Waters 3100 Detector Operator`s Guide, 71500135102rB

Waters 3100 Detector Operator`s Guide, 71500135102rB
Waters 3100 Detector
Operator’s Guide
71500135102/Revision B
Copyright © Waters Corporation 2007.
All rights reserved.
Copyright notice
© 2007 WATERS CORPORATION. PRINTED IN THE UNITED STATES OF
AMERICA AND IRELAND. ALL RIGHTS RESERVED. THIS DOCUMENT
OR PARTS THEREOF MAY NOT BE REPRODUCED IN ANY FORM
WITHOUT THE WRITTEN PERMISSION OF THE PUBLISHER.
The information in this document is subject to change without notice and
should not be construed as a commitment by Waters Corporation. Waters
Corporation assumes no responsibility for any errors that may appear in this
document. This document is believed to be complete and accurate at the time
of publication. In no event shall Waters Corporation be liable for incidental or
consequential damages in connection with, or arising from, its use.
Trademarks
ESCi, UPLC, and Waters are registered trademarks of Waters Corporation.
Empower, IntelliStart, IonSABRE, MassLynx, and ZSpray are trademarks of
Waters Corporation.
Nalgene is a registered trademark of Nalge Nunc International.
PEEK is a trademark of Victrex Corporation.
snoop is a registered trademark 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.
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.
ii
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.
Waters contact information
Contacting medium
Information
Internet
The Waters Web site includes e-mail
addresses for Waters locations worldwide.
Visit www.waters.com, and click About Waters
> Worldwide Offices.
Telephone
From the USA or Canada, phone 800
252-HPLC, or fax 508 872-1990.
For other locations worldwide, phone and fax
numbers appear in the Waters Web site.
Conventional mail
Waters Corporation
34 Maple Street
Milford, MA 01757
USA
iii
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.
Considerations specific to the 3100 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.
iv
Flammable solvents hazard
Warning: To prevent the ignition of accumulated solvent vapors inside
the source, maintain a continuous flow of nitrogen through the source
whenever significant amounts of flammable solvents are used during
the instrument’s operation.
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.
High temperature hazard
Warning: To avoid burn injuries, avoid touching the source enclosure
with your hand when operating or servicing the instrument.
3100 detector high temperature hazard
Source enclosure assembly
v
High voltage hazard
Warning:
• To avoid electric shock, do not remove the 3100 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.
vi
Operating this instrument
When operating this instrument, follow standard quality control procedures
and the guidelines presented in this section.
Symbols
Symbol
Definition
Authorized representative of the European
Community
Confirms that a manufactured product complies with
all applicable European Community directives.
For in vitro diagnostic use
Intended use
Waters designed the Single Quad (3100) Detector for use as a research tool to
deliver authenticated mass measurement in MS mode.
The Waters 3100 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 3100 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.
To calibrate mass spectrometers, consult the calibration section of the
operator’s guide for the instrument you are calibrating.
vii
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:
viii
•
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.
IVD authorized representative information
IVD authorized representative
Waters Corporation (Micromass UK Limited) is
registered in the United Kingdom with the Medicines
and Healthcare Products Regulatory Agency (MHRA)
at Market Towers, 1 Nine Elms Lane, London,
SW8 5NQ. The reference number is IVD000167.
Waters Corporation (Micromass UK Ltd.)
Floats Road
Wythenshawe
Manchester M23 9LZ
United Kingdom
Telephone:
+44-161-946-2400
Fax:
+44-161-946-2480
Contact:
Quality manager
ix
x
Table of Contents
Copyright notice ................................................................................................... ii
Trademarks ............................................................................................................ ii
Customer comments ............................................................................................. ii
Contacting Waters ............................................................................................... iii
Safety considerations .......................................................................................... iv
Considerations specific to the 3100 detector ..................................................... iv
Safety advisories ................................................................................................. vi
Operating this instrument ................................................................................ vii
Symbols ............................................................................................................. vii
Intended use...................................................................................................... vii
Calibrating ........................................................................................................ vii
Quality control ................................................................................................. viii
IVD authorized representative information ................................................. ix
IVD authorized representative .......................................................................... ix
1 Waters 3100 Detector Overview .......................................................... 1-1
Overview ............................................................................................................. 1-2
Waters 3100 Detector ...................................................................................... 1-2
Software and data system ............................................................................... 1-4
Ionization techniques and source probes ................................................... 1-4
Electrospray ionization (ESI) .......................................................................... 1-4
Combined electrospray ionization and atmospheric pressure chemical ionization
(ESCi) ......................................................................................................... 1-5
Atmospheric pressure chemical ionization..................................................... 1-5
Atmospheric pressure photoionization ........................................................... 1-6
Table of Contents
xi
Ion optics ............................................................................................................. 1-6
MS operating modes ......................................................................................... 1-7
Sample inlet ........................................................................................................ 1-7
Vacuum system .................................................................................................. 1-7
Rear panel ........................................................................................................... 1-8
IntelliStart fluidics system overview ........................................................... 1-9
IntelliStart fluidics system operation ........................................................ 1-10
Operating the IntelliStart fluidics system ................................................... 1-10
Operating the IntelliStart fluidics system from the Tune window............. 1-11
Programming the MS instrument method to operate the IntelliStart fluidics
system ....................................................................................................... 1-11
2 Preparing the Detector for Operation .............................................. 2-1
Starting the detector ........................................................................................
Configuring IntelliStart...................................................................................
Verifying the instrument’s state of readiness ................................................
Tuning and calibration information ...............................................................
Monitoring the detector LEDs ........................................................................
2-2
2-4
2-4
2-4
2-4
Preparing the IntelliStart fluidics system .................................................. 2-6
Installing the solvent manifold drip tray ....................................................... 2-6
Installing the reservoir bottles........................................................................ 2-7
Diverter valve positions................................................................................... 2-8
Purging the infusion syringe......................................................................... 2-11
Rebooting the detector .................................................................................. 2-11
Rebooting the detector by pressing the reset button ................................... 2-11
Shutting down the detector ..........................................................................
Putting the detector in Standby mode for overnight shutdown ..................
Complete detector shutdown.........................................................................
Emergency detector shutdown ......................................................................
xii
Table of Contents
2-12
2-13
2-13
2-14
3 ESI and ESCi Modes of Operation ..................................................... 3-1
Introduction ....................................................................................................... 3-2
Installing the ESI probe .................................................................................. 3-2
Installing the corona pin ................................................................................. 3-5
Optimizing the ESI probe for ESCi operation ........................................... 3-8
Removing the corona pin ................................................................................ 3-9
Removing the ESI probe ............................................................................... 3-11
4 Operating the Detector ......................................................................... 4-1
Setting-up the instrument .............................................................................. 4-2
Performing a sample tune .............................................................................. 4-6
Developing experiment methods .................................................................. 4-7
Verifying the system ....................................................................................... 4-10
5 Maintenance Procedures ..................................................................... 5-1
Maintenance schedule ..................................................................................... 5-3
Spare parts ......................................................................................................... 5-5
Safety and handling ......................................................................................... 5-5
Preparing the instrument for working on the source ............................. 5-6
Operating the source isolation valve ........................................................... 5-7
Removing O-rings and seals ........................................................................... 5-9
Cleaning the instrument case ...................................................................... 5-10
Cleaning the source cleanout tray ..............................................................
Removing the source cleanout tray from the source ....................................
Cleaning the source cleanout tray ................................................................
Refitting the source cleanout tray to the source ..........................................
Table of Contents
5-10
5-11
5-12
5-14
xiii
Emptying the instrument exhaust trap bottle ......................................... 5-15
Emptying the roughing pump exhaust liquid trap bottle ..................... 5-16
Gas ballasting the roughing pump ............................................................. 5-20
Gas ballasting a pump fitted with a screwdriver-operated gas ballast
valve.......................................................................................................... 5-21
Gas ballasting a pump fitted with a handle-operated gas ballast valve .... 5-22
Checking the roughing pump oil level ....................................................... 5-23
Adding oil to the roughing pump ................................................................ 5-23
Cleaning the source components ................................................................ 5-25
Cleaning the sample cone and gas cone ....................................................
Removing the cone gas assembly from the source .......................................
Disassembling the cone gas assembly ..........................................................
Cleaning the sample cone and gas cone........................................................
Assembling the cone gas assembly ...............................................................
Fitting the cone gas assembly to the source.................................................
5-25
5-25
5-28
5-29
5-32
5-33
Cleaning the ion block, isolation valve, and extraction cone ..............
Removing the ion block assembly from the source assembly ......................
Disassembling the source ion block assembly..............................................
Cleaning the ion block, isolation valve, and extraction cone.......................
Assembling the source ion block assembly...................................................
Fitting the ion block assembly to the source assembly................................
5-35
5-35
5-37
5-44
5-46
5-49
Cleaning the source hexapole assembly .................................................... 5-51
Removing the ion block assembly, ion block support, and hexapole from the
source assembly ....................................................................................... 5-51
Cleaning the hexapole assembly ................................................................... 5-52
Fitting the hexapole assembly, PEEK ion block support, and ion block assembly
to the source assembly ............................................................................. 5-55
xiv
Table of Contents
Replacing the ESI probe tip ......................................................................... 5-57
Replacing the ESI probe sample capillary ............................................... 5-58
Cleaning the IonSABRE APCI probe tip ................................................... 5-65
Replacing the IonSABRE APCI probe sample capillary ....................... 5-65
Removing the existing capillary.................................................................... 5-65
Installing the new capillary .......................................................................... 5-69
Cleaning or replacing the corona pin ........................................................ 5-73
Replacing the APCI probe heater ............................................................... 5-74
Replacing the ion block source heater ...................................................... 5-77
Replacing the source assembly seals ......................................................... 5-81
Removing the source enclosure from the instrument .................................. 5-81
Disassembling the source enclosure and probe adjuster assembly............. 5-84
Removing the seals from the source enclosure and probe adjuster
assembly ..................................................................................................... 5-85
Fitting the new source enclosure and probe adjuster assembly seals ........ 5-88
Assembling the probe adjuster assembly and source enclosure.................. 5-89
Fitting the source enclosure to the instrument............................................ 5-90
Maintaining the detector air filters ............................................................
Cleaning the air filter inside the instrument’s door ....................................
Replacing the air filter inside the instrument’s door...................................
Cleaning the air filter inside the instrument’s lower bezel .........................
Replacing the air filter inside the lower bezel..............................................
Cleaning the air filter behind the source probe ...........................................
Replacing the air filter behind the source probe ..........................................
Table of Contents
5-91
5-91
5-92
5-93
5-94
5-95
5-97
xv
Replacing the roughing pump oil ............................................................... 5-98
Replacing the roughing pump’s oil demister element ......................... 5-101
6 Optional APCI Mode of Operation ..................................................... 6-1
Atmospheric pressure chemical ionization ................................................ 6-2
IonSABRE APCI probe .................................................................................... 6-3
Installing the IonSABRE APCI probe .......................................................... 6-3
Installing the corona pin ................................................................................. 6-6
Removing the corona pin ................................................................................ 6-6
Removing the IonSABRE APCI probe ......................................................... 6-7
A Safety Advisories .................................................................................. A-1
Warning symbols ............................................................................................... A-2
Task-specific hazard warnings........................................................................ A-2
Warnings that apply to particular instruments, instrument components, and
sample types ...............................................................................................A-3
Caution symbol .................................................................................................. A-5
Warnings that apply to all Waters instruments ......................................... A-6
Electrical and handling symbols ................................................................. A-13
Electrical symbols .......................................................................................... A-13
Handling symbols .......................................................................................... A-14
B External Connections .......................................................................... B-1
Detector external wiring and vacuum connections ................................ B-2
Connecting the oil-filled roughing pump ................................................... B-3
Making the electrical connections for a roughing pump with an external relay
box
B-8
Making the electrical connections for a roughing pump without an external
relay box .....................................................................................................B-9
Connecting the oil-free roughing pump ................................................... B-10
Making the electrical connections for an oil-free roughing pump............... B-17
xvi
Table of Contents
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-25
I/O signal connectors ..................................................................................... B-26
Signal connections ......................................................................................... B-28
Connecting to the electricity source ......................................................... B-31
C Materials of Construction and Compliant Solvents ..................... C-1
Preventing contamination ............................................................................. C-2
Items exposed to solvent ................................................................................ C-2
Solvents used to prepare mobile phases .................................................... C-3
D Preparing Samples for LC/MS System Check with Empower
software ....................................................................................................... D-1
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
Index ..................................................................................................... Index-1
Table of Contents
xvii
xviii
Table of Contents
1
Waters 3100 Detector Overview
This chapter describes the instrument, including its controls and gas
and plumbing connections.
