probe
B
LC Idle Off
A
Off
Column
Syringe
Infusion position
Probe
Infusion B
Infusion Off
A
On
Column
Syringe
Probe
Combined B
Idle Off
A
Off
Column
Syringe
Waste position
In the waste position, both the LC flow and the infusion syringe flow are
directed to waste. The syringe mode can be only static or dispensing (that is,
never drawing).
Probe
Waste B
Idle Off
A
Off
Column
Syringe
PO W ER O PER ATE
DESOLVATION NEBULIZER
RP00026
Topic Page
Introduction 3-2
Installing the ESI probe 3-2
Installing the corona pin 3-5
Removing the corona pin 3-7
Removing the ESI probe 3-9
3-1
Introduction
The ESI and ESCi ionization mode options use the standard ESI probe that is
fitted to the instrument when it is shipped from the factory. For ESCi
operation, the corona pin is used in conjunction with the ESI probe. The
following sections explain how to install and remove the ESI probe and corona
pin.
For further instruction, see “Electrospray ionization (ESI)” on page 1-7 and
“Combined ESI and APCI (ESCi)” on page 1-7.
1. Prepare the instrument for working on the source (see “Preparing the
instrument for work performed on the source” on page 4-8).
3. Remove the protective sleeve, if fitted, from the ESI probe tip.
Probe adjuster
assembly contacts
TP02632
POWER OPERATE
connection
HV APPI
ESI probe
electrical lead
PROBE
Probe adjuster
assembly
electrical lead
RP00017
Probe adjuster assembly ESI probe
6. Connect the ESI probe’s PTFE tube to the nebulizer gas connection.
7. Ensure that the probe adjuster assembly’s electrical lead is connected to
the instrument’s probe connection.
8. Connect the ESI probe’s electrical lead to the instrument’s HV
connection.
RP00028
5. Use the needle-nose pliers to fit the corona pin to the mounting contact.
Requirement: Ensure that the corona pin is securely mounted and that
its tip aligns with the sample cone aperture.
Corona pin
6. Use the vernier probe adjuster to position the ESI probe tip so that it is
pointing approximately midway between the tips of the sample cone and
corona pin. (See the figure page 3-4.)
7. Close the source enclosure door, and secure it with both spring-clips.
8. Close the instrument’s access door.
4. Use the needle-nose pliers to remove the corona pin from its mounting
contact. Store the corona pin in a safe location. (See the figure “Source,
showing the corona pin, ESi probe tip, and sample cone” on page 3-7.)
1. Prepare the instrument for working on the source (see “Preparing the
instrument for work performed on the source” on page 4-8).
Warning: The ESI probe and source can be hot. To avoid burn
injuries, take great care while working with the instrument’s
access door open.
8. Carefully remove the ESI probe from the probe adjuster assembly.
9. If available, fit the protective sleeve to the ESI probe tip.
10. Close the instrument’s access door.
Topic Page
Maintenance schedule 4-3
Spare parts 4-5
Troubleshooting with Connections Insight 4-5
Safety and handling 4-7
Preparing the instrument for work performed on the source 4-8
Operating the source isolation valve 4-9
Removing O-rings and seals 4-11
Cleaning the instrument’s exterior 4-12
Emptying the exhaust trap bottle 4-12
Emptying the roughing pump exhaust liquid trap bottle 4-14
Gas ballasting the roughing pump 4-16
Checking the roughing pump oil level 4-19
Adding oil to the roughing pump 4-19
Cleaning the source components 4-21
Cleaning the sample cone and gas cone 4-21
Cleaning the ion block, isolation valve, and extraction cone 4-31
Cleaning the source hexapole assembly 4-47
Replacing the ESI probe tip 4-54
Replacing the ESI probe sample capillary 4-55
Cleaning the IonSABRE APCI probe tip 4-62
Replacing the IonSABRE APCI probe sample capillary 4-62
4-1
Contents
Topic Page
Cleaning or replacing the corona pin 4-70
Replacing the APCI probe heater 4-71
Replacing the ion block source heater 4-75
Replacing the source assembly seals 4-79
Maintaining the instrument air filters 4-90
Replacing the roughing pump oil 4-95
Replacing the roughing pump’s oil demister element 4-98
Maintenance schedule
Warning: The probe and source can be hot. To avoid burn injuries, take
great care while working with these components.
1. In the Instrument Console, click Stop Flow to stop the LC flow or, if
column flow is required, divert the LC flow to waste as follows:
a. In the Instrument Console system tree, expand SQ Detector,
Interactive Fluidics.
b. Click Control .
c. Select Waste as the flow state.
2. In the Instrument Console, click Standby , and confirm that the
Operate indicator is not illuminated.
3. Wait 3 minutes to allow the desolvation gas flow to cool the probe and
source.
4. In the Instrument Console, click API to stop the desolvation gas
flow.
1. Prepare the instrument for working on the source (see “Preparing the
instrument for work performed on the source” on page 4-8).
Caution: Do not apply any downward force to the source enclosure door
while the door is open.
1. Open the source isolation valve by moving its handle clockwise to the
horizontal position.
2. Close the source enclosure door, and secure it with both spring-clips.
3. Close the instrument’s access door.
Tool 1
Tool 2
To remove an O-ring
Use a soft cloth, dampened with water, to clean the outside surfaces of the
instrument.
To laboratory
exhaust port
From instrument (10-mm OD)
exhaust connection
(12-mm OD)
Required materials:
• Chemical-resistant, powder-free gloves
®
• snoop (or equivalent) leak detector liquid
9. Use snoop (or equivalent) leak detector liquid to ensure that there are no
leaks at the exhaust trap bottle cap.
Roughing pump exhaust liquid trap bottle for an oil-filled roughing pump
TP02800
Roughing pump exhaust liquid trap bottle for an oil-free roughing pump
TP02997
TP02800
TP02996
2. Unscrew and remove the roughing pump liquid trap bottle cap.
7. Use snoop (or equivalent) leak detector liquid to ensure that there are no
leaks at the liquid trap bottle cap.
Roughing pump
The roughing pump draws large quantities of solvent vapors. The vapors tend
to condense in the pump oil, diminishing pumping efficiency. Gas ballasting
purges condensed contaminants from the oil.
Gas ballast the roughing pump when these conditions apply:
• With ESI operation, once a week.
• With frequent APCI operation, once a day.
• When the roughing pump oil appears cloudy.
• When the vacuum pressure is higher than normal.
• When condensate forms in the roughing pump exhaust line.
• When you change the roughing pump oil.
Warning: To avoid burn injuries, take great care while working with
the roughing pump: it can be hot.
1. Use the flat-blade screwdriver to turn the gas ballast valve on the pump
a quarter-turn to the open, , position.
TP02654
, position.
Warning: To avoid burn injuries, take great care while working with
the roughing pump: it can be hot.
1. Move the gas ballast valve handle on the pump a counterclockwise from
the horizontal position to the vertical position.
TP02654
Note: This procedure is not required for an Alcatel oil-free roughing pump.
Requirement: You must check the oil level while the roughing pump is
running.
The roughing pump oil level appears in the roughing pump’s oil level sight
glass. Check the oil level at weekly intervals; you must maintain the oil level
so that it is at or near the MAX level when the pump is not operating.
Tip: The oil level in the sight glass is lower when the roughing pump is
running than when it is stopped. When the pump is running, the oil level is
typically at 30% to 60% of the MAX level. For further information, see the
figure “Roughing pump” on page 4-16 and “Adding oil to the roughing pump”
on page 4-19.
2. Use the 8-mm Allen wrench to unscrew and remove the roughing pump’s
oil filler plug (see the figure “Roughing pump” on page 4-16).
3. Using the funnel, add Anderol vacuum oil, type GS 495, into the oil filler
aperture until the oil reaches the oil level sight glass MAX level.
4. Ensure that the O-ring on the oil filler plug is clean and properly seated.
Caution: To avoid oil leakage, when fitting the oil filler plug to
the roughing pump,
• ensure that the plug is not cross-threaded.
• ensure that the O-ring is not pinched.
• do not over-tighten the plug.
5. Use the 8-mm Allen wrench to fit and tighten the roughing pump’s oil
filler plug.
Tip: When the oil filler plug is tightened, the plug seals with an O-ring.
Compression is controlled by the O-ring groove depth in the plug.
Increased torque does not improve the plug seal; it only makes the plug
difficult to remove later.
6. Start the instrument (see “Starting the instrument” on page 2-2).
Tips: After you add oil to the pump, the following situations can occur:
• The oil level drops slightly during the first month of operation.
• The oil changes color (darkens) over time.
Warning: The source can be hot. To avoid burn injuries, take great care
while working with the instrument’s access door open.
Caution: Do not apply any downward force to the source enclosure door
while the door is open.
1. Close the source isolation valve (see “Operating the source isolation
valve” on page 4-9).
2. Disconnect the PTFE tube from the cone gas assembly connection tube.
Connection tube
PTFE tube
RP00006
Caution: Do not open the isolation valve at any time when the
cone gas assembly has been removed from the ion block
assembly.
4. Slide the cone gas assembly out of the ion block assembly.
1. Position the cone gas assembly inlet over the extraction tool on the
source enclosure door.
Alternative: Use the hand-held extraction tool supplied with the
instrument. This tool is used in a similar manner to that fitted to the
source enclosure door.
Extraction tool
Source enclosure
door
RP00020
2. Carefully push down on the gas cone to separate the gas cone, sample
cone, and O-ring.
O-ring
Sample cone
Gas cone
RP00021
Warning: Use extreme care when working with formic acid. Work in a
fume hood, and use suitable protective equipment.
Caution: The sample cone is fragile. Never place it on its tip; always
place it on its flanged base.
1. If the sample cone contains debris, place a drop of formic acid on its
orifice.
2. Immerse the sample cone and gas cone separately in glass vessels
containing 1:1 methanol/water.
Tip: If the components are obviously contaminated, use 45:45:10
methanol/water/formic acid.
3. Place the vessels in the ultrasonic bath for 30 minutes.
4. If you used formic acid in the cleaning solution, do as follows:
a. Rinse the components by immersing them separately in glass
vessels containing water and then placing the vessels in the
ultrasonic bath for 20 minutes.
b. Displace the water by immersing the components in separate glass
vessels containing methanol and then placing the vessels in the
ultrasonic bath for 10 minutes.
5. Carefully remove the components from the vessels, and blow-dry them
with inert, oil-free gas.
6. Inspect each component for persisting contamination. If contamination
is present, do as follows:
a. Use the wash-bottle containing 1:1 methanol/water to rinse the
component over the large beaker.
b. Blow-dry the component with inert, oil-free gas.
7. Inspect each component for persisting contamination. If contamination
is present, dispose of the component, and obtain a new one before
reassembling the cone gas assembly.
Caution:
• To avoid recontaminating the cone gas assembly, wear clean
chemical-resistant, powder-free gloves during this procedure.
• The sample cone is fragile. Never place it on its tip; always place it
on its flanged base.
O-ring
Sample cone
Gas cone
TP02663
2. Fit a new O-ring into the groove created between the sample cone and
gas cone.
Ion block
assembly
Cone gas
assembly
RP00009
3. Grasp the cone gas assembly connection tube and use it as a handle to
rotate the cone gas assembly 90 degrees, moving the connection tube
from the horizontal to the vertical position.
4. Connect the PTFE tube to the cone gas assembly connection tube.
5. Open the source isolation valve.
6. Close the source enclosure door, and secure it with both spring-clips.
7. Close the instrument’s access door.
1. Vent and shut-down the instrument (see the mass spectrometer’s online
Help for details).
Cleaning the ion block, isolation valve, and extraction cone 4-31
4. Close the source isolation valve (see “Operating the source isolation
valve” on page 4-9).
5. Disconnect the PTFE tube from the cone gas assembly connection tube.
6. Use the 6-mm Allen wrench to unscrew and remove the 2 ion block
assembly securing screws and associated washers.
Washers
RP000010
7. Remove the ion block assembly from the PEEK ion block support.
RP00011
TP02650
2. Grasp the cone gas assembly connection tube and use it as a lever to
rotate the cone gas assembly 90 degrees.
Cleaning the ion block, isolation valve, and extraction cone 4-33
Caution: To ensure correct operation of the ion block assembly after
reassembly,
• the gas cone position block must not be removed
• the screws holding the gas cone position blocks in place must not be
adjusted.
3. Slide the cone gas assembly out of the ion block assembly.
4. Use the 2.5-mm Allen wrench to loosen the 4 ion block cover plate
captive securing screws.
TP02649
Isolation valve
O-ring
7. Use the O-ring removal kit to carefully remove the isolation valve O-ring
(see “Removing O-rings and seals” on page 4-11).
Cleaning the ion block, isolation valve, and extraction cone 4-35
9. Use the 2.5-mm Allen wrench to loosen the captive PEEK terminal block
securing screw.
PEEK terminal block securing screw
TP02616
10. Use the needle-nose pliers to grasp the PEEK terminal block and
partially lift it out of the ion block.
TP02618
12. Use the O-ring removal kit to carefully remove the cover seal from the
ion block (see also “Removing O-rings and seals” on page 4-11).
Cover seal
TP02619
Cleaning the ion block, isolation valve, and extraction cone 4-37
Warning: The cover seal can be contaminated with
biohazardous and/or toxic materials. Ensure that it is
correctly disposed of according to local environmental
regulations.
Seal
TP02648
15. Dispose of the blanking plug seal in accordance with local environmental
regulations.
Securing
screw
Extraction
cone
TP02612
Caution:
• Take great care not to damage the extraction cone aperture
when removing the extraction cone from the ion block.
• The extraction cone is fragile. Never place it on its tip; always
place it on its flanged base.
17. Remove the extraction cone retainer and extraction cone from the ion
block.
Extraction cone retainer Extraction cone aperture
TP02613
Cleaning the ion block, isolation valve, and extraction cone 4-39
18. Remove the extraction cone retainer from the extraction cone.
19. Remove the extraction cone seal from the ion block.
TP02614
Warning: Use extreme care when working with formic acid. Use a
fume hood and appropriate protective equipment.
Caution: The extraction cone is fragile. Never place it on its tip; always
place it on its flanged base.
1. Immerse the ion block, isolation valve, and extraction cone separately in
glass vessels containing 1:1 methanol/water.
4. Carefully remove the components from the vessels, and blow-dry them
using inert, oil-free gas.