Contents
Topic
Page
Overview
1-2
Ionization techniques and source probes
1-4
Ion optics
1-6
MS operating modes
1-7
Sample inlet
1-7
Vacuum system
1-7
Rear panel
1-8
IntelliStart fluidics system overview
1-9
IntelliStart fluidics system operation
1-10
1-1
Overview
Waters 3100 Detector
The Waters® 3100 Detector is a single-quadrupole, atmospheric pressure
®
ionization (API) mass spectrometer. Designed for routine 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 detector specifications, see the Waters 3100 Detector Site Preparation
Guide.
Waters 3100 Detector
TP02592
1-2
Waters 3100 Detector Overview
Waters 3100 Detector with doors open
NEBULIZER
POWER
OPERATE
DESOLVATION
HV
PROBE
TP02627
IntelliStart technology
IntelliStart™ technology monitors LC/MS performance and reports when the
detector is ready for use.
The IntelliStart software automatically tunes and mass calibrates the
detector and displays performance readbacks. Integrated with Empower™
chromatography or MassLynx™ mass spectrometry software, IntelliStart
enables simplified setup of the system for use in routine analytical and open
access applications. (See “Software and data system” on page 1-4).
The IntelliStart fluidics system is built into the detector. 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 detector’s online Help for further details of IntelliStart.
Overview
1-3
Software and data system
The detector is controlled by either Empower chromatography software or
MassLynx mass spectrometry software. Each is a high-performance
application that acquires, analyzes, manages, and distributes ultraviolet
(UV), evaporative light scattering, analog, and mass spectrometry data.
Both Empower and MassLynx software enable these major operations:
•
Configuring the instrument.
•
Creating LC and MS methods that define operating parameters for a
run.
•
Using IntelliStart software to tune and mass calibrate the detector.
•
Running samples.
•
Monitoring the run.
•
Acquiring data.
•
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.
Ionization techniques and source probes
Electrospray ionization (ESI)
In electrospray ionization (ESI), a strong electrical charge is given the eluent
as it emerges from a nebulizer. The droplets that compose the resultant
aerosol undergo a reduction in size (solvent evaporation). As solvent continues
to evaporate, the charge density increases until the droplet surfaces eject ions
(ion evaporation). The ions can be singly or multiply charged. The multiply
charged ions are of particular interest because the detector separates them
according to their mass-to-charge ratios (m/z), permitting the detection of
high-molecular-weight compounds.
The instrument can accommodate eluent flow rates of up to 1 mL/min.
1-4
Waters 3100 Detector Overview
Combined electrospray ionization and atmospheric pressure
chemical ionization (ESCi)
Combined electrospray ionization and atmospheric pressure chemical
ionization (ESCi) is supplied as standard equipment on the detector. In ESCi,
the standard ESI probe is used in conjunction with a corona pin to allow
alternating acquisition of ESI and APCI ionization data, facilitating high
throughput and wider compound coverage. See “Electrospray ionization (ESI)”
on page 1-4.
ESCi mode
Corona pin
TP02695
Sample cone tip
Atmospheric pressure chemical ionization
A dedicated high performance atmospheric pressure chemical ionization
(APCI) probe is offered as an option. See Chapter 6, “Optional APCI Mode of
Operation”, for full details.
Ionization techniques and source probes
1-5
Atmospheric pressure photoionization
Atmospheric pressure photoionization (APPI) is offered as an option. It uses
photons generated by a krypton-discharge ultraviolet (UV) lamp (∼10.2 eV) to
produce sample ions from vaporized LC eluent.
Ion optics
The detector’s ion optics operate as follows:
1.
Samples from the LC or Intellistart fluidics system are introduced at
atmospheric pressure into the ionization source.
2.
The ions pass through the sample cone into the vacuum system.
3.
Ions are filtered according to their mass-to-charge ratio (m/z).
4.
The transmitted ions are detected by the photomultiplier detection
system.
5.
The signal is amplified, digitized, and sent to the Empower
chromatography or MassLynx mass spectrometry software.
Ion optics overview
Sample cone
Sample inlet
Transfer optics
Conversion dynode
Quadrupole
Detector
Isolation valve
Z-Spray ion source
1-6
Waters 3100 Detector Overview
MS operating modes
The detector has two modes of operation:
•
Scanning, where the detector is scanned to separate the ions in the ion
beam according to their mass-to-charge (m/z) ratio and hence produce a
mass spectrum.
•
Selected Ion Recording (SIR), where the detector is tuned to detect an
ion, or ions, with specific m/z ratios.
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.
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.
Vacuum leaks and electrical or vacuum pump failures cause vacuum loss,
which protective interlocks guard against. The system monitors
turbomolecular pump speed and continuously measures vacuum pressure
with a built-in Pirani gauge. The gauge also serves as a switch, stopping
operation when it senses vacuum loss.
A vacuum isolation valve isolates the source from the mass analyzer, allowing
routine source maintenance without venting.
MS operating modes
1-7
Rear panel
The following figure shows the rear panel locations of the connectors used to
operate the detector with external devices.
Detector rear panel
1
2
3
4
5
6
ACN 065444751
7
8
9
10
Analog
Out
Stop Flow
2
4
5
Out
Ground
Switch 2
1
3
Ground
Not used
Out
6
7
8
9
10
In
Inject Start
Ground
In
Event
Switch 3
Out
Ground
Switch 4
Out
Serial Number
Nitrogen inlet
Event inputs
and outputs
RS 232
API Gas
6.9 Bar Maximum
Power cord
Shielded
Ethernet
ETHERNET
V ~ 200 - 240
Hz 50 - 60
VA 900
!
Roughing pump
relay switch
PUMP
SOURCE
VENT
Source vent
Turbo vacuum
VACUUM
VACUUM
Source
vacuum
Waters Corporation
34 Maple Street Milford, MA 01757 U.S.A.
TP02591
1-8
Waters 3100 Detector Overview
IntelliStart fluidics system overview
The IntelliStart fluidics system is built into the detector. 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 IntelliStart system incorporates a multi-position valve with these
attributes:
•
An input connection from an external LC column.
•
An input connection from the detector’s infusion syringe. (The detector’s
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 detector’s probe.
•
An output connection to a waste line.
Fluidics system
Probe
B
LC
Idle
Off
A
Off
Column
Syringe
LC
Waste
Reservoir A
Reservoir B
IntelliStart fluidics system overview
1-9
IntelliStart fluidics system operation
Control of solvent and sample delivery during auto-tuning, auto-calibration,
and method development is automatically performed by the software.
IntelliStart configuration requirements can be set in the system console. You
can edit the parameters, frequency, and extent of the automation you want
IntelliStart to perform. See the detector’s online Help for further details of
IntelliStart.
Operating the IntelliStart fluidics system
To enable the fluidics system controls (Empower only)
In the console system tree, expand 3100 Detector.
To set the infusion flow rate
In the console window, click the current flow rate.
To select the reservoir
In the console window, click the highlighted reservoir bottle text—A or
B.
To select the flow state
In the console window, click the diverter valve position label.
To start the infusion syringe flow
In the console window, click
. A status bar indicates the amount of
fluid in the syringe and the amount of time remaining before the fluid
empties. When the syringe is empty the system becomes idle.
To refill the infusion syringe
In the console window, click
1-10
Waters 3100 Detector Overview
.
To purge the infusion syringe
In the console window, click
. For further details, see “Purging the
infusion syringe” on page 2-11.
To stop the current action
In the console window, click
.
To disable the fluidics system controls (Empower only)
In the console window, click Control
.
Operating the IntelliStart fluidics system from the Tune window
To operate the IntelliStart fluidics system from the Tune window
1.
In the Console system tree, click 3100 Detector.
2.
Click Tune
3.
In the 3100 Detector Tune window, click the Fluidics tab.
4.
Set the Flow Control parameters according to the instructions in the
Empower or MassLynx online Help.
.
Programming the MS instrument method to operate the IntelliStart
fluidics system
In the MS instrument method, you can program the operation of the system’s
multi-position valve to infuse sample during a run. The valve can also divert
LC flow to waste as a timed event.
To program the MS instrument method using MassLynx software
1.
In the MassLynx window, click MS Method.
2.
In the MS Methods window, click Options > Method Events.
IntelliStart fluidics system operation
1-11
3.
In the Method events dialog box, select the desired flow state, as
indicated by the following table.
Flow states and results
Flow state setting
LC flows to
Syringe flows to
LC
3100 probe
Waste
Combined
3100 probe
3100 probe
Infusion
Waste
3100 Probe
Waste
Waste
Waste
No change
No change
No change
Tip: At the time you power-on the instrument, the LC state is “waste”.
For further instruction, see the MassLynx online Help topic “Advanced
Methods and Events”.
To program the MS instrument method using Empower software
1-12
1.
In the Empower Pro interface click Run Samples, select your system,
and then click OK.
2.
In the Run Samples window, click Edit > Instrument Method.
3.
In the instrument method editor, click the button representing your MS
detector.
4.
Click Events.
Waters 3100 Detector Overview
5.
On the Events tab, select the desired flow path, as indicated by the
following table.
Flow paths and results
Flow path setting
LC flows to
Syringe flows to
LC
3100 probe
Waste
Combined
3100 probe
3100 probe
Infusion
Waste
3100 Probe
Waste
Waste
Waste
No change
No change
No change
Tip: At the time you power-on the instrument, the LC state is “waste”.
For further instruction, see the Empower online Help topic “Configuring
events”.
IntelliStart fluidics system operation
1-13
1-14
Waters 3100 Detector Overview
2
Preparing the Detector for
Operation
This chapter describes how to start and shut-down the detector.
Contents
Topic
Page
Starting the detector
2-2
Preparing the IntelliStart fluidics system
2-6
Rebooting the detector
2-11
Shutting down the detector
2-12
2-1
Starting the detector
Caution: Using incompatible solvents can cause severe damage to the
instrument. Refer to Appendix C, “Materials of Construction and
Compliant Solvents”, for 3100 detector solvent information.
Starting the detector entails powering-on the workstation, logging into the
workstation, powering-on the detector and all the other instruments, and
starting the Empower or MassLynx software.
Requirement: You must power-on and log in to the workstation first to ensure
that it obtains the IP addresses of the system instruments.
To start the detector
Warning: During analyses that require flammable solvents, to avoid
ignition of the solvents, never let the nitrogen supply pressure fall
below 690 kPa (6.9 bar, 100 psi).
1.
Ensure the nitrogen supply is connected to the instrument’s API gas
connection.
Requirement: The nitrogen must be dry and oil-free, with a purity of at
least 95%. Regulate the supply at 600 to 690 kPa (6.0 to 6.9 bar, 90 to
100 psi).
For more information on connections, see the figure “Detector rear
panel” on page 1-8.
2.
Power-on the HPLC system workstation, and log in before powering-on
the other instruments.
3.
Press the power switch on the top, left-hand side of the detector and
HPLC instruments. Each system instrument “beeps” and runs a series
of startup tests.
4.
Allow 3 minutes for the embedded PC to initialize. An audible alert
sounds when the PC is ready.
The power and status LEDs change as follows:
•
2-2
Each system instrument’s power LED shows green.
Preparing the Detector for Operation
•
During initialization, the binary solvent manager’s and sample
manager’s status LED flashes green.
•
After the instruments are successfully powered-on, all power LEDs
show steady green. The binary solvent manager’s flow LED, the
sample manager’s run LED, and the detector’s Operate LED remain
off.
5.
Start Empower or MassLynx software. You can monitor the console for
messages and LED indications.
6.
Launch IntelliStart using one of the following methods.
•
MassLynx – In the MassLynx main window’s lower left-hand corner,
click IntelliStart.
•
Empower – In the Run Samples window, right-click the detector’s
control panel, and then click Launch Intellistart.
Result: The detector’s console appears. The detector is in Standby mode.
7.
Click Control > Pump to start the roughing pump. The Operate LED
remains off.
Tip: There is a 20-second delay, during which the turbopump is starting,
before the roughing pump starts. IntelliStart displays “Instrument in
standby”.
8.
Click Resolve
or Operate
to put the detector into Operate mode.
When the detector is in good operating condition, IntelliStart displays
“Ready”.
Tip: Clicking Resolve
prepares the system for operation, putting the
detector into Operate mode. If clicking Resolve fails to put the
instrument into Operate mode, IntelliStart displays corrective actions.
Starting the detector
2-3
Configuring IntelliStart
To configure IntelliStart
1.
In the console system tree, expand 3100 Detector.
2.
Click IntelliStart.
3.
Click Configure > IntelliStart Configuration.
4.
In the IntelliStart Configuration dialog box, in the Checks list, select the
check boxes for the items you want checked during 3100 detector
startup. Clear the check boxes of items you do not want checked.
Tip: To display detailed information for an item, highlight it and then
click Properties.
5.
Click OK.
Verifying the instrument’s state of readiness
When the detector is in good operating condition, the power and Operate
LEDs show constant green. You can view any error messages in IntelliStart.
To access IntelliStart
1.
In the console system tree, expand 3100 Detector.
2.
Click IntelliStart.
Tuning and calibration information
The detector must be tuned and calibrated prior to use, tasks normally
performed from IntelliStart.
For further instruction, see the detector’s online Help topic “Instrument
Setup” and Chapter 4, “Operating the Detector”.
Monitoring the detector LEDs
Light-emitting diodes on the detector indicate its operational status.
2-4
Preparing the Detector for Operation
Power LED
The power LED, to the top, left-hand side of the detector’s front panel,
indicates when the detector 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 detector’s online Help topic “Monitoring the detector LEDs” for details
of the Operate LED indications.
Starting the detector
2-5
Preparing the IntelliStart fluidics system
For additional information, see “Connecting the liquid waste line” on
page B-23.
Installing the solvent manifold drip tray
Required material
Chemical-resistant, powder-free gloves
To install the solvent manifold drip tray
Warning: The solvent manifold drip tray can be contaminated
with biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
Install the solvent manifold drip tray as shown below:
TP02685
2-6
Preparing the Detector for Operation
Installing the reservoir bottles
An optional Low-volume Adaptor Kit is available for infusing smaller
volumes. The low-volume vials have a volume of 1.5 mL.
Required material: Chemical-resistant, powder-free gloves
To install the reservoir bottles
Warning: The reservoir bottles can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
1.
Remove the reservoir bottle caps.
2.
Screw the reservoir bottles onto the detector as shown below.
TP02630
To install low-volume vials
Warning: The reservoir bottles can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
1.
If a standard reservoir bottle is fitted, remove the reservoir bottle.
2.
Screw the low-volume adaptor into the manifold and tighten it
finger-tight.
Preparing the IntelliStart fluidics system
2-7
3.
Screw the low-volume vial into the adaptor.
TP02630
Diverter valve positions
Column and syringe in home position after power-up
After power-up, the flow path between the column and waste is open. The
syringe is empty, and the flow path between it and waste is open.
Probe
B
Waste
Idle
Off
A
Off
Column
Syringe
LC
2-8
Waste
Preparing the Detector for Operation
Reservoir A
Reservoir B
LC position
In the LC position, the flow path between the LC and probe is open, and the
flow path between the syringe and waste is also open.
Probe
B
LC
Idle
Off
A
Off
Column
Syringe
LC
Waste
Reservoir A
Reservoir B
Infusion position
Probe
B
Infusion
Infusion
Off
A
On
Column
Syringe
LC
Waste
Reservoir A
Reservoir B
Preparing the IntelliStart fluidics system
2-9
Combined position with LC flow and syringe in idle mode
Probe
B
Combined
Idle
Off
A
Off
Column
Syringe
LC
Waste
Reservoir A
Reservoir B
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
B
Waste
Idle
Off
A
Off
Column
Syringe
LC
2-10
Waste
Preparing the Detector for Operation
Reservoir A
Reservoir B
Purging the infusion syringe
Whenever you replace a solution bottle, purge the infusion syringe with the
solution that you are going to use next.
Tip: Depending on the solutions used, the IntelliStart fluidics system can
require more than one purge cycle to minimize carryover.
To purge the infusion syringe
1.
In the console system tree, expand 3100 Detector.
2.
If you use MassLynx software, click Interactive Display; otherwise click
Interactive Fluidics.
3.
If you use Empower software, click Control
4.
Select the required solution reservoir.
5.
Click
.
to purge the system.
Tip: System purge takes approximately 2 minutes and uses a total
volume of 800 µL.
Rebooting the detector
Reboot the detector when any of these conditions applies
•
The Tune window fails to respond.
•
Empower or MassLynx software fails to initialize.
•
Immediately following a software upgrade.
Rebooting the detector by pressing the reset button
The reset button shuts down the electronics momentarily and causes the
detector to reboot.
To reboot the detector by pressing the reset button
1.
Open the detector’s front, left-hand door.
Rebooting the detector
2-11
2.
Press the red reset button on the top, left-hand side of the instrument.
Reset button
TP02687
Shutting down the detector
Recommendation: Leave the detector in Operate mode except when
performing routine maintenance.
If you must shut down the detector, refer to the instructions in this section.
Caution: Buffers left in the system can precipitate and damage
instrument components.
Tip: Set system shutdown parameters in the shutdown editor. Consult the
MassLynx online Help for more information.
2-12
Preparing the Detector for Operation
Putting the detector in Standby mode for overnight shutdown
To put the detector in Standby mode overnight
1.
Ensure that there is sufficient capacity in the waste container for the LC
flow that is to be diverted to waste. See “Connecting the liquid waste
line” on page B-23.
2.
In the console, click
to stop the LC flow or, if column flow is
required, divert the LC flow to waste as follows:
3.
a.
In the console system tree, expand 3100 Detector.
b.
If you use MassLynx software, click Interactive Display; otherwise
click Interactive Fluidics.
c.
If you use Empower software, click Control
d.
Click the current diverter valve position label.
e.
In the Select a Flow State dialog box, select Waste.
f.
Click OK.
Click Standby
.
to shut off heaters and voltages.
Tip: You can create a method to stop the gas flow or lower the
temperature. See the Empower or MassLynx online Help for more
information on creating methods.
Complete detector shutdown
To completely shut down the detector
1.
Put the detector in Standby mode. See “Putting the detector in Standby
mode for overnight shutdown” on page 2-13.
2.
In the console, click API
3.
Click Control > Vent.
.
Result: The turbomolecular pump is switched off. When the
turbomolecular pump runs down to half its normal operating speed, the
vent valve opens and the instrument is automatically vented. The
Operate LED changes from green to red and then turns off.
Shutting down the detector
2-13
4.
Exit MassLynx or Empower software.
5.
After the roughing pump shuts off, operate the power button (on the
front of the instrument) to power-off the detector.
Warning: The 3100 detector’s power switch does not isolate the
instrument from the main power supply. To isolate the
instrument, you must disconnect the power cable from the back
of the instrument.
6.
Disconnect the power cable from the back of the detector.
7.
Power-off all other instruments and the workstation.
Note: The fans inside some instruments run continuously, even after
you power-off the instruments.
Emergency detector shutdown
To shut down the detector in an emergency
Warning: The 3100 detector’s power switch does not isolate the
instrument from the main power supply. To isolate the instrument,
you must disconnect the power cable from the back of the instrument.
Caution: Data can be lost during an emergency shutdown.
2-14
1.
Operate the power button on the front of the detector.
2.
Disconnect the power cable from the back of the detector.
Preparing the Detector for Operation
3
ESI and ESCi Modes of
Operation
This chapter describes how to prepare the detector for the following
modes of operation:
•
ESI (electrospray ionization).
•
ESCi (combined electrospay and atmospheric pressure chemical
ionization).
If your system uses APCI mode, see Chapter 6, “Optional APCI Mode of
Operation”.
Contents
Topic
Page
Introduction
3-2
Installing the ESI probe
3-2
Installing the corona pin
3-5
Optimizing the ESI probe for ESCi operation
3-8
Removing the corona pin
3-9
Removing the ESI probe
3-11
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 1-4. and
“Combined electrospray ionization and atmospheric pressure chemical
ionization (ESCi)” on page 1-5.
Installing the ESI probe
Required material: Chemical-resistant, powder-free gloves
To install the ESI probe
Warning: The HPLC system connections, ESI probe, and source
can be contaminated with biohazardous and/or toxic materials.
Always wear chemical-resistant, powder-free gloves while
performing this procedure.
Warning: To avoid electric shock, ensure that the instrument is
suitably prepared before commencing this procedure.
1.
Prepare the instrument for working on the source. See “Preparing the
instrument for working on the source” on page 5-6.
Warning: The source can be hot. To avoid burn injuries, take
great care while working with the instrument’s access door open.
2.
Open the instrument’s access door.
Warning: The ESI probe tip is sharp. To avoid puncture wounds,
handle the ESI probe with care.
3.
3-2
Remove the protective sleeve, if fitted, from the ESI probe tip.
ESI and ESCi Modes of Operation
4.
Ensure that the contacts on the ESI probe align with the probe adjuster
assembly contacts, and carefully slide the ESI probe into the hole in the
probe adjuster assembly.
ESI probe
Probe adjuster assembly
Probe adjuster
assembly contacts
TP02632
5.
Secure the ESI probe by tightening the 2 thumbscrews.
Installing the ESI probe
3-3
ESI probe mounted on the source enclosure, showing the connections
to the front panel
Vernier probe adjuster
Thumbscrew
Nebulizer gas connection
Diverter valve
Desolvation gas connection
ESI probe
electrical lead
Probe adjuster
assembly
electrical lead
Probe adjuster assembly
3-4
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.
ESI and ESCi Modes of Operation
Warning: To avoid electric shock, do not use stainless steel
tubing to connect the diverter valve to the ESI probe; use the
PEEK™ tubing supplied with the instrument.
9.
Using tubing greater than or equal to 0.004-inch (ID), connect the
diverter valve to the ESI probe.
Tip: Two tubes of different ID are supplied with the instrument.
Requirement: If you are replacing the tubing supplied with the
instrument, you must minimize the length of the tube connecting the
diverter valve to the ESI probe. Doing so minimizes delays and
dispersion.
10. Close the instrument’s access door.
Installing the corona pin
Required materials:
•
Chemical-resistant, powder-free gloves
•
Needle-nose pliers
To install the corona pin
Warning: The HPLC system connections, ESI probe, and source
can be contaminated with biohazardous and/or toxic materials.
Always wear chemical-resistant, powder-free gloves while
performing this procedure.
Warning: To avoid electric shock, ensure that the instrument is in
Standby mode when commencing this procedure.
1.
In the console, click Standby
indicator is not illuminated.
, and confirm that the Operate
Warning: The source can be hot. To avoid burn injuries, take
great care while working with the instrument’s access door open.
Installing the corona pin
3-5
2.
Open the instrument’s access door.
Warning: The probe tip is sharp. To avoid puncture wounds, take
great care while working with the source enclosure door open if
an ESI probe is fitted.
Caution: Do not apply any downward force to the source
enclosure door while the door is open.
3.
Unlatch the source enclosure door’s handle by pulling it upward to the
horizontal position and then rotating it 90 degrees clockwise, and then
open the door.
4.
Use the needle-nose pliers to remove the blanking plug from the corona
pin mounting contact. Store the blanking plug in a safe location.
Corona pin mounting contact
Corona pin mounting
contact blanking plug
TP02660
3-6
ESI and ESCi Modes of Operation
Warning: The corona pin tip is sharp. To avoid puncture wounds,
handle the corona pin with care.
Caution: To avoid damaging to the corona pin’s tip and bending
the pin, use the needle-nose pliers to grip the corona pin at the
end that fits into the mounting contact.
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 orifice.
Corona pin
ESI probe tip
Corona pin
Sample cone tip
TP02695
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 “ESI probe mounted on the source enclosure,
showing the connections to the front panel” on page 3-4.)
7.
Close the source enclosure door and fasten the handle by rotating it 90
degrees counterclockwise to the vertical position and then pushing it
downward.
8.
Close the instrument’s access door.
Installing the corona pin
3-7
Optimizing the ESI probe for ESCi operation
Required material: 80:20 acetonitrile/water
To optimize the ESI probe for ESCi operation
1.
In the console, click 3100 Detector, and then click Tune
.
2.
In the Tune window, click Setup > Inter-scan Setup.
3.
In the Inter-scan Setup dialog box, click Reset to Defaults.
4.
Click OK.
5.
In the Tune window, click Ion Mode > ESCi+.
6.
Select box numbers 1 and 2, clear box numbers 3 and 4 (above the peak
display).
7.
In row 1, set Ion Mode to ES.
8.
In row 2, set Ion Mode to APCI.
9.
In each row, set Mass to 42 and Span to 5.
10. Start an infusion of 80:20 acetonitrile/water.
11. Use the vernier probe adjuster to ensure that the ESI probe tip is
pointing approximately midway between the tips of the sample cone and
corona pin.
12. In the Tune window, observe the 42 Da peak in the ES+ and APCI+ peak
displays, and increase the values of Capillary (kV) and Corona [(µA) in
the current mode or kV in the voltage mode] to produce the most intense
ESI+ and APCI+ signal.
13. Use the vernier probe adjuster to gradually move the probe
bi-directionally to determine the best position for both the ESI+ and
APCI+ signals.
14. To determine whether you have discrete ionization in the ESI or APCI
mode, set the Capillary parameter to 0 kV and observe that little or no
3-8
ESI and ESCi Modes of Operation
signal remains in ESI mode. Then set the Corona parameter to 0 µA or
0 kV, and observe that little or no signal remains in APCI mode.
Result: The ESI probe is now optimized for ESCi mode.
Tip: If necessary, repeat the above procedure using the analyte of
interest, because ionization potentials can vary with different samples.