Cleaning the ion block, isolation valve, and extraction cone 4-41
5. Inspect each component for persisting contamination. If contamination
is present, do as follows:
a. Use the wash-bottle containing 1:1 methanol/water to rinse the
component over the large beaker.
b. Blow-dry the component with inert, oil-free gas.
6. Inspect each component for persisting contamination. If contamination
is present, dispose of the component, and obtain a new one before
reassembling the ion block assembly.
Caution:
• To avoid recontaminating the ion block assembly, wear clean
chemical-resistant, powder-free gloves during this procedure.
• The sample cone is fragile. Never place it on its tip; always place it
on its flanged base.
3. Fit the extraction cone retainer and extraction cone to the ion block.
4. Use the 2.5-mm Allen wrench to tighten the captive screw securing the
extraction cone retainer.
5. Fit a new blanking plug seal to the ion block blanking plug.
Cleaning the ion block, isolation valve, and extraction cone 4-43
14. If an ion block assembly set screw is fitted, use the 1.5 mm Allen wrench
to loosen the set screw. If an ion block assembly set screw is not fitted go
to step 18.
TP02651
15. To tighten the ion block assembly set screw, hold the ion block in
position against the PEEK ion block support on the instrument.
16. Carefully tighten the set screw until it makes contact with the
thermocouple.
17. Remove the ion block from the PEEK ion block support on the
instrument.
18. Fit the ion block cover plate to the ion block assembly, and then use the
2.5-mm Allen wrench to tighten the 4 ion block cover plate captive
securing screws.
19. Holding the cone gas assembly so that the connection tube is horizontal
and at the top, slide the cone gas assembly into the ion block assembly.
20. Grasp the cone gas assembly connection tube, and use it as a handle to
rotate the cone gas assembly 90 degrees, moving the connection tube
from the horizontal to the vertical position.
1. Unscrew and remove the 3 thumbscrews that secure the right-hand side
flange to the source enclosure.
Thumbscrew
Spring-clip
RP00024
Cleaning the ion block, isolation valve, and extraction cone 4-45
Caution: Do not apply any downward force to the source
enclosure door while the door is open.
4. Fit the ion block assembly to the PEEK ion block support.
5. Use the 6-mm Allen wrench to fit and then slowly and evenly tighten the
2 ion block assembly securing screws and their associated washers.
6. Look through the hole in the side of the source enclosure and view the
area where the ion block assembly meets the PEEK ion block support. If
you see a gap, the extraction cone has slipped out of position during
installation. If this is the case, remove the ion block assembly, refit the
extraction cone, and reinstall the ion block assembly on the PEEK ion
block support.
7. When you are satisfied with the installation of the ion block assembly,
fit the side flange to the source enclosure.
8. Fit and tighten the 3 thumbscrews that secure the right-hand side
flange to the source enclosure.
9. Connect the PTFE tube to the cone gas assembly connection tube.
10. Open the source isolation valve (see “Operating the source isolation
valve” on page 4-9).
11. Close the source enclosure door, and secure it with both spring-clips.
To remove the ion block assembly, ion block support, and hexapole
1. Remove the ion block assembly from the PEEK ion block support (see
“Removing the ion block assembly from the source assembly” on
page 4-31).
2. Use the 3-mm Allen wrench to unscrew and remove the 3 screws
securing the PEEK ion block support to the adaptor housing.
Adaptor housing
6. Carefully grasp the source hexapole assembly and remove it from the
adaptor housing.
3. Use the hook to carefully suspend the hexapole assembly into the glass
vessel with the bottom of the assembly clear of the bottom of the vessel.
Hook
TP02658
4. Add 1:1 methanol/water to the glass vessel until the hexapole assembly
is immersed completely.
5. Place the vessel in the ultrasonic bath for 30 minutes.
6. Carefully remove the hexapole assembly from the vessel, and blow-dry it
using inert, oil-free gas.
To fit the hexapole assembly and PEEK ion block support to the source
Caution: To avoid damage, when fitting the hexapole assembly into the
adaptor housing, observe these precautions:
• Avoid scratching the internal surfaces of the adaptor block.
• Do not compress the hexapole rods.
1. Carefully fit the source hexapole assembly into the adaptor housing,
aligning the notches in the differential aperture at its rear with the two
bottom support rails on the analyzer assembly. Then carefully slide the
assembly fully into place.
2. Ensure that the grooves for the PEEK ion block support O-rings are free
from dirt and debris.
Tip: If contamination is present, use 1:1 methanol/water, applied to a
lint-free cloth, to carefully clean the grooves.
3. Fit new O-rings to the PEEK ion block support.
Tip: To fit an O-ring in its groove, start fitting the O-ring at the notch in
the groove and then progressively work the ring into the groove in either
direction from the notch.
4. Fit the PEEK ion block support to the instrument’s housing.
Hexapole spring
Hexapole rod
TP02659
6. Fit the ion block assembly to the PEEK ion block support (see “Fitting
the ion block assembly to the source assembly” on page 4-45).
Warning: The probe and source can be hot. To avoid burn injuries, take
great care while performing this procedure.
1. Remove the probe from the source (see also “Removing the ESI probe” on
page 3-9).
2. Use the 6-mm (¼-inch) wrench to unscrew and remove the probe tip.
Warning: The probe and source can be hot. To avoid burn injuries, take
great care while performing this procedure.
1. Remove the probe from the source (see “Installing the corona pin” on
page 3-5).
2. Use the screwdriver to remove the 2 probe end-cover retaining screws.
Retaining screws
TP03004
Setscrew
TP03005
End-cover
TP03006
Probe tip
TP03007
Coupling
LC union
TP03009
Seal
TP03011
GVF16 Ferrule Capillary Coupling
Conductive sleeve
TP03012
11. Slide a new GVF16 ferrule onto the PTFE liner tube.
12. Fit a new seal into the groove facing the short end of the coupling.
Seal
Coupling
TP03013
13. Slide the coupling—short end first—onto the capillary, followed by the
new PTFE liner tube and ferrule and screw the coupling into the LC
union.
TP03014
Compression Coupling
screw
TP03015
Conductive sleeve
Coupling
LC union
TP03009
25. Replace the probe tip, and then screw down until the capillary protrudes
approximately 0.5 mm from the end of the tip.
Capillary protrudes 0.5 mm
from the end of the probe tip
5. Click Operate .
6. Wait 10 minutes.
Rationale: The high APCI probe heater temperature removes any
chemical contamination from the probe tip.
Warning: The probe and source can be hot. To avoid burn injuries, take
great care while performing this procedure.
1. Remove the probe from the source (see “Removing the IonSABRE APCI
probe” on page 5-6).
2. Use the 2.5-mm Allen wrench to remove the 2 probe end-cover retaining
screws.
End-cover retaining screws
TP02676
TP02677
Capillary
TP02674
Nebulizer adjuster knob
TP02675
7. Use the 7-mm wrench to loosen the locknut securing the PEEK union
and UNF coupling.
PEEK union 7-mm wrench
TP02672
TP02679
TP02667
TP02671
PEEK tubing
TP02668
Caution:
• When handling the probe heater, take great care to grip the
heater so as not to damage its electrical wiring.
• Take great care not to damage the probe heater’s electrical
connections, capillary sleeve, or capillary when fitting the
heater over the capillary sleeve.
19. Fit the probe heater (see “Replacing the APCI probe heater” on
page 4-71, step 5 through step 8).
20. Fit the probe to the instrument (see “Installing the IonSABRE APCI
probe” on page 5-3).
21. In the ACQUITY UPLC Console, click API to start the desolvation
gas flow.
22. Use the probe adjuster knob to adjust the capillary so that the capillary
protrudes approximately 0.5 mm from the end of the probe.
Warning: The probe and source can be hot. To avoid burn injuries, take
great care while performing this procedure.
Caution: Do not apply any downward force to the source enclosure door
while the door is open.
1. Remove the corona pin from the source (see “Removing the corona pin”
on page 3-7).
2. Replace the pin if it is deformed or otherwise damaged.
Requirement: Otherwise clean the tip of the pin with the lapping film,
and then wipe it clean with a methanol-saturated tissue.
3. Install the corona pin in the source (see “Installing the corona pin” on
page 3-5).
1. Remove the probe from the source (see “Removing the IonSABRE APCI
probe” on page 5-6).
2. Use the jeweler’s screwdriver to loosen the 2 set screws securing the
probe heater cover to the probe.
3. Carefully pull the probe heater cover off the probe, revealing the probe
heater.
Probe heater electrical wiring
TP02680
Caution:
• When handling the probe heater, take great care to grip the
heater so as not to damage its electrical wiring.
• To avoid damaging the probe heater’s electrical connections,
do not twist the heater when removing it from the probe
assembly.
4. Gripping the probe heater as shown, carefully pull it off the probe
assembly.
Probe heater
TP02678
5. Carefully slide the probe heater over the capillary sleeve on the probe
assembly.
Probe heater connections
TP02670
Capillary Capillary sleeve
6. Fit the probe heater to the probe assembly, ensuring that the heater is
fully seated on the probe assembly.
TP02669
1. Remove the ion block assembly from the instrument (see “Removing the
ion block assembly from the source assembly” on page 4-31).
2. Ensure that the isolation valve is closed.
TP02650
TP02649
TP02616
TP02617
7. Use the needle-nose pliers to gently grasp the heat-shrink tubing on the
heater cartridge assembly and slide the assembly out of the ion block.
Heat-shrink tubing
TP02618
9. Use the needle-nose pliers to gently grasp the heat-shrink tubing on the
new heater cartridge assembly and slide the assembly into the ion
block..
10. Use the needle-nose pliers to position the 2 heater wire ring tags fully
down on the PEEK block terminals.
11. Use the 1.5-mm Allen wrench to fit and tighten the 2 screws securing
the heater wires to the PEEK terminal block.
12. Fit the ion block cover plate to the ion block assembly, and then use the
2.5-mm Allen wrench to tighten the 4 captive screws securing ion block
cover plate.
13. Fit the ion block assembly to the instrument (see “Fitting the ion block
assembly to the source assembly” on page 4-45).
1. Vent and shut-down the instrument (see the mass spectrometer’s online
Help for details).
Source enclosure
Source enclosure securing screw
securing screws
RP00027
RP000 27
Caution: Do not apply any downward force to the source
enclosure door when removing the source enclosure from the
instrument’s housing.
1. Use the 4-mm Allen wrench to remove the 4 screws securing the probe
adjuster assembly to the source enclosure.
Probe adjuster
assembly
Probe adjuster assembly
securing screw
Thumbscrew
Source enclosure
side flange
RP00024
To remove the seals from the source enclosure and probe adjuster
assembly
1. Use the O-ring removal kit to carefully remove the probe adjuster
assembly probe seal from the probe adjuster assembly (see “Removing
O-rings and seals” on page 4-11).
Probe adjuster assembly probe seal
TP02632
Probe adjuster
assembly flange seal
Source enclosure
housing seal
Source side
flange seal
RP00025
Source enclosure
door seal
RP00019
Caution: Do not apply any downward force to the source enclosure door
while the door is open.
1. Ensure that all the grooves for seals are free from dirt and debris.
Tip: If contamination is present, use 1:1 methanol/water, applied to a
lint-free cloth, to carefully clean the grooves.
2. Fit the new door glass seal to the source enclosure door.
3. Fit the glass to the source enclosure door.
4. Fit the glass retaining plate to the source enclosure door.
5. Fit and tighten the 4 screws securing the glass retaining clips to the
source enclosure door.
Caution: Ensure that the tails of the source enclosure door seals
are correctly located in the groove when fitting them to the
source enclosure door.
6. Fit the new source enclosure door seal to the source enclosure door.
7. Close the source enclosure door, and secure it with both spring-clips.
2. Fit and tighten the 3 thumbscrews that secure the source enclosure side
flange to the source enclosure.
3. Fit the probe adjuster assembly to the source enclosure.
4. Use the 4-mm Allen wrench to fit and tighten the 4 screws securing the
probe adjuster assembly to the source enclosure.
Caution:
• To avoid recontaminating the source, wear clean,
chemical-resistant, powder-free gloves during this procedure.
• Do not apply any downward force to the source enclosure door when
fitting the source enclosure to the instrument’s housing.
2. Use the 5-mm Allen wrench to tighten the 3 captive screws securing the
source enclosure.
3. Connect the 2-pin connector at the rear of the source enclosure.
4. Connect the PTFE tubing to the desolvation gas connection at the
instrument’s front panel
5. Connect the probe’s electrical connection at the instrument’s front panel.
6. If using ESCi mode or an IonSABRE APCI probe, carefully fit the corona
pin (see “Installing the corona pin” on page 3-5).
7. Close the source enclosure door, and secure it with both spring-clips.
TP02636
Screws
2. Use a vacuum cleaner to clean the air filter located inside the
instrument’s lower bezel.
Air filter
Frame
TP02638
Screws
Air filter
Frame
TP02638
Screws
3. Remove the air filter from the air filter frame and dispose of it.
4. Align the new air filter within the air filter frame.
5. Use the T10 TORX driver to fit and tighten the 4 screws securing the air
filter and frame to the inside of the lower bezel.
6. Reinstall the lower bezel.
RP00023
Air filter
Frame
TP02637
Frame
Air filter
TP02640
4. Place the container for used oil under the pump’s drain plug.
6. Use the 8-mm Allen wrench to remove the oil drain plug.
7. Tip the pump toward the drain plug aperture and allow the oil to drain
completely into the container.
11. Using the funnel, pour all the oil from the 1-L container into the oil filler
aperture.
12. Wait a few minutes, and then recheck the oil level.
13. Ensure that the O-ring on the oil filler plug is clean and properly seated.
14. Use the 8-mm Allen wrench to refit the oil filler plug.
15. Start the instrument (see “Starting the instrument” on page 2-2).
16. Gas-ballast the roughing pump (see “Gas ballasting the roughing pump”
on page 4-16).
Tips: After you add oil to the pump, the following situations can occur:
• The oil level drops slightly during the first month of operation.
• The oil changes color (darkens) over time.
• After running the pump for 12 to 48 hours, it is common to see a few
drops of oil near the filler plug. Excess oil around the lip of the filler
plug will run down and drip off the pump once the pump reaches
operating temperature.
• When the pump begins to run at normal operating temperature,
spilled oil smells slightly.
3. Use the 6-mm Allen wrench to remove the 4 bolts securing the exhaust
flange to the roughing pump.
Securing bolt
Exhaust flange
TP02694
TP02693
5. Use the 10-mm wrench to remove the nut that secures the oil demister
element to the exhaust flange.