Removing the corona pin
Required materials:
•
Chemical-resistant, powder-free gloves
•
Needle-nose pliers
To remove the corona pin
Warning: The HPLC system connections, corona pin, ESI probe,
and source can be contaminated with biohazardous and/or toxic
materials. Always wear chemical-resistant, powder-free gloves
while performing this procedure.
Warning: To avoid electric shock, ensure that the instrument is in
Standby mode when commencing this procedure.
1.
In the console, click Standby
indicator is not illuminated.
, and confirm that the Operate
Warning: The source can be hot. To avoid burn injuries, take
great care while working with the instrument’s access door open.
2.
Open the instrument’s access door.
Removing the corona pin
3-9
Warning: The probe tip is sharp. To avoid puncture wounds, take
great care while working with the source enclosure door open if
an ESI probe is fitted.
Caution: Do not apply any downward force to the source
enclosure door while the door is open.
3.
Unlatch the source enclosure door’s handle by pulling it upward to the
horizontal position and then rotating it 90 degrees clockwise, and then
open the door.
Warning: The corona pin tip is sharp. To avoid puncture wounds,
handle the corona pin with care.
Caution: To avoid damaging to the corona pin’s tip and bending
the pin, use the needle-nose pliers to grip the corona pin at the
end that fits into the mounting contact.
3-10
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 “Corona
pin” on page 3-7.)
5.
Use the needle-nose pliers to fit the blanking plug to the corona pin
mounting contact. (See the figure “Corona pin mounting contact” on
page 3-6.)
6.
Close the source enclosure door and fasten the handle by rotating it 90
degrees counterclockwise to the vertical position and then pushing it
downward.
7.
Close the instrument’s access door.
ESI and ESCi Modes of Operation
Removing the ESI probe
Required material: Chemical-resistant, powder-free gloves
To remove the ESI probe
Warning: The HPLC system connections, ESI probe, and source
can be contaminated with biohazardous and/or toxic materials.
Always wear chemical-resistant, powder-free gloves while
performing this procedure.
Warning: To avoid electric shock, ensure that the instrument is
suitably prepared before commencing this procedure.
1.
Prepare the instrument for working on the source. See “Preparing the
instrument for working on the source” on page 5-6.
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.
2.
Open the instrument’s access door.
3.
Disconnect the diverter valve tubing from the ESI probe.
4.
Disconnect the ESI probe’s electrical lead from the high voltage
connection.
5.
Ensure that the API gas is turned off.
6.
Disconnect the ESI probe’s PTFE tube from the nebulizer gas
connection.
7.
Undo the 2 thumbscrews securing the ESI probe to the probe adjuster
assembly.
Warning: The ESI probe tip is sharp. To avoid puncture wounds,
handle the probe with care.
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.
Removing the ESI probe
3-11
3-12
ESI and ESCi Modes of Operation
4
Operating the Detector
This chapter is an introduction to operating your detector; it explains
these tasks:
•
Setting-up your detector.
•
Performing a sample tune.
•
Developing instrument methods.
•
Verifying the system.
Contents
Topic
Page
Setting-up the instrument
4-2
Performing a sample tune
4-6
Developing experiment methods
4-7
Verifying the system
4-10
4-1
Setting-up the instrument
The IntelliStart instrument setup calibrates the instrument and then, by
default, performs a sample tune. If calibration is unnecessary, you can
perform only a sample tune. See “Performing a sample tune” on page 4-6.
In the following example, sodium cesium iodide is used as the calibrant
solution and sulfadimethoxine is used as the tune sample.
Tips:
•
You can substitute solutions suitable for your requirements.
•
Instrument setup need only be performed every 3 to 6 months,
depending on your usage requirements.
See the detector’s online Help for further details of IntelliStart.
Requirement: If you use Empower software, your project must contain the
instrument methods supplied during installation of the detector software. See
the Empower online Help for further details on restoring projects.
Required materials:
•
Sodium cesium iodide solution (2 ng/µL)
•
Sulfadimethoxine solution (100 pg/µL)
To prepare the IntelliStart fluidics system
Requirement: Ensure that there is enough solution in each reservoir for
approximately 5 minutes of operation after purging the reservoirs.
Recommendation: In general, place calibrant solution in reservoir A and
sample solution in reservoir B.
1.
Ensure that IntelliStart fluidics system’s reservoir A is filled with
sodium cesium iodide solution.
2.
Ensure that reservoir B is filled with sulfadimethoxine solution.
3.
Launch the console using one of the following methods.
4.
4-2
•
MassLynx – In the MassLynx main window, click MS Console.
•
Empower – In the Run Samples window, right-click the detector’s
control panel, and then click Launch Instrument Console.
In the console system tree, expand 3100 Detector.
Operating the Detector
5.
If you use MassLynx software, click Interactive Display; otherwise click
Interactive Fluidics.
6.
If the calibration reservoir is selected, click
to purge the system.
Tip: System purge takes approximately 2 minutes.
7.
If the sample reservoir is selected, click on the reservoir display and in
the Select Reservoir dialog box, select the calibration reservoir.
8.
Click OK.
Result: The calibration reservoir is selected, and the system is purged.
To specify the instrument set-up parameters
1.
In the console system tree, click 3100 Detector.
2.
Ensure that Ion Mode is ES+.
3.
Click IntelliStart.
4.
Ensure that Instrument Setup is selected.
5.
If you require system pre-checking, select Pre-checks.
Rationale: If Pre-checks is selected, when IntelliStart starts the
instrument setup, it determines whether the existing calibration is still
valid. If so, it does not perform a full calibration but proceeds to sample
tuning the instrument.
For further details, see the detector’s online Help topic “IntelliStart flow
diagram”.
6.
Click Start
to open the IntelliStart Setup Parameters dialog box.
7.
In the Instrument Setup tab’s Reference list, click Naics.
Rationale: Naics is the calibration reference for sodium cesium iodide
when working in ES+ ion mode.
Setting-up the instrument
4-3
8.
If you use MassLynx software, click “Fill from reference file”; otherwise,
click “Get Reference Masses”.
Result: The default mass values appear in the Instrument Tune Masses
text boxes.
Rule: You must click “Fill from reference file” or “Get Reference Masses”
to obtain the masses from the reference each time you select a new
calibration reference.
Tip: You can use alternative reference solutions to calibrate at different
masses.
9.
The tune and calibration results are saved with the names specified. You
can use the default names or enter your own.
To specify the sample tune parameters using MassLynx software
This procedure applies only if you are using MassLynx software. If you are
using Empower software, see “To specify the sample tune parameters using
Empower software” on page 4-4.
1.
In the IntelliStart Setup Parameters dialog box, click the Sample Tune
tab.
2.
For the first sample tune mass, select the check box and enter a value of
311.
3.
Clear all the check boxes for other sample tune masses.
4.
In the Tune text box, enter sulfadimethoxine.ipr.
Rationale: The sample tune results are written to this file.
To specify the sample tune parameters using Empower software
This procedure applies only if you are using Empower software. If you are
using MassLynx software, see “To specify the sample tune parameters using
MassLynx software” on page 4-4.
4-4
1.
In the IntelliStart Setup Parameters dialog box, click the Sample Tune
tab.
2.
For the first sample tune mass, select the check box and enter a value of
311.
Operating the Detector
3.
Clear all the check boxes for other sample tune masses.
4.
In the Save Sample Tune Parameters As box, enter sulfadimethoxine.
To start instrument setup
1.
Click Start.
Result: A message appears reminding you to ensure that the calibrant
solutions, calibration parameters, and LC flow are set correctly.
2.
Click OK.
Result: An autotune on the calibrant is followed by automatic
calibration. The console displays the progress of the setup.
Example display during calibration
IntelliStart creates tune and calibration settings, which are saved as
specified on the Instrument Setup Parameters dialog box’s Instrument
Setup tab. Once calibration is complete, the sample tune starts on the
mass defined in the IntelliStart Setup Parameters dialog box. When the
sample tune is complete, the sample tune results are saved with the
name sulfadimethoxine.
Setting-up the instrument
4-5
Performing a sample tune
In the following example, sulfadimethoxine is used as the tuning sample.
Required material: Sulfadimethoxine solution (100 pg/µL)
To perform a sample tune
1.
Prepare the IntelliStart fluidics system with sulfadimethoxine solution
in reservoir B. See “To prepare the IntelliStart fluidics system” on
page 4-2.
2.
In the console system tree, click 3100 Detector.
3.
Ensure that the Ion Mode is ES+.
4.
Click IntelliStart.
5.
Clear the Instrument Setup check box.
6.
If you require system pre-checking, select Pre-checks.
Rationale: If Pre-checks is selected, when IntelliStart starts the sample
tune, it determines whether the existing tune is still valid. If so, no
sample tune is performed.
See the detector’s online Help topic “IntelliStart flow diagram”.
7.
Click Start.
8.
In the IntelliStart Setup Parameters dialog box’s Sample Tune tab,
specify the sample tune parameters as described for your data system in
“To specify the sample tune parameters using MassLynx software” on
page 4-4 or “To specify the sample tune parameters using Empower
software” on page 4-4.
9.
Click Start.
Result: A message appears reminding you to ensure that the tune
solutions, tune parameters, and LC flow are set correctly.
10. Click OK.
Result: The console displays the progress of the setup. When the sample
tune is complete, the sample tune results are saved with the name
sulfadimethoxine.
4-6
Operating the Detector
Developing experiment methods
IntelliStart enables you to automatically develop quantitative SIR methods
for compounds of interest. Up to four compounds can be handled in a single
process. In this example, a method for sulfadimethoxine is created.
Required material: Sulfadimethoxine solution (100 pg/µL)
To create a method
1.
Prepare the IntelliStart fluidics system with sulfadimethoxine solution
in reservoir B. See “To prepare the IntelliStart fluidics system” on
page 4-2.
2.
In the console system tree, click 3100 Detector.
3.
Ensure that the Ion Mode is ES+.
4.
Click IntelliStart.
5.
Clear the Instrument Setup check box.
6.
Click Develop Method.
7.
If you require system pre-checking, select Pre-checks. See the detector’s
online Help topic “IntelliStart flow diagram”.
8.
Click Start.
9.
In the IntelliStart Setup Parameters dialog box, click the Method
Developer tab if you use MassLynx software, or the Develop Method tab
if you use Empower software.
Rule: The masses, tune parameters, and IntelliStart fluidics system
parameters already set in IntelliStart are used.
10. Select the parameters shown in the following figures.
Developing experiment methods
4-7
Method Developer tab (MassLynx)
4-8
Operating the Detector
Develop Method tab (Empower)
In this case, a method called sulfadimethoxine is created.
In MassLynx software, the validation pane selections save optimization
data for validation purposes and create an autotune report file
(Sulfadimethoxine.xml). In Empower software, an autotune report file is
printed.
For further information on the parameters available in the Develop
Method tab, see the detector’s online Help.
11. Click Start.
Result: A message appears reminding you to ensure that the sample
solutions, sample tune parameters, and LC flow are set correctly.
Developing experiment methods
4-9
12. Click OK.
Result: The console displays the progress of the method development.
When the method development is complete, the method settings are
saved with the name sulfadimethoxine.
A green check mark indicates a successful run; a red cross indicates a
failure.
Verifying the system
Using IntelliStart, you can verify that your system is performing to an
acceptable standard. You can run the system verification in one of the
following three ways:
•
Manually from the console.
•
Manually as part of an autotune sequence.
•
If you use MassLynx, automatically on a scheduled time and date.
For instructions on preparing a sulfadimethoxine standard for use with the
supplied LC/MS System Check projects, see “Preparing Samples for LC/MS
System Check with Empower software” on page D-1.
For detailed information on setting up system verification, see the detector’s
online Help.
4-10
Operating the Detector
5
Maintenance Procedures
This chapter provides the maintenance guidelines and procedures
necessary to maintain the instrument’s performance.
Keep to a maintenance schedule, and perform maintenance as required
and described in this chapter.
Contents
Topic
Page
Maintenance schedule
5-3
Spare parts
5-5
Safety and handling
5-5
Preparing the instrument for working on the source
5-6
Operating the source isolation valve
5-7
Removing O-rings and seals
5-9
Cleaning the instrument case
5-10
Cleaning the source cleanout tray
5-10
Emptying the instrument exhaust trap bottle
5-15
Emptying the roughing pump exhaust liquid trap bottle
5-16
Gas ballasting the roughing pump
5-20
Checking the roughing pump oil level
5-23
Adding oil to the roughing pump
5-23
Cleaning the source components
5-25
Cleaning the sample cone and gas cone
5-25
Cleaning the ion block, isolation valve, and extraction cone
5-35
Cleaning the source hexapole assembly
5-51
Replacing the ESI probe tip
5-57
Replacing the ESI probe sample capillary
5-58
Cleaning the IonSABRE APCI probe tip
5-65
Replacing the IonSABRE APCI probe sample capillary
5-65
5-1
Contents
5-2
Topic
Page
Cleaning or replacing the corona pin
5-73
Replacing the APCI probe heater
5-74
Replacing the ion block source heater
5-77
Replacing the source assembly seals
5-81
Maintaining the detector air filters
5-91
Replacing the roughing pump oil
5-98
Replacing the roughing pump’s oil demister element
5-101
Maintenance Procedures
Maintenance schedule
The following table lists periodic maintenance schedules that ensure optimum
instrument performance.