Spring
Securing nut
TP02686
TP02692
TP02682
2. Holding the oil demister element slightly elevated to prevent the loss of
the spring, fit the exhaust flange to the oil demister element.
Caution: The nut that secures the oil demister element to the
exhaust flange must not be overtightened; ensure that only
approximately 1 mm of thread is exposed beyond the nut when it
is tightened.
3. Use the 10-mm wrench to fit and tighten the nut that secures the oil
demister element to the exhaust flange.
1 mm exposed thread
after tightening
TP02686
5. Use the 6-mm Allen wrench to fit the 4 bolts securing the exhaust flange
to the roughing pump.
6. Start the instrument (see “Starting the instrument” on page 2-2).
Topic Page
Atmospheric pressure chemical ionization 5-2
IonSABRE APCI probe 5-2
Installing the IonSABRE APCI probe 5-3
Installing the corona pin 5-5
Removing the corona pin 5-5
Removing the IonSABRE APCI probe 5-6
5-1
Atmospheric pressure chemical ionization
APCI, an option for the instrument, produces singly charged protonated or
deprotonated molecules for a broad range of nonvolatile analytes.
The APCI interface consists of the standard source fitted with a corona pin
and a heated IonSABRE APCI probe. Mobile phase from the ACQUITY UPLC
column enters the probe, where it is pneumatically converted to an aerosol,
rapidly heated, and vaporized or gasified at the probe tip.
APCI mode
Sample cone
Corona pin
Hot gas from the IonSABRE APCI probe passes between the sample cone and
the corona pin, which is typically operated with a discharge current of 5 µA.
Mobile phase molecules rapidly react with ions generated by the corona
discharge to produce stable reagent ions. Analyte molecules introduced into
the mobile phase react with the reagent ions at atmospheric pressure and
typically become protonated (in the positive ion mode) or deprotonated (in the
negative ion mode). The sample and reagent ions then pass through the
sample cone and into the mass spectrometer.
1. Prepare the instrument for working on the source (see “Preparing the
instrument for work performed on the source” on page 4-8).
Probe adjuster
assembly contacts
TP02632
Desolvation gas
connection
PO W ER O PER ATE
DESOLVATION NEBULIZER
HV
APCI probe APPI
electrical lead
PROBE
Probe adjuster
assembly electrical
lead (not connected
when using the
IonSABRE APCI
probe) RP00022
5. Connect the IonSABRE APCI probe’s PTFE tube to the nebulizer gas
connection.
6. At the instrument’s front panel, disconnect the probe adjuster
assembly’s electrical lead from the probe connection.
7. Connect the IonSABRE APCI probe’s electrical lead to the instrument’s
probe connection.
1. Prepare the instrument for working on the source (see “Preparing the
instrument for work performed on the source” on page 4-8).
Contents
Topic Page
Warning symbols A-2
Caution symbol A-5
Warnings that apply to all Waters instruments A-5
Electrical and handling symbols A-11
A-1
Warning symbols
Warning symbols alert you to the risk of death, injury, or seriously adverse
physiological reactions associated with an instrument’s use or misuse. Heed
all warnings when you install, repair, and operate Waters instruments.
Waters assumes no liability for the failure of those who install, repair, or
operate its instruments to comply with any safety precaution.
Specific warnings
The following warnings can appear in the user manuals of particular
instruments and on labels affixed to them or their component parts.
Burst warning
This warning applies to Waters instruments fitted with nonmetallic tubing.
This warning applies to certain instruments when they are in Operate mode.
Biohazard warning
This warning applies to Waters instruments that can be used to process
material that might contain biohazards: substances that contain biological
agents capable of producing harmful effects in humans.
Caution symbol
The caution symbol signifies that an instrument’s use or misuse can damage
the instrument or compromise a sample’s integrity. The following symbol and
its associated statement are typical of the kind that alert you to the risk of
damaging the instrument or sample.
Important: Toute modification sur cette unité n’ayant pas été expressément
approuvée par l’autorité responsable de la conformité à la réglementation peut
annuler le droit de l’utilisateur à exploiter l’équipement.
注意:未經有關法規認證部門允許對本設備進行的改變或修改,可能會使使用者喪失操作該設
備的權利。
注意:未经有关法规认证部门明确允许对本设备进行的改变或改装,可能会使使用者丧失操
作该设备的合法性。
注意:規制機関から明確な承認を受けずに本装置の変更や改造を行うと、本装置のユー
ザーとしての承認が無効になる可能性があります。
警告:當在有壓力的情況下使用聚合物管線時,小心注意以下幾點。
• 當接近有壓力的聚合物管線時一定要戴防護眼鏡。
• 熄滅附近所有的火焰。
• 不要使用已經被壓癟或嚴重彎曲管線。
• 不要在非金屬管線中使用四氫呋喃或濃硝酸或濃硫酸。
• 要了解使用二氯甲烷及二甲基亞楓會導致非金屬管線膨脹,大大降低管線的耐壓能力。
警告:圧力のかかったポリマーチューブを扱うときは、注意してください。
• 加圧されたポリマーチューブの付近では、必ず保護メガネを着用してください。
• 近くにある火を消してください。
• 著しく変形した、または折れ曲がったチューブは使用しないでください。
• 非金属チューブには、テトラヒドロフラン(THF)や高濃度の硝酸または硫酸などを流
さないでください。
• 塩化メチレンやジメチルスルホキシドは、非金属チューブの膨張を引き起こす場合が
あり、その場合、チューブは極めて低い圧力で破裂します。
Attention: L’utilisateur doit être informé que si le matériel est utilisé d’une
façon non spécifiée par le fabricant, la protection assurée par le matériel risque
d’être défectueuses.
警告:使用者必須非常清楚如果設備不是按照製造廠商指定的方式使用,那麼該設備所提供
的保護將被消弱。
警告:使用者必须非常清楚如果设备不是按照制造厂商指定的方式使用,那么该设备所提供
的保护将被削弱。
警告: ユーザーは、製造元により指定されていない方法で機器を使用すると、機器が提供
している保証が無効になる可能性があることに注意して下さい。
Electrical symbols
These can appear in instrument user manuals and on the instrument’s front
or rear panels.
Electrical power on
Standby
Direct current
Alternating current
Fuse
Keep upright!
Keep dry!
Fragile!
Use no hooks!
Caution:
• Contact Waters Technical Service before moving the
instrument.
• If you must transport the instrument, or remove it from
service, contact Waters Technical Service for recommended
cleaning, flushing, and packaging procedures.
See “Troubleshooting with Connections Insight” on page 4-5.
Contents
Topic Page
External wiring and vacuum connections B-2
Connecting the oil-filled roughing pump B-3
Connecting the oil-free roughing pump B-10
Connecting to the nitrogen gas supply B-18
Connecting the nitrogen exhaust line B-20
Connecting the liquid waste line B-23
Connecting the workstation B-25
Connecting Ethernet cables B-26
I/O signal connectors B-26
Connecting to the electricity source B-31
B-1
External wiring and vacuum connections
Rear panel connections appear in the figure below.
Rear panel
!