The maintenance frequencies shown apply to instruments that normally
receive moderate use.
Maintenance schedule
Procedure
Frequency
For information...
Clean the instrument case.
As required.
See page 5-10.
Clean the source cleanout
tray.
Check daily, clean
when excessively
fouled.
See page 5-10.
Empty the exhaust trap bottle Check daily, empty as
in the instrument exhaust
required.
line.
See page 5-15.
Empty the liquid trap bottle
Check daily, empty as
in the roughing pump exhaust required.
line.
See page 5-16.
Gas ballast the roughing
pump.
ESI – weekly;
APCI – daily.
See page 5-20.
Inspect and adjust the
roughing pump oil level.
Weekly.
See page 5-23.
Clean the source components. When sensitivity
decreases to
unacceptable levels.
See page 5-25.
Clean or replace the ESI
probe tip.
When sensitivity
decreases to
unacceptable levels.
See page 5-57.
Replace the ESI probe
capillary.
When sensitivity
decreases to
unacceptable levels or
sample flow is
inconsistent.
See page 5-58.
Maintenance schedule
5-3
Maintenance schedule
5-4
Procedure
Frequency
For information...
Clean the APCI probe tip.
(Options using the APCI
IonSABRE probe only.)
When sensitivity
decreases to
unacceptable levels.
See page 5-65.
Replace the APCI probe
capillary.
When sensitivity
decreases to
unacceptable levels or
sample flow is
inconsistent.
See page 5-65.
Clean or replace the corona
pin (APCI and ESCi modes).
When the corona pin is See page 5-73.
corroded or black, or
the sensitivity
decreases to
unacceptable levels.
Replace the APCI probe
heater.
If the heater fails when See page 5-74.
the instrument is
pumped down
(evacuated).
Replace the ion block heater
cartridge.
If the heater fails to
heat when the
instrument is pumped
down (evacuated).
See page 5-77.
Replace the source assembly
seals.
Annually.
See page 5-81.
Clean or replace the
instrument’s air filters.
Annually.
See page 5-91.
Change the roughing pump
oil.
Annually.
See page 5-98.
Replace the roughing pump’s
demister element.
Annually.
Tip: Applications that
contaminate the
roughing pump oil
reduce this period,
which must be
determined from
experience.
See page 5-101.
Maintenance Procedures
Spare parts
Waters recommends that you replace only the parts mentioned in this
document. For spare parts details, see the Waters Quality Parts Locator on
the Waters Web site’s Services/Support page.
Safety and handling
Bear in mind the following safety considerations when performing
maintenance procedures:
Warning: The instrument components can be contaminated with
biologically hazardous materials. Always wear
chemical-resistant, powder-free gloves while handling the
components.
Warning: To prevent injury, always observe Good Laboratory Practices
when handling solvents, changing tubing, or operating the instrument.
Know the physical and chemical properties of the solvents used (see
the Material Safety Data Sheets for the solvents in use).
Warning: To avoid electric shock,
• do not remove the instrument’s panels. There are no
user-serviceable items inside the instrument.
• ensure that the instrument is in Standby mode before commencing
any maintenance.
Warning: The probe and source can be hot. To avoid burn injuries, take
great care while working with these components.
Caution: When performing maintenance inside the source enclosure,
ensure that the following criteria are met:
• Instrument is in Standby mode.
• LC flow is diverted to waste or set to off.
• Desolvation gas is turned off.
See Appendix A for safety advisory information.
Spare parts
5-5
Preparing the instrument for working on the source
For safety reasons, you must follow the procedure described below before
working on the source (for example, when changing the probe, installing or
removing the corona pin, operating the source isolation valve, and when
maintaining the source).
To prepare the instrument for working on the source
1.
In the console, click Standby
indicator is not illuminated.
, and confirm that the Operate
Requirement: Before you continue, stop the LC flow or divert it to waste.
2.
5-6
In the 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 console system tree, expand 3100 Detector.
b.
Click Show Tune
c.
In the Tune window, click the Fluidics tab.
d.
In the Flow Control panel, select Waste as the flow state.
.
3.
Wait 3 minutes to allow the desolvation gas flow to cool the probe and
source.
4.
In the console, click API
Maintenance Procedures
to stop the desolvation gas flow.
Operating the source isolation valve
You must close the source isolation valve to isolate the source from the
instrument vacuum system for certain maintenance procedures.
Required material: Chemical-resistant, powder-free gloves
To close the source isolation valve before starting a maintenance procedure
Warning: The source components can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
Warning: To avoid electric shock, ensure that the instrument is
suitably prepared before commencing this procedure.
1.
Prepare the instrument for working on the source. See “Preparing the
instrument for working on the source” on page 5-6.
Warning: The source can be hot. To avoid burn injuries, take
great care while working with the instrument’s access door open.
2.
Open the instrument’s access door.
Warning: To avoid puncture wounds, take great care while
working with the source enclosure door open if one or both of
these conditions apply:
• An ESI probe is fitted (the probe tip is sharp).
• A corona pin is fitted (the pin tip is sharp).
Caution: Do not apply any downward force to the source
enclosure door while the door is open.
3.
Unfasten the source enclosure door’s handle and open the door.
Operating the source isolation valve
5-7
4.
Close the source isolation valve by moving its handle counterclockwise,
to the vertical position.
Isolation valve handle in closed position
TP02635
To open the source isolation valve after completing a maintenance
procedure
Warning: The source components can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
Warning: To avoid puncture wounds, take great care while working
with the source enclosure door open if one or both of these conditions
apply:
• An ESI probe is fitted (the probe tip is sharp).
• A corona pin is fitted (the pin tip is sharp).
Caution: Do not apply any downward force to the source enclosure door
while the door is open.
1.
5-8
Open the source isolation valve by moving its handle clockwise to the
horizontal position.
Maintenance Procedures
2.
Close the source enclosure door and fasten the handle by rotating it 90
degrees counterclockwise to the vertical position and then pushing it
downward.
3.
Close the instrument’s access door.
Removing O-rings and seals
When performing certain maintenance procedures, you must remove O-rings
or seals from instrument components. An O-ring removal kit is provided with
the instrument. You must dispose of all used O-rings and seals; do not re-use
old O-rings or seals on the instrument.
O-ring removal kit
Tool 1
Tool 2
To remove an O-ring
Caution: When removing an O-ring or seal from a component, be
careful not to scratch the component with either removal tool.
1.
Use the forked end of tool 1 to impale the O-ring or seal.
Removing O-rings and seals
5-9
2.
Pull the O-ring or seal from its groove; if necessary, use tool 2 as an aid.
Warning: The O-ring or seal can be contaminated with
biohazardous and/or toxic materials. Ensure that it is
correctly disposed of according to local environmental
regulations.
3.
Dispose of the O-ring or seal in accordance with local environmental
regulations.
Cleaning the instrument case
Caution: Do not use abrasives or solvents to clean the instrument’s
case.
Use a soft cloth, dampened with water, to clean the outside surfaces of the
detector.
Cleaning the source cleanout tray
The source cleanout tray minimizes the buildup of contaminants on the floor
of the source. The tray can easily be removed for cleaning; check it daily and
clean it when it is excessively fouled.
Source cleanout tray
Cleanout tray handle
5-10
Maintenance Procedures
Removing the source cleanout tray from the source
Required material: Chemical-resistant, powder-free gloves
To remove the source cleanout tray
Warning: The source components can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
Warning: To avoid electric shock, ensure that the instrument is
suitably prepared before commencing this procedure.
1.
Prepare the instrument for working on the source. See “Preparing the
instrument for working on the source” on page 5-6.
Warning: The source can be hot. To avoid burn injuries, take
great care while working with the instrument’s access door open.
2.
Open the instrument’s access door.
Warning: To avoid puncture wounds, take great care while
working with the source enclosure door open if one or both of
these conditions apply:
• An ESI probe is fitted (the probe tip is sharp).
• A corona pin is fitted (the pin tip is sharp).
Caution: Do not apply any downward force to the source
enclosure door while the door is open.
3.
Unfasten the source enclosure door’s handle and open the door.
4.
Disconnect the PTFE tube from the cone gas assembly connection tube.
5.
Grasp the cleanout tray handle and carefully maneuver the cleanout
tray out of the source.
Cleaning the source cleanout tray
5-11
Source cleanout tray in position in the source
Cone gas
connection tube
Cleanout tray
handle
PTFE tube
TP02732
Cleaning the source cleanout tray
Required materials:
5-12
•
Chemical-resistant, powder-free gloves
•
Appropriately sized glass vessel in which to completely immerse the
source cleanout tray
•
HPLC-grade (or better) methanol
•
HPLC-grade (or better) water
•
Formic acid
•
Ultrasonic bath
•
Source of oil-free, inert gas (nitrogen or helium) for drying (air-drying
optional)
•
Wash-bottle containing HPLC-grade (or better) 1:1 methanol/water
•
Large beaker
Maintenance Procedures
To clean the source cleanout tray
Warning: The source cleanout tray can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
Warning: Use extreme care when working with formic acid. Work in a
fume hood, and use suitable protective equipment.
1.
Immerse the source cleanout tray in a glass vessel containing 1:1
methanol/water.
Tip: If the source cleanout tray is heavily contaminated, use 45:45:10
methanol/water/formic acid.
2.
Place the vessel in the ultrasonic bath for 30 minutes.
3.
If you used formic acid in the cleaning solution do as follows:
a.
Rinse the source cleanout tray by immersing it in a glass vessel
containing water and then placing the vessel in the ultrasonic bath
for 20 minutes.
b.
Displace the water by immersing the source cleanout tray in a glass
vessel containing methanol and then placing the vessel in the
ultrasonic bath for 10 minutes.
Caution: To avoid recontaminating the source cleanout tray,
wear clean, chemical-resistant, powder-free gloves for the rest of
this procedure.
4.
Carefully remove the source cleanout tray from the vessel, and blow-dry
with inert, oil-free gas.
Cleaning the source cleanout tray
5-13
Refitting the source cleanout tray to the source
Required material: Chemical-resistant, powder-free gloves
To refit the source cleanout tray
Warning: The source components can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
Warning: The source can be hot. To avoid burn injuries, take great care
while working with the instrument’s access door open.
Warning: To avoid puncture wounds, take great care while working
with the source enclosure door open if one or both of these conditions
apply:
• An ESI probe is fitted (the probe tip is sharp).
• A corona pin is fitted (the pin tip is sharp).
Caution: Do not apply any downward force to the source enclosure door
while the door is open.
5-14
1.
Grasp the cleanout tray handle and carefully maneuver the cleanout
tray into the source.
2.
Connect the PTFE tube to the cone gas assembly connection tube.
3.
Close the source enclosure door and fasten the handle by rotating it 90
degrees counterclockwise to the vertical position and then pushing it
downward.
4.
Close the instrument’s access door.
Maintenance Procedures
Emptying the instrument exhaust trap bottle
Check the exhaust trap bottle in the instrument exhaust line daily and empty
it before it is completely full.
Instrument exhaust trap bottle
To laboratory
exhaust port
(10-mm OD)
From instrument
exhaust connection
(12-mm OD)
Required materials:
•
Chemical-resistant, powder-free gloves
•
snoop (or equivalent) leak detector liquid
®
To empty the exhaust trap bottle
1.
In the console, click Stop Flow
to stop the LC flow.
Emptying the instrument exhaust trap bottle
5-15
2.
In the console, click API
to stop the desolvation gas flow.
Warning: The waste liquid in the exhaust trap bottle
comprises LC solvents and analytes. Always wear
chemical-resistant, powder-free gloves while handling the
exhaust trap bottle.
3.
Unscrew and remove the exhaust trap bottle cap.
Warning: The waste liquid can be contaminated with
biohazardous and/or toxic materials. Ensure that it is
correctly disposed of according to local environmental
regulations.
4.
Dispose of the waste liquid in accordance with local environmental
regulations.
5.
Fit and tighten the exhaust trap bottle cap.
6.
Ensure that the exhaust trap bottle is secured in the upright position.
7.
In the console, click API
8.
In the console, click Start Flow
to start the desolvation gas flow.
to start the LC flow.
Warning: To confirm the integrity of the source exhaust
system, the following leak test must be performed.
Caution: To avoid damage to the instrument, snoop (or
equivalent) leak detector liquid must be used only for the
purpose described in the following step; it must not be used on
any other part of the instrument.
9.
Use snoop (or equivalent) leak detector liquid to ensure that there are no
leaks at the exhaust trap bottle cap.