Event inputs
and outputs
RS 232
1 1
Analog O ut InjectS tart In
2 2
3 G round 3 G round
4 4
N otused Event In
5
6
Stop Flow O ut
5
6
Sw itch 3 O ut
ETHERNET
7 7
ACN 065444751 8 G round 8 G round
9 9
Shielded
Sw itch 2 O ut Sw itch 4 O ut
10 10
Serial Number
Source vent
VACUUM
Source
vacuum
RP00001
Required materials:
• Chemical-resistant, powder-free gloves
• 7-mm nut driver
• 8-mm Allen wrench
• Sharp knife
• 1-L exhaust trap bottle (included in the startup kit)
• Elbows (included in the Waters Rough Pump Connect Kit)
• NW25 tee (included in the startup kit)
• NW25 center rings (included in the startup kit)
• NW25 clamps (included in the startup kit)
• PVC exhaust tubing (included in the Waters Rough Pump Connect Kit)
• PVC hose clamps (included in the Waters Rough Pump Connect Kit)
• 1-inch ID vacuum hose (included in the Waters Rough Pump Connect
Kit)
Caution:
• To ensure correct operation of the roughing pump, the pump
must be installed within 1 degree of horizontal.
• The area where the roughing pump is located must have an
ambient temperature of 15 to 40 ºC (59 to 104 ºF).
• To ensure proper ventilation, the pump must be installed with
the following minimum clearances:
TP02689
1-inch ID
vacuum hose
Clamps
Flange
NW25 tee
Pump inlet
TP02625
4. Attach the flanged end of a length of 1-inch ID vacuum hose to each open
port on the NW25 tee. Use the NW25 center rings and clamps provided
in the startup kit. Use the 7-mm nut driver to install the clamps.
5. Connect the opposite ends of the two lengths of vacuum hose in step 4 to
the two, 1-inch OD, straight, vacuum ports on the instrument’s rear
panel. Secure the hose ends with clamps supplied in the startup kit;
install 2 clamps on each hose end.
7. Connect an elbow to the other end of the PVC exhaust tubing, and
connect the elbow to one of the fittings on the exhaust trap bottle
(included in the startup kit).
Exhaust port
Elbow
TP02800
10. Route the open end of the exhaust tubing to a suitable exhaust vent.
11. Check the oil level in the pump.
See “Checking the roughing pump oil level” on page 4-19, and, if needed,
“Adding oil to the roughing pump” on page 4-19.
12. Make the electrical connections to the roughing pump.
• If your roughing pump has an external relay box, see “Making the
electrical connections for a roughing pump with an external relay
box” on page B-8.
• If your roughing pump does not have an external relay box, see
“Making the electrical connections for a roughing pump without an
external relay box” on page B-9.
RS 232
G round
O ut
1
2
3
InjectS tart
G round
In
4 4
power connector
N otused Event In
5
6
Stop Flow O ut
5
6
Sw itch 3 O ut
ETHERNET
7 7
ACN 065444751 8 G round 8 G round
9 9
Sw itch 2 O ut Sw itch 4 O ut
10 10
Serial Number
!
IVD
V ~ 200 - 240
Hz 50 - 60
VA 900
PUMP
API Gas
6.9 Bar Maximum
VACUUM
SOURCE VENT
VACUUM
01757 U.S.A.
Relay box
RP00013
To power source
RS 232
G round
O ut
1
2
3
InjectS tart
G round
In
power connector
4 4
N otused Event In
5
6
Stop Flow O ut
5
6
Sw itch 3 O ut
ETHERNET
7 7
ACN 065444751 8 G round 8 G round
9 9
Sw itch 2 O ut Sw itch 4 O ut
10 10
Serial Number
!
IVD
V ~ 200 - 240
Hz 50 - 60
VA 900
PUMP
API Gas
6.9 Bar Maximum
VACUUM
SOURCE VENT
VACUUM
01757 U.S.A.
RP00015
To power
source
Exhaust port
Noise reduction
flange
cover
Inlet flange
TP02995
Required materials:
• Chemical-resistant, powder-free gloves
• 7-mm nut driver
• 8-mm Allen wrench
DN 25 nipple
DN 40 nipple
Clamps
TP02996
Caution:
• To ensure correct operation of the roughing pump, the pump
must be installed within 1 degree of horizontal.
• The area where the roughing pump is located must have an
ambient temperature of 15 to 40 ºC (59 to 104 ºF).
• To ensure proper ventilation, the pump must be installed with
the following minimum clearances:
TP02995
NW25 tee
Elbow
1-inch ID
vacuum hose
Isolation valve
DN40 nipple
on pump inlet
TP02997
3. Attach the flanged end of a length of 1-inch ID vacuum hose to each open
port on the NW25 tee.
Tip: Use the NW25 center rings and clamps provided in the startup kit.
Use the 7-mm nut driver to install the clamps.
4. Connect the opposite ends of the two lengths of vacuum hose in step 3 to
the two, 1-inch OD, straight, vacuum ports on the instrument’s rear
Caution:
• To prevent condensation from forming in the exhaust tubing
between the roughing pump and the exhaust trap bottle, you
must minimize the length of the tube.
• To avoid gas leaks, use the sharp knife to cut the PVC exhaust
tubing squarely (that is, perpendicular to its horizontal axis).
5. Attach the DN25 elbow to the DN25 nipple on the pump exhaust outlet
and secure the connection with a clamp.
6. Install the external silencer, with the arrow pointing toward the pump,
to the open port of the DN25 elbow, and then secure the connection with
a clamp.
7. Attach the DN25 reducing nipple to the outlet of the external silencer
and secure the connection with a clamp.
8. Connect an approximately 300 mm (12 inch) length of 12.7-mm clear
PVC exhaust tubing to the DN25 reducing nipple, securing the tubing
with a hose clamp.
9. Connect an elbow to the other end of the PVC exhaust tubing, and
connect the elbow to one of the fittings on the exhaust trap bottle
(included in the startup kit).
Exhaust port
TP02997
Elbow
TP02800
TP02996
Caution: To avoid gas leaks, use the sharp knife to cut the PVC
exhaust tubing squarely (that is, perpendicular to its horizontal
axis).
10. Connect a length of 12.7-mm clear PVC exhaust tubing to an elbow and
connect the elbow to the other fitting on the exhaust trap bottle. The exit
line of the exhaust trap bottle can be at any elevation.
11. Secure the exhaust trap bottle in a conspicuous location.
12. Route the open end of the exhaust tubing to a suitable exhaust vent.
13. Make the electrical connections to the roughing pump.
RS 232
1 1
Analog O ut InjectS tart In
2 2
3 G round 3 G round
4 4
N otused Event In
5
6
Stop Flow O ut
5
6
Sw itch 3 O ut
ETHERNET
7 7
ACN 065444751 8 G round 8 G round
9 9
Sw itch 2 O ut Sw itch 4 O ut
10 10
Serial Number
!
IVD
V ~ 200 - 240
Hz 50 - 60
VA 900
VACUUM
SOURCE VENT
VACUUM
01757 U.S.A.
To power source
RP00014
Caution: To avoid gas leaks, use the sharp knife to cut the PTFE
tubing squarely (that is, perpendicular to its horizontal axis).
1. Use the sharp knife to cut a 3.8 to 5.0-cm (1.5 to 2-inch) length of 6-mm
PTFE tubing.
2. Connect this piece of tubing to one end of the nitrogen supply in-line
filter.
3. Connect the remaining length of the 6-mm PTFE tubing to the other end
of the filter.
4. Connect the free end of the short piece of 6-mm PTFE tubing to the
nitrogen inlet port on the rear of the instrument.