Emptying the roughing pump exhaust liquid trap bottle
Check the liquid trap bottle in the roughing pump exhaust line daily and
empty it before it is completely full.
5-16
Maintenance Procedures
Roughing pump exhaust liquid trap bottle for an oil-filled roughing pump
TP02800
Emptying the roughing pump exhaust liquid trap bottle
5-17
Roughing pump exhaust liquid trap bottle for an oil-free roughing pump
TP02997
TP02800
TP02996
Required materials:
5-18
•
Chemical-resistant, powder-free gloves
•
snoop (or equivalent) leak detector liquid
Maintenance Procedures
To empty the exhaust liquid trap bottle
1.
Close the source isolation valve. See “Operating the source isolation
valve” on page 5-7.
Warning: The liquid in the roughing pump liquid trap
bottle can be contaminated with analyte accumulated
during normal operation. Always wear chemical-resistant,
powder-free gloves while handling the bottle.
Warning: To avoid burn injuries, take great care while working
near the roughing pump: it can be hot.
2.
Unscrew and remove the roughing pump liquid trap bottle cap.
Warning: The waste liquid can be contaminated with
biohazardous and/or toxic materials. Ensure that it is
correctly disposed of according to local environmental
regulations.
3.
Dispose of the waste liquid in accordance with local environmental
regulations.
4.
Fit and tighten the roughing pump liquid trap bottle cap.
5.
Ensure that the roughing pump liquid trap bottle is secured in the
upright position.
6.
Open the source isolation valve. See “Operating the source isolation
valve” on page 5-7.
Caution: To avoid damage to the instrument, snoop (or
equivalent) leak detector liquid must be used only for the
purpose described in the following step; it must not be used on
any other part of the instrument.
7.
Use snoop (or equivalent) leak detector liquid to ensure that there are no
leaks at the liquid trap bottle cap.
Emptying the roughing pump exhaust liquid trap bottle
5-19
Gas ballasting the roughing pump
Note: This procedure is not required for an Alcatel oil-free roughing pump.
Roughing pump
Exhaust port flange
Oil filler plug
Oil-level sight glass
TP02689
Drain plug
Gas ballast valve
Caution: Failure to routinely gas ballast the roughing pump shortens
oil life and, consequently, pump life.
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:
5-20
•
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.
Maintenance Procedures
Your roughing pump can be fitted with either of the following:
•
A screwdriver-operated gas ballast valve. See “Gas ballasting a pump
fitted with a screwdriver-operated gas ballast valve” on page 5-21.
•
A handle-operated gas ballast valve. See “Gas ballasting a pump fitted
with a handle-operated gas ballast valve” on page 5-22.
Gas ballasting a pump fitted with a screwdriver-operated gas
ballast valve
Required material: Flat-blade screwdriver
To gas ballast the roughing pump
Warning: To avoid burn injuries, take great care while working with
the roughing pump: it can be hot.
Caution: To avoid damage,
• do not vent the instrument when the roughing pump is gas
ballasting.
• do not gas ballast the roughing pump while the detector is in
Operate mode.
• avoid gas ballasting the roughing pump for more than 2 hours.
1.
Use the flat-blade screwdriver to turn the gas ballast valve on the pump
a quarter-turn to the open,
, position.
TP02654
Gas ballasting the roughing pump
5-21
2.
Run the pump for 30 to 60 minutes.
Tip: It is normal for the roughing pump temperature to increase during
ballasting. To maintain an ambient temperature of <40 C (104 F)
where the pump is located, ensure there is adequate ventilation.
3.
Use the flat-blade screwdriver to turn the gas ballast valve to the closed,
, position.
Gas ballasting a pump fitted with a handle-operated gas ballast
valve
To gas ballast the roughing pump
Warning: To avoid burn injuries, take great care while working with
the roughing pump: it can be hot.
Caution: To avoid damage,
• do not vent the instrument when the roughing pump is gas
ballasting.
• do not gas ballast the roughing pump while the detector is in
Operate mode.
• avoid gas ballasting the roughing pump for more than 2 hours.
1.
Move the gas ballast valve handle on the pump a counterclockwise from
the horizontal position to the vertical position.
TP02654
5-22
Maintenance Procedures
2.
Run the pump for 30 to 60 minutes.
Tip: It is normal for the roughing pump temperature to increase during
ballasting. To maintain an ambient temperature of <40 C (104 F)
where the pump is located, ensure there is adequate ventilation.
3.
Move the gas ballast valve handle on the pump clockwise from the
vertical position to the horizontal position.
Checking the roughing pump oil level
Caution: To ensure correct operation of the roughing pump, do not
operate the pump with the oil level at less than 30% of the MAX level.
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 5-20 and “Adding oil to the roughing pump”
on page 5-23.
Adding oil to the roughing pump
If you check the roughing pump oil level and it is found to be low, you must
add oil to the roughing pump. See “Checking the roughing pump oil level” on
page 5-23.
Required materials:
•
Chemical-resistant, powder-free gloves
•
8-mm Allen wrench
•
Container to catch used oil
•
Funnel
•
Anderol vacuum oil, type GS 495
Checking the roughing pump oil level
5-23
To add oil to the roughing pump
1.
Vent and shut-down the detector. See “Shutting down the detector” on
page 2-12 for more details.
Warning: The pump oil can be contaminated with analyte
accumulated during normal operation. Always wear
chemical-resistant, powder-free gloves when adding or
replacing oil.
Warning: To avoid burn injuries, take great care while working
with the roughing pump: it can be hot.
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 5-20.
Caution: To maintain pump performance, use only Anderol
vacuum oil, type GS 495.
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 detector. See “Starting the detector” on page 2-2.
Tips: After you add oil to the pump, the following situations can occur:
5-24
•
The oil level drops slightly during the first month of operation.
•
The oil changes color (darkens) over time.
Maintenance Procedures
•
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.
Cleaning the source components
Clean the sample cone and gas cone when these conditions apply:
•
The sample cone and gas cone are visibly fouled.
•
LC and sample-related causes for decreased signal intensity have been
dismissed.
See “Cleaning the sample cone and gas cone” on page 5-25.
If cleaning the sample cone and gas cones fails to increase signal sensitivity,
also clean the ion block, isolation valve, and extraction cone. See “Cleaning the
ion block, isolation valve, and extraction cone” on page 5-35.
If cleaning the ion block, isolation valve, and extraction cone fails to increase
signal sensitivity, also clean the source hexapole assembly. See “Cleaning the
source hexapole assembly” on page 5-51.
Cleaning the sample cone and gas cone
The cone gas assembly (comprising the sample cone, O-ring, and gas cone) can
be removed for cleaning without venting the instrument.
Removing the cone gas assembly from the source
Required material: Chemical-resistant, powder-free gloves
Cleaning the source components
5-25
To remove the cone gas assembly from the source
Warning: The source components can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
Warning: To avoid electric shock, ensure that the instrument is in
Standby mode before commencing this procedure.
Warning: To avoid puncture wounds, take great care while working
with the source enclosure door open if one or both of these conditions
apply:
• An ESI probe is fitted (the probe tip is sharp).
• A corona pin is fitted (the pin tip is sharp).
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 5-7.
2.
Disconnect the PTFE tube from the cone gas assembly connection tube.
Cone gas assembly
Connection tube
PTFE tube
TP02644
5-26
Maintenance Procedures
3.
Grasp the cone gas assembly connection tube, and use it as a lever to
rotate the cone gas assembly 90 degrees, moving the connection tube
from the vertical to the horizontal position.
Cone gas assembly
rotated 90 degrees
TP02643
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.
Ion block assembly
TP02642
Cleaning the sample cone and gas cone
5-27
Disassembling the cone gas assembly
Required material: Chemical-resistant, powder-free gloves
To disassemble the cone gas assembly
Warning: The cone gas assembly can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
Caution: Do not apply excessive force to the source enclosure door
when using the extraction tool on the source door.
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.
Cone gas assembly
Extraction tool
Source enclosure
door
TP02641
5-28
Maintenance Procedures
Caution: The sample cone is fragile. Never place it on its tip;
always place it on its flanged base.
2.
Carefully push down on the gas cone to separate the gas cone, sample
cone, and O-ring.
O-ring
Sample cone
Gas cone
TP02645
Warning: The O-ring can be contaminated with
biohazardous and/or toxic materials. Ensure that it is
correctly disposed of according to local environmental
regulations.
3.
Dispose of the O-ring in accordance with local environmental
regulations.
Cleaning the sample cone and gas cone
Required materials:
•
Chemical-resistant, powder-free gloves.
•
Appropriately sized glass vessels in which to completely immerse
components when cleaning. Use only glassware not previously cleaned
with surfactants.
•
HPLC-grade (or better) methanol.
•
HPLC-grade (or better) water.
Cleaning the sample cone and gas cone
5-29
•
Formic acid.
•
Ultrasonic bath.
•
Source of oil-free, inert gas (nitrogen or helium) for drying (air-drying
optional).
•
Wash-bottle containing HPLC-grade (or better) 1:1 methanol/water.
•
Large beaker.
To clean the sample cone and gas cone
Warning: The sample cone and gas cone can be contaminated
with biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
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.
5-30
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.
Maintenance Procedures
Caution: To avoid recontaminating the components, wear clean,
chemical-resistant, powder-free gloves for the rest of this
procedure.
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:
7.
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.
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.
Cleaning the sample cone and gas cone
5-31
Assembling the cone gas assembly
Required material: Chemical-resistant, powder-free gloves
To assemble 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.
1.
Carefully fit the sample cone into the gas cone.
O-ring
Sample cone
Gas cone
TP02663
2.
5-32
Fit a new O-ring into the groove created between the sample cone and
gas cone.
Maintenance Procedures
Fitting the cone gas assembly to the source
Required material: Chemical-resistant, powder-free gloves
To fit the cone gas assembly to the source
Warning: The source components can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
Warning: To avoid puncture wounds, take great care while working
with the source enclosure door open if one or both of these conditions
apply:
• An ESI probe is fitted (the probe tip is sharp).
• A corona pin is fitted (the pin tip is sharp).
Caution: To avoid damage,
• do not apply any downward force to the source enclosure door while
the door is open.
• do not open the source isolation valve before fitting the cone gas
assembly to the ion block assembly.
1.
Ensure that the source isolation valve is in the closed position. See
“Operating the source isolation valve” on page 5-7.
Cleaning the sample cone and gas cone
5-33
2.
Hold the cone gas assembly so that the connection tube is horizontal and
at the top, then slide the cone gas assembly into the ion block assembly.
Ion block
assembly
Cone gas
assembly
TP02642
5-34
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 fasten the handle by rotating it 90
degrees counterclockwise to the vertical position and then pushing it
downward.
7.
Close the instrument’s access door.
Maintenance Procedures
Cleaning the ion block, isolation valve, and extraction
cone
The ion block and extraction cone must be cleaned if cleaning the sample cone
and gas cone fails to increase signal sensitivity.
Removing the ion block assembly from the source assembly
Required materials:
•
Chemical-resistant, powder-free gloves
•
6-mm Allen wrench
To remove the ion block assembly
Warning: The source components can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
1.
Vent and shut-down the detector. See “Shutting down the detector” on
page 2-12.
Warning: The source can be hot. To avoid burn injuries, allow it
to cool for at least 30 minutes before proceeding.
2.
Open the instrument’s access door.
Warning: To avoid puncture wounds, take great care while
working with the source enclosure door open if one or both of
these conditions apply:
• An ESI probe is fitted (the probe tip is sharp).
• A corona pin is fitted (the pin tip is sharp).
Caution: Do not apply any downward force to the source
enclosure door while the door is open.
3.
Unfasten the source enclosure door’s handle and open the door.
4.
Close the source isolation valve. See “Operating the source isolation
valve” on page 5-7.
Cleaning the ion block, isolation valve, and extraction cone
5-35
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
Ion block securing screws
TP02646
7.
Remove the ion block assembly from the PEEK ion block support.
Ion block assembly
5-36
Maintenance Procedures
Disassembling the source ion block assembly
Required materials:
•
Chemical-resistant, powder-free gloves
•
2.5-mm and 6-mm Allen wrenches
•
O-ring removal kit
•
Needle-nose pliers
To disassemble the ion block assembly
Warning: The ion block assembly can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
1.
Ensure that the isolation valve is closed.
Isolation valve handle
in closed position
Gas cone position
blocks
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
5-37
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.
Ion block cover plate securing screw
Ion block cover plate
TP02649
5.
5-38
Remove the ion block cover plate.
Maintenance Procedures
6.
Grasp the isolation valve and pull it out of the ion block.
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 5-9.
Warning: The isolation valve O-ring can be contaminated
with biohazardous and/or toxic materials. Ensure that it is
correctly disposed of according to local environmental
regulations.
8.
Dispose of the isolation valve O-ring in accordance with local
environmental regulations.
Cleaning the ion block, isolation valve, and extraction cone
5-39
9.
Use the 2.5-mm Allen wrench to loosen the captive PEEK terminal block
securing screw.
PEEK terminal block securing screw
TP02616
Caution: To avoid damaging the heater cartridge assembly
wires, do not bend or twist them either side of the heater
cartridge assembly heat-shrink tubing when removing the
assembly from the ion block.
10. Use the needle-nose pliers to grasp the PEEK terminal block and
partially lift it out of the ion block.
5-40
Maintenance Procedures
11. Holding the PEEK ion block gently, use the needle-nose pliers to gently
grasp the heat-shrink tubing on the heater cartridge assembly and slide
it and the PEEK terminal block out of the ion block.
Heat-shrink tubing
PEEK terminal block
Heater cartridge assembly
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 5-9.
Cover seal
TP02619
Cleaning the ion block, isolation valve, and extraction cone
5-41
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.
13. Dispose of the cover seal in accordance with local environmental
regulations.
14. Use the 6-mm Allen wrench to remove the ion block blanking plug and
associated seal.
Blanking plug
Seal
TP02648
Warning: The blanking plug seal can be contaminated with
biohazardous and/or toxic materials. Ensure that it is
correctly disposed of according to local environmental
regulations.
15. Dispose of the blanking plug seal in accordance with local environmental
regulations.
5-42
Maintenance Procedures
16. Use the 2.5-mm Allen wrench to loosen the captive extraction cone
retainer securing screw.
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
5-43
18. Remove the extraction cone retainer from the extraction cone.
19. Remove the extraction cone seal from the ion block.
Extraction cone seal
TP02614
Cleaning the ion block, isolation valve, and extraction cone
Required materials:
5-44
•
Chemical-resistant, powder-free gloves.
•
Appropriately sized glass vessels in which to completely immerse
components when cleaning. Use only glassware not previously cleaned
with surfactants.
•
HPLC-grade (or better) methanol.
•
HPLC-grade (or better) water.
•
Formic acid.
•
Ultrasonic bath.
•
Source of oil-free, inert gas (nitrogen or helium) for drying (air-drying
optional).
•
Wash-bottle containing HPLC-grade (or better) 1:1 methanol/water.
•
Large beaker.
Maintenance Procedures
To clean the ion block components
Warning: The ion block components can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
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.
Caution: To avoid damage, do not clean non-metal parts (for example,
the heater cartridge assembly) in this way.
Tip: If the components are obviously contaminated, use 45:45:10
methanol/water/formic acid.
2.
Place the vessels in the ultrasonic bath for 30 minutes.
3.
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 separately in
glass vessels containing methanol and then placing the vessels in
the ultrasonic bath for 10 minutes.
Caution: To avoid recontaminating the components, wear clean,
chemical-resistant, powder-free gloves for the rest of this
procedure.
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
5-45
5.
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.
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.
Assembling the source ion block assembly
Required materials:
•
Chemical-resistant, powder-free gloves
•
1.5-mm, 2.5-mm, and 6-mm Allen wrenches
•
Needle-nose pliers
•
Isopropyl alcohol in small container
To assemble 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.
1.
Fit the extraction cone seal to the ion block.
2.
Fit the extraction cone retainer to the extraction cone.
Caution: Take great care not to damage the extraction cone
aperture when fitting the extraction cone to the ion block.
5-46
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.
Maintenance Procedures
6.
Use the 6-mm Allen wrench to fit and tighten the blanking plug to the
ion block.
Caution: To avoid damaging the heater cartridge assembly
wires, do not bend or twist them either side of the heater
cartridge assembly heat-shrink tubing when fitting the assembly
to the ion block.
7.
Using the needle-nose pliers to gently grasp the heat-shrink tubing on
the heater cartridge assembly, slide the assembly and the PEEK
terminal block into the ion block.
8.
Use the 2.5-mm Allen wrench to tighten the captive PEEK terminal
block securing screw.
9.
Ensure that the grooves for the cover seal and extraction cone seal 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.
10. Fit a new cover seal to the ion block, ensuring that it is correctly seated.
11. Soak a new isolation valve O-ring in isopropyl alcohol for a few minutes.
Rationale: Doing so lubricates the O-ring and aids your fitting the
O-ring to the isolation valve.
12. Fit the new O-ring to the isolation valve.
13. Fit the isolation valve to the ion block assembly.
Cleaning the ion block, isolation valve, and extraction cone
5-47
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.
Ion block assembly set
screw
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.
Caution: To avoid damage to the thermocouple, do not
overtighten the set screw.
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.
5-48
Maintenance Procedures
Fitting the ion block assembly to the source assembly
Required materials:
•
Chemical-resistant, powder-free gloves
•
6-mm Allen wrench
To fit the ion block assembly
Warning: To avoid puncture wounds, take great care while working
with the source enclosure door open if one or both of these conditions
apply:
• An ESI probe is fitted (the probe tip is sharp).
• A corona pin is fitted (the pin tip is sharp).
Caution: To avoid recontaminating the ion block assembly, wear clean
chemical-resistant, powder-free gloves during this procedure.
1.
Unscrew and remove the 3 thumbscrews that secure the right-hand side
flange to the source enclosure.
Thumbscrew
Source enclosure side flange
TP02657
2.
Remove the side flange from the source enclosure.
Rationale: This step allows you to see the ion block assembly as you fit it
to the PEEK ion block support.
Cleaning the ion block, isolation valve, and extraction cone
5-49
Caution: Do not apply any downward force to the source
enclosure door while the door is open.
3.
Unfasten the source enclosure door’s handle and open the door.
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 5-7.
11. Close the source enclosure door and fasten its handle by rotating it 90
degrees counterclockwise to the vertical position and then pushing it
downward.
5-50
Maintenance Procedures
Cleaning the source hexapole assembly
The source hexapole assembly must be cleaned if cleaning the ion block,
isolation valve, and extraction cone fails to increase signal sensitivity.
Removing the ion block assembly, ion block support, and
hexapole from the source assembly
Required materials:
•
Chemical-resistant, powder-free gloves
•
3-mm Allen wrench
•
O-ring removal kit
To remove the ion block assembly, ion block support, and hexapole
Warning: The source components can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing
this procedure.
1.
Remove the ion block assembly from the PEEK ion block support. See
“Removing the ion block assembly from the source assembly” on
page 5-35.
Cleaning the source hexapole assembly
5-51
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
PEEK ion block
support
Securing screws
Hexapole
assembly
3.
Remove the PEEK ion block support from the adaptor housing.
4.
Use the O-ring removal kit to carefully remove all the O-rings from the
PEEK ion block support. See “Removing O-rings and seals” on page 5-9.
Warning: The O-rings can be contaminated with
biohazardous and/or toxic materials. Ensure that they are
correctly disposed of according to local environmental
regulations.
5.
Dispose of the O-rings in accordance with local environmental
regulations.
Caution: To avoid damage, when removing the hexapole
assembly from the adaptor housing, observe these precautions:
• Avoid scratching the internal surfaces of the adaptor block.
• Do not compress the hexapole rods.
6.
Carefully grasp the source hexapole assembly and remove it from the
adaptor housing.
Cleaning the hexapole assembly
Required materials:
5-52
Maintenance Procedures
•
Chemical-resistant, powder-free gloves.
•
500-mL measuring cylinder or appropriately sized glass vessel in which
to completely immerse the hexapole when cleaning. Use only glassware
not previously cleaned with surfactants.
•
Length of small diameter stainless steel tube.
•
HPLC-grade (or better) methanol.
•
Ultrasonic bath.
•
Source of oil-free, inert gas (nitrogen or helium) for drying (air-drying
optional).
•
HPLC-grade (or better) 1:1 methanol/water.
•
Wash-bottle containing HPLC-grade (or better) 1:1 methanol/water.
•
Large beaker.
•
Small, flat-blade screwdriver.
To clean the source hexapole assembly
Warning: The source hexapole assembly can be contaminated
with biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
1.
Bend the stainless steel tube into a hook shape.
2.
Insert one end of the hook into one of the holes on the hexapole
assembly’s rear support ring.
Cleaning the source hexapole assembly
5-53
Caution: To avoid vibration damage to the hexapole assembly,
ensure that the bottom of the assembly is not in contact with the
bottom of the glass vessel.
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
Rear support ring
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.
Caution: To avoid recontaminating the hexapole assembly, wear
clean, chemical-resistant, powder-free gloves for the rest of this
procedure.
6.
5-54
Carefully remove the hexapole assembly from the vessel, and blow-dry it
using inert, oil-free gas.
Maintenance Procedures
7.
8.
Inspect the hexapole assembly for persisting contamination, If
contamination is present, do as follows:
a.
Use the wash-bottle containing methanol to rinse the source
hexapole assembly over the large beaker.
b.
Blow-dry the hexapole assembly with inert, oil-free gas.
Use the small flat-blade screwdriver to ensure that the hexapole
assembly screws are tight.
Fitting the hexapole assembly, PEEK ion block support, and ion
block assembly to the source assembly
Required materials:
•
Chemical-resistant, powder-free gloves
•
3-mm Allen wrench
•
Lint-free cloth
•
HPLC-grade (or better) 1:1 methanol/water
To fit the hexapole assembly and PEEK ion block support to the source
Caution: To avoid recontaminating the source, wear clean,
chemical-resistant, powder-free gloves during this procedure.
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.
Cleaning the source hexapole assembly
5-55
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.
Caution: To ensure correct operation of the instrument, neither
hexapole spring must touch a hexapole rod.
5.
Use the 3-mm Allen wrench to fit and tighten the 3 PEEK ion block
support securing screws.
Tip: Look through the PEEK ion block support as you tighten the
securing screws. Ensure that neither hexapole spring buckles and
touches a hexapole rod.
Hexapole spring
Hexapole rod
TP02659
6.
5-56
Fit the ion block assembly to the PEEK ion block support. See “Fitting
the ion block assembly to the source assembly” on page 5-49.
Maintenance Procedures
Replacing the ESI probe tip
Replace the ESI probe tip if a blockage occurs in the internal metal sheathing
through which the stainless steel capillary passes or if the probe tip threads
are damaged.
Required materials:
•
Chemical-resistant, powder-free gloves
•
6-mm (¼-inch) wrench
To replace the ESI probe tip
Warning: The probe and source components can be contaminated
with biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
Warning: The probe and source can be hot. To avoid burn injuries, take
great care while performing this procedure.
Warning: The ESI probe tip is sharp. To avoid puncture wounds,
handle the probe with care.
1.
Remove the probe from the source. See also “Installing the corona pin”
on page 3-5.
2.
Use the 6-mm (¼-inch) wrench to unscrew and remove the probe tip.
Warning: The probe tip can be contaminated with
biohazardous and/or toxic materials. Ensure that it is
correctly disposed of according to local environmental
regulations.
3.
Dispose of the probe tip in accordance with local environmental
regulations.
4.
Use the 6-mm (¼-inch) wrench to fit and tighten the new probe tip to the
probe.
Replacing the ESI probe tip
5-57
5.
Adjust the probe tip so that the fully extended capillary (when the probe
nebulizer adjuster knob is fully screwed down) protrudes by
approximately 1 to 1.5 mm.
6.
Fit the probe to the source. See also “Installing the ESI probe” on
page 3-2.
Replacing the ESI probe sample capillary
The stainless steel sample capillary in the ESI probe must be replaced if it
becomes blocked and cannot be cleared, or if it becomes contaminated or
damaged.
Required materials:
5-58
•
Chemical-resistant, powder-free gloves
•
1.5-mm Allen wrench
•
6-mm (¼-inch) wrench
•
5/16-inch wrench
•
7/16-inch wrench
•
Flat-blade screwdriver
•
Needle-nose pliers
•
LC pump
•
HPLC-grade (or better) 1:1 acetonitrile/water
Maintenance Procedures
To replace the capillary
Warning: The probe and source components can be contaminated
with biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
Warning: The probe and source can be hot. To avoid burn injuries, take
great care while performing this procedure.
Warning: The ESI probe tip is sharp. To avoid puncture wounds,
handle the probe with care.
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
Replacing the ESI probe sample capillary
5-59
3.
Use the 1.5-mm wrench to loosen the set screw on the LC PEEK union.
Setscrew
TP03005
4.
Remove the end-cover.
End-cover
TP03006
5.
Use the 6-mm wrench to remove the probe tip.
Probe tip
TP03007
5-60
Maintenance Procedures
6.
Use the 5/16-inch and 7/16-inch wrenches to unscrew the coupling.
Coupling
LC union
TP03009
7.
Withdraw the LC union, coupling and capillary from the probe.
8.
Remove the LC union, capillary and seal from the coupling.
Seal
TP03011
GVF16 Ferrule
LC union
Capillary
Coupling
PTFE liner
Warning: The capillary, PTFE liner, ferrule assembly, and
seal can be contaminated with biohazardous and/or toxic
materials. Ensure that they are correctly disposed of
according to local environmental regulations.
9.