RS 232
1 1
Analog O ut InjectS tart In
2 2
3 G round 3 G round
4 4
N otused Event In
5
6
Stop Flow O ut
5
6
Sw itch 3 O ut
ETHERNET
7 7
ACN 065444751 8 G round 8 G round
9 9
Sw itch 2 O ut Sw itch 4 O ut
10 10
Serial Number
V ~ 200 - 240
Hz 50 - 60
!
VA 900
PUMP
API Gas
6.9 Bar Maximum
Nitrogen inlet
VACUUM
SOURCE VENT
Source vent
VACUUM
Source
vacuum
RP00001
7. Connect the free end of the long piece of 6-mm PTFE tubing to the 6-mm
stud.
Warning:
• LC solvents and analytes can be carried in the nitrogen
exhaust, which must be vented via the nitrogen exhaust trap
bottle and laboratory exhaust system. The laboratory exhaust
system must provide a minimum vacuum of 0.20 kPa (2 mbar,
0.03 psi) below atmospheric pressure (negative pressure).
• The exhaust connections can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves when performing this
procedure.
• To avoid the buildup of hazardous gases, do not place the
nitrogen exhaust trap bottle in an enclosed cabinet.
Caution: To avoid gas leaks, use the sharp knife to cut the PTFE
tubing squarely (that is, perpendicular to its horizontal axis).
Caution: To avoid gas leaks, use the sharp knife to cut the PTFE
tubing squarely (that is, perpendicular to its horizontal axis).
4. Cut a second length of 10-mm tubing long enough to connect the exhaust
trap bottle to the exhaust vent.
5. Insert one end of the tubing into the remaining port on the exhaust trap
bottle. Route the other end to the exhaust vent.
6. Use snoop (or equivalent) leak detector liquid to ensure that there are no
leaks at the instrument exhaust and laboratory exhaust system line
connections.
To laboratory
exhaust port
From instrument (10-mm OD)
exhaust connection
(12-mm OD)
2. Slide a drain line over the barbed fitting of the drain (located at the
bottom of the instrument).
Drain cup
Barbed fitting
TP02684
Drain line
3. Route the waste line to the waste container. If necessary, shorten the
waste tube so that its end is above the surface of the waste solvent.
Correct Incorrect
TP01807
Caution: Do not connect the instrument’s power supply cord until you
complete the installation procedures in the previous sections.
The instrument’s rear panel includes two removable connectors that hold the
screw terminals for I/O signals. These connectors are keyed so that they can
receive a signal cable inserted only one way.
Connector I Connector II
Connector
Signal cable
TP02585
3. Slide the clamp (with the bend facing down) into the protective shield.
4. Insert the clamp and shield (with the bend facing down) into the
connection cover, and loosely tighten with one self-tapping screw.
Clamp
Shield
Connection cover
TP02586
Cable leads
Clamp
TP02587
6. Place the second connection cover over the first cover, and snap it into
place.
Signal connector
Connection cover
TP02588
Warning: To avoid electrical shock, use the SVT-type power cord in the
United States and HAR-type (or better) in Europe. For information
regarding what cord to use in other countries, contact your local
Waters distributor.
1. Connect the female end of the power cord to the receptacle on the rear
panel of the instrument.
2. Connect the male end of the instrument power cord to a suitable 200 to
240 V AC wall outlet.
3. Connect the power cord from the roughing pump relay box to a 200 to
240 V AC wall outlet.
The system software controls electrical power to the pump.
Contents
Topic Page
Preventing contamination C-2
Items exposed to solvent C-2
Solvents used to prepare mobile phases C-3
C-1
Preventing contamination
For information on preventing contamination, refer to Controlling
Contamination in LC/MS Systems (part number 715001307). You can find
this document on http://www.waters.com; click Services and Support and then
Support Center.
Item Material
Autotune reservoirs High-density polyethylene
Corona discharge pin mounting PEEK™
contact
Gas exhaust port Aluminium
Gas tubes Fluorinated ethylene propylene
Ion block Stainless steel
Ion block support PEEK
Isolation valve Gold-plated aluminium/bronze
O-rings ®
Viton or PTFE-encapsulated Viton
Probe adjuster bellows PTFE/Viton
Probe adjuster assembly Anodized aluminium, glass filled
acetal, and stainless steel
Probe shaft PEEK
Push-in gas fittings Nickel/brass
Solvent waste/leak management Tygon tubing
Source enclosure Alochromed aluminium
Source enclosure view port Toughened plate glass
Item Material
Trap bottle Polypropylene
Trap bottle push-in fittings Nitrile butadiene rubber, stainless
steel, polybutylene terephthalate,
and polyoxymethylene
Topic Page
Assembling required materials D-2
Preparing the sulfadimethoxine standard D-2
Storing the solutions D-3
Using the solution in an LC/MS System Check run D-3
D-1
Assembling required materials
You must assemble the following materials before starting to prepare your
sample:
• Solution kit containing 1 mg/mL sulfadimethoxine stock in methanol.
This solution kit is provided with your instrument.
• 1 L of solvent made up of 90:10 water/acetonitrile plus 0.1% formic acid
(v/v).
• Clean class A volumetric flasks: 100-mL (2), 10-mL.
• Clean class A pipettes (TD), 1-mL (3).
• PTFE-sealed screw-top amber sample bottles (glass or Nalgene™):
125-mL (2), 15-mL (2).
• Sample vial, 2-mL.
D-2 Preparing Samples for LC/MS System Check with Empower software
5. Into the 10-mL volumetric flask, pour 2 mL of the solution created in
step 4.
6. Dilute to the 10 mL mark with solvent.
Result: The flask contains the 20 pg/µL sulfadimethoxine standard
solution.
Index-1
roughing pump B-3, B-10 vacuum connections B-2
signal connections B-29 verifying state of 2-4
vacuum B-2 disassembling
workstation B-25 cone gas assembly 4-24
Connections Insight, troubleshooting ion block assembly 4-33
with 4-5 probe adjuster 4-82
console, Waters Instrument 1-6 source enclosure 4-82
construction materials C-1 diverter valve positions 2-8
contamination, preventing C-2 door glass, tightening guidelines 4-86
corona pin drain tube positioning B-24
cleaning 4-4, 4-70 drip tray, installing 2-6
installing 3-6
mounting contact blanking plug E
installing 3-9 electrical symbols A-11
removing 3-5 electricity source, connecting B-31
removing 3-7 electrospray ionization 1-7
replacing 4-4, 4-70 emergency shutdown 2-12
covers, for signal connectors B-28 emptying
customer comments iii exhaust trap bottle 4-3, 4-12
liquid trap bottle 4-3, 4-14
D equipment guidelines viii, 5
demister element, replacing 4-4, 4-98 error messages, viewing 2-4
detector ESCi 1-7
calibrating 2-4 ESI
compliant solvents C-1 optimizing probe for ESCi 3-7
external wiring B-2 ESI probe
flow rates 2-5 capillary, replacing 4-3, 4-55
I/O signal connectors B-26 installing 3-2
materials of construction C-1 removing 3-9
operate LED 2-5 tip
power LED 2-5 cleaning 4-3, 4-54
preparing for working on the source replacing 4-54
4-8 Ethernet, connecting B-26
rear panel B-2 event signal connection B-28
rebooting 2-11 exhaust system
signal connectors B-26 checking for leaks 4-13, B-21
specifications 1-2 requirements B-20
starting 2-2 exhaust systems, separation of B-7,
tuning 2-4 B-20
Index-2
exhaust trap bottle B-22 handling symbols A-12
connecting B-7, B-16 hazards
emptying 4-3, 4-12 flammable solvents v
external connections B-1 high temperature vi I
extraction cone high voltage vii
cleaning 4-31 solvent leakage v
handling guidelines 4-39 heater cartridge assembly
extraction tool, cone gas assembly 4-24 replacing 4-75
hexapole assembly
F cleaning 4-47, 4-49
flammable solvents v, A-3 handling 4-48, 4-52
flow path diagrams 2-8 high temperature hazard vi
flow rates 2-5 high voltage hazard vii
fluidics system home position, of fluidics system
diverter valve positions diverter valve 2-8
combined 2-10
home 2-8 I
infusion 2-9 I/O signal connectors B-26
LC 2-9 in vitro diagnostic applications ix
waste 2-10 infusion position, of fluidics system
diverter valve 2-9
G inject start signal connection B-28
gas ballasting, roughing pump 4-3, inlet, overview 1-10
4-16 installing
gas cone, cleaning 4-21, 4-25 APCI probe 5-2
guidelines APCI probe sample capillary 4-66
calibration ix corona pin 3-6
demister element nut tightening corona pin mounting contact
4-101 blanking plug 3-9
door glass tightening 4-86 drip tray, solvent manifold 2-6
probe adjuster screw tightening ESI probe 3-2
4-87 low-volume vials 2-7
quality control ix reservoir bottles 2-7
thumbscrew tightening 4-87 solvent manifold drip tray 2-6
H instrument
handling case, cleaning 4-3, 4-12
extraction cone 4-39 LAN card B-26
hexapole assembly 4-48, 4-52 leaving ready for operation 2-12
waste liquid 4-13 integral reservoirs 1-3, 1-12
Index-3
IntelliStart cleaning 4-90
configuring 2-4 replacing 4-91
operating 1-13 low-volume vials, installing 2-7
overview 1-3, 1-12
intended use viii M
ion block maintenance
cleaning 4-31 safety 4-7
disassembling 4-33 schedule 4-3
grub screw 4-44 mass spectrometer
heater cartridge assembly, leaving ready for operation 2-12
replacing 4-75 mass spectrometer shock hazard A-4
removing 4-31 MassLynx software 1-5
ion optics 1-9 materials of construction C-1
ionization modes 3-2 mobile phases, solvents used in
APCI 1-8, 5-1 preparation of C-3
APPI 1-8 mode
ESI 1-7 scanning 1-10
IonSABRE APCI probe 5-2 selected ion recording 1-10
IP addresses 2-2 monitoring, system instrument LEDs
isolating source from instrument 4-9 2-5
isolation valve, cleaning 4-31 MS operating modes 1-10
IVD authorized representative x multi-mode ESCi source 1-2
L N
LAN card B-26 network cables B-25
LC, position of fluidics system diverter nitrogen
valve 2-9 exhaust, connecting B-20
LC/MS System Check D-1 supply
Leak sensors 1-10 connecting B-18
leaks, checking for 4-13, 4-60, 4-67, pressure requirements v, 2-2
B-21 NW25 tee, connecting B-5, B-14
LED O
monitoring 2-5 oil, roughing pump
operate 2-5 adding 4-20
power 2-3, 2-5 changing 4-4
status 2-3 checking level 4-3, 4-19, 4-97
liquid trap bottle, emptying 4-3, 4-14 replacing 4-95
liquid waste line, connecting B-23 opening source isolation valve 4-10
lower bezel air filter operate LED 2-5
Index-4
operating modes, MS 1-10 replacing
operating source isolation valve 4-9 air filter
O-ring removal kit 4-11 behind source probe 4-94
O-rings, removing 4-11 inside lower bezel 4-91 I
overview 1-2 APCI probe heater 4-4, 4-71
corona pin 4-4, 4-70
P demister element 4-4, 4-98
PEEK terminal block, removing 4-36, ESI probe capillary 4-3, 4-55
4-76 ESI probe tip 4-54
photomultiplier detection system 1-9 ion block heater cartridge assembly
power LED 2-3, 2-5 4-75
power supply, connecting to B-25 sample capillary 4-62
powering-on 2-2 source assembly seals 4-4, 4-79
pressure test, performing 4-79, 4-89 requirements
preventing contamination C-2 exhaust system B-20
probe adjuster nitrogen supply pressure v, 2-2
assembling 4-87 reservoir bottles, installing 2-7
disassembling 4-82 reservoirs, integral 1-3, 1-12
probe capillary reset button 2-11
replacing 4-4 roughing pump 1-10
pump, gas ballasting 4-3 clearances B-4, B-13
Q connecting B-3, B-10
quality control guidelines ix gas ballasting 4-3, 4-16
oil
R adding 4-20
rear panel B-2 checking level 4-3, 4-19, 4-97
rebooting detector 2-11 replacing 4-95
relay box, connecting B-9 replacing demister element 4-4,
removing 4-98
APCI probe sample capillary 4-62 setting up B-4, B-13
corona pin 3-7 site requirements B-4, B-13
corona pin mounting contact
blanking plug 3-5 S
ESI probe 3-9 safety advisories A-1
ion block assembly 4-31 safety procedures, maintenance 4-7
O-rings 4-11 sample 4-62
PEEK terminal block 4-36, 4-76 sample bottles D-3
seals 4-11 sample capillary, replacing 4-62
replacement parts 4-5 sample cone, cleaning 4-21, 4-25
Index-5
sample inlet, overview 1-10 replacing 4-94
scan speed 1-2 spare parts 4-5
scanning mode 1-10 specifications 1-2
seals, removing 4-11 SQ detector
selected ion recording (SIR) mode 1-10 overview 1-2
shutdown starting, detector 2-2
emergency 2-12 status LED 2-3
signal connections, connecting B-29 stop flow signal connection B-28
site requirements, roughing pump B-4, sulfadimethoxine standard D-1
B-13 switch signal connection B-28
solvent leakage hazard v symbols
solvent manifold drip tray, installing caution A-5
2-6 electrical A-11
solvent vapor leakage, avoiding 4-79 handling A-12
solvents warning A-2
compliant C-1
exposure of detector components to T
C-2 thumbscrews, tightening 4-87
use in mobile phases C-3 tightening
source demister element nut 4-101
cleaning 4-3, 4-21 thumbscrews 4-87
enclosure trademarks ii
assembling 4-87 trap bottle
disassembling 4-82 connecting B-22
seals, replacing 4-79 emptying 4-12
hexapole assembly troubleshooting 4-5
cleaning 4-49 tuning 2-4
ion block assembly, assembling turbomolecular pump 1-10
4-42 V
isolation valve vacuum
closing 4-9 connections B-2
opening 4-10 system 1-10
operating 4-9 valve
preparing for work on 4-8 diverter 2-8
pressure test 4-89 source isolation 4-9
replacing assembly seals 4-4
types 1-2 W
source probe air filter warning symbols A-2, A-5
cleaning 4-92 waste
Index-6
bottle, emptying 4-14
line, connecting B-23
liquid, handling 4-13
waste position, of fluidics system I
diverter valve 2-10
Waters Instrument, console 1-6
wiring, external B-2
workstation, connecting B-25
Z
ZSpray source 1-2
Index-7
Index-8