Dispose of the capillary, PTFE liner, ferrule assembly, and seal in
accordance with local environmental regulations.
Replacing the ESI probe sample capillary
5-61
10. Use the needle-nose pliers to remove the conductive sleeve from the
inner bore of the probe assembly fitting.
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.
5-62
Maintenance Procedures
14. Slide a compression screw and ferrule onto a piece of 1/16 × 0.0025 bore
(5M) PEEK tubing and connect the tubing to the opposite side of the LC
union.
TP03014
PEEK tubing
Compression
screw
LC union
Capillary
Coupling
15. Push the capillary into the union until it seats.
16. Tighten the adaptor nut on the LC union so that it is snug but not tight.
17. Gently tug the capillary to make sure it remains secure.
18. Remove the PEEK tubing from the union.
19. Check for leaks in the assembly by attaching the free end of the PEEK
tubing to an LC pump and pumping 1:1 acetonitrile/water through it at
1 mL/min.
20. If leakage occurs, disassemble and remake the connection, and then
repeat the leak test.
21. When performing the leak test, check the backpressure on the LC pump,
which will be relatively high if the capillary is blocked. If this is the case,
replace the capillary.
22. When the leak test is performed successfully, disconnect the PEEK
tubing from the LC pump.
23. Slide the conductive sleeve onto the capillary, and then feed the
capillary through the probe.
TP03015
Conductive sleeve
Replacing the ESI probe sample capillary
5-63
24. Attach the coupling nut to the probe, and gently tighten it with the
7/16-inch wrench.
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
26. Fit the probe end-cover.
27. Fit and tighten the two probe end-cover retaining screws.
28. Tighten the set screw to clamp the LC union in place.
29. Attach the nebulizer gas connection to the probe.
30. Fit the probe to the instrument.
5-64
Maintenance Procedures
Cleaning the IonSABRE APCI probe tip
Clean the APCI probe tip when a buffer buildup is detected on the probe tip or
when the signal intensity weakens.
To clean the APCI probe tip
1.
Stop the liquid flow.
2.
In the Tune window, click Gas
3.
In the Source tab, set Desolvation to 650 L/hr.
4.
Set APcI Probe Temp to 650 °C.
5.
Click Operate
6.
Wait 10 minutes.
to start the desolvation gas flow.
.
Rationale: The high APCI probe heater temperature removes any
chemical contamination from the probe tip.
Replacing the IonSABRE APCI probe sample capillary
Replace the stainless steel sample capillary in the APCI probe if it becomes
blocked and you cannot clear it, or if it becomes contaminated or damaged.
Removing the existing capillary
Required materials:
•
Chemical-resistant, powder-free gloves
•
Needle-nose pliers
•
7-mm wrench
•
2.5-mm Allen wrench
Cleaning the IonSABRE APCI probe tip
5-65
To remove the existing capillary
Warning: The probe and source components can be contaminated
with biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
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 6-7.
2.
Use the 2.5-mm Allen wrench to remove the 2 probe end-cover retaining
screws.
End-cover retaining screws
TP02676
5-66
Maintenance Procedures
3.
Remove the end-cover.
End-cover
TP02677
4.
Unscrew and remove the nebulizer adjuster knob to reveal a PEEK
union/UNF coupling assembly and the capillary.
Capillary
Nebulizer adjuster knob
5.
TP02674
Remove the nebulizer adjuster knob, PEEK union/UNF coupling
assembly, and capillary from the probe.
Replacing the IonSABRE APCI probe sample capillary
5-67
6.
Remove the PEEK union/UNF coupling assembly and capillary from the
nebulizer adjuster knob.
PEEK union/UNF assembly
TP02675
7.
Use the 7-mm wrench to loosen the locknut securing the PEEK union
and UNF coupling.
PEEK union
7-mm wrench
TP02672
Locknut
5-68
Maintenance Procedures
UNF coupling
8.
Unscrew the PEEK union from the UNF coupling. This connection is
finger-tight only.
TP02679
9.
Remove the ferrule from the capillary.
Ferrule
TP02667
10. Remove the capillary from the UNF coupling.
Installing the new capillary
Required materials:
•
Chemical-resistant, powder-free gloves
•
Needle-nose pliers
•
7-mm wrench
•
2.5-mm Allen wrench
•
Length of red PEEK tubing
•
LC pump
•
HPLC-grade (or better) 1:1 acetonitrile/water
Replacing the IonSABRE APCI probe sample capillary
5-69
To install the new capillary
Warning: The probe and source components can be contaminated
with biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
1.
Insert a square-cut length of red PEEK tubing in the probe inlet
connector, and screw the connector, finger-tight, into the PEEK union.
This step ensures a minimum dead volume when fitting the capillary.
Probe inlet connector
TP02671
PEEK tubing
5-70
2.
Fit the UNF coupling to the new capillary.
3.
Use the needle-nose pliers to slide a new ferrule onto the capillary.
4.
Insert the capillary in the PEEK union, and ensure that it is fully
seated.
5.
Screw the UNF coupling into the PEEK union, finger-tight only.
6.
Pull on the capillary gently, testing to ensure that it stays in place.
7.
Use the 7-mm wrench to tighten the locknut against the PEEK union.
8.
Check for leaks in the assembly by attaching the free end of the PEEK
tubing to an LC pump and pumping 1:1 acetonitrile/water at 1 mL/min.
Maintenance Procedures
9.
If leakage occurs, disassemble and remake the connection, and repeat
the leak test.
10. When performing the leak test, check the backpressure on the LC pump,
which will be high if the capillary is blocked. If this is the case, replace
the capillary.
11. When the leak test has been performed successfully, disconnect the
PEEK tubing from the LC pump.
12. Remove the probe inlet connector and PEEK tubing from the PEEK
union.
13. Remove the probe heater. See “Replacing the APCI probe heater” on
page 5-74, step 2 through step 4.
14. Fit the PEEK union/UNF coupling assembly to the nebulizer adjuster
knob.
15. Carefully thread the capillary through the probe assembly.
16. Depress the PEEK union so that the locating pin on the UNF coupling is
fully engaged in the locating slot at the head of the probe assembly.
When the union is fully depressed, tighten the nebulizer adjuster knob.
Do not tighten the knob fully.
Locating pin
Locating slot
TP02668
17. Fit the probe end-cover to the probe assembly.
Replacing the IonSABRE APCI probe sample capillary
5-71
18. Use the 2.5-mm Allen wrench to fit and tighten the 2 end-cover securing
screws.
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 5-74, step 5 through step 8.
20. Fit the probe to the instrument. See “Installing the IonSABRE APCI
probe” on page 6-3.
21. In the 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.
5-72
Maintenance Procedures
Cleaning or replacing the corona pin
Required materials:
•
Chemical-resistant, powder-free gloves
•
Needle-nose pliers
•
HPLC-grade (or better) methanol
•
Lint-free tissue
To clean or replace the corona pin
Warning: The probe and source components can be contaminated
with biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
Warning: The probe and source can be hot. To avoid burn injuries, take
great care while performing this procedure.
Warning: To avoid electric shock, ensure that the instrument is in
Standby mode before commencing this procedure.
Warning: The corona pin tip is sharp. To avoid puncture wounds,
handle the corona pin with care.
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 3-9.
2.
Replace the pin if it is deformed or otherwise damaged. 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.
Cleaning or replacing the corona pin
5-73
Replacing the APCI probe heater
Replace the APCI probe heater if it fails to heat.
Required materials:
•
Chemical-resistant, powder-free gloves
•
Flat-blade jeweler’s screwdriver
To replace the APCI probe heater
Warning: The probe and source components can be contaminated
with biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
1.
Remove the probe from the source. See “Removing the IonSABRE APCI
probe” on page 6-7.
2.
Use the jeweler’s screwdriver to loosen the 2 set screws securing the
probe heater cover to the probe.
Set screw
5-74
Maintenance Procedures
TP02673
Probe
heater cover
Caution: Take great care not to damage the probe heater’s
electrical wiring when removing the probe heater cover or while
the probe heater is exposed.
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
Replacing the APCI probe heater
5-75
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.
5.
Carefully slide the probe heater over the capillary sleeve on the probe
assembly.
Probe heater connections
TP02670
Capillary
Capillary sleeve
Caution: To avoid damaging the probe heater’s electrical
connections, do not twist the heater when fitting it to the probe
assembly.
6.
Fit the probe heater to the probe assembly, ensuring that the heater is
fully seated on the probe assembly.
TP02669
5-76
Maintenance Procedures
7.
Fit the probe heater cover to the probe assembly.
8.
Use the jeweler’s screwdriver to tighten the 2 set screws securing the
probe heater cover to the probe.
9.
Fit the probe to the instrument. See “Installing the IonSABRE APCI
probe” on page 6-3.
10. In the console, click API
to start the desolvation gas flow.
11. Use the probe adjuster knob to adjust the capillary so that the capillary
protrudes approximately 0.5 mm from the end of the probe.
Replacing the ion block source heater
Replace the ion block source heater if it fails to heat when the instrument is
pumped down (evacuated).
Required materials:
•
Chemical-resistant, powder-free gloves
•
Needle-nose pliers
•
1.5-mm and 2.5-mm Allen wrenches
To replace the ion block source heater
Warning: The ion block assembly can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
1.
Remove the ion block assembly from the instrument. See “Removing the
ion block assembly from the source assembly” on page 5-35.
Replacing the ion block source heater
5-77
2.
Ensure that the isolation valve is closed.
Isolation valve handle
in closed position
TP02650
3.
Use the 2.5-mm Allen wrench to loosen the 4 captive screws securing the
ion block cover plate.
Ion block cover plate captive
securing screw
Ion block cover plate
TP02649
4.
5-78
Remove the ion block cover plate.
Maintenance Procedures
5.
Use the 1.5-mm Allen wrench to remove the 2 screws securing the
heater wires to the PEEK terminal block.
Heater cartridge wire
securing screws
TP02616
PEEK terminal block
6.
Use the needle-nose pliers to carefully swing the ring terminal tags out
of the terminal block.
Ring terminal tag
TP02617
Replacing the ion block source heater
5-79
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
Heater cartridge assembly
TP02618
8.
Dispose of the heater cartridge assembly.
Caution: To avoid damaging the heater cartridge assembly
wires, do not bend or twist them either side of the heater
cartridge assembly heat-shrink tubing when fitting the assembly
to the ion block.
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..
Caution: To avoid a short circuit to the ion block cover, ensure
that the two heater cartridge ring tags are pushed fully down on
the PEEK block terminals.
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.
5-80
Maintenance Procedures
13. Fit the ion block assembly to the instrument. See “Fitting the ion block
assembly to the source assembly” on page 5-49.
Replacing the source assembly seals
Warning: To avoid possible excessive leakage of solvent vapor
into the laboratory atmosphere, the seals listed below must be
renewed, at intervals of no greater than 1 year, exactly as
described in this section.
To avoid possible excessive leakage of solvent vapor into the laboratory
atmosphere, the following seals must be renewed at intervals of no greater
than 1 year:
•
Source enclosure door seal
•
Source enclosure door glass seal
•
Source enclosure housing seal
•
Source enclosure side flange seal
•
Probe adjuster assembly probe seal
•
Probe adjuster assembly flange seal
To complete this procedure, you must pressure test the source, as described in
the Waters Micromass Source Pressure Test Unit Operator’s Guide.
Removing the source enclosure from the instrument
Required materials:
•
Chemical-resistant, powder-free gloves
•
5-mm Allen wrench
Replacing the source assembly seals
5-81
To remove the source enclosure
Warning: The source components can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
1.
Vent and shut-down the detector. See “Shutting down the detector” on
page 2-12.
Warning: The source can be hot. To avoid burn injuries, allow it
to cool for at least 30 minutes before proceeding.
2.
Remove the probe from the source.
•
If you are removing an ESI probe, see “Installing the corona pin” on
page 3-5.
•
If you are removing an IonSABRE APCI probe, see “Removing the
IonSABRE APCI probe” on page 6-7.
Caution: Do not apply any downward force to the source
enclosure door while the door is open.
3.
Unfasten the source enclosure door’s handle and open the door.
Warning: The corona pin tip is sharp. To avoid puncture wounds,
handle the corona pin with care.
5-82
4.
If using ESCi mode or an IonSABRE APCI probe, carefully remove the
corona pin. See “Removing the corona pin” on page 3-9.
5.
Disconnect the probe’s electrical connection at the instrument’s front
panel.
6.
Disconnect the PTFE tubing at the desolvation gas connection on the
front panel.
7.
Disconnect the 2-pin connector at the rear of the source enclosure.
Maintenance Procedures
8.
Use the 5-mm Allen wrench to loosen the 3 captive source enclosure
securing screws.
Source enclosure
securing screw
Source enclosure
securing screws
TP02656
Caution: Do not apply any downward force to the source
enclosure door when removing the source enclosure from the
instrument’s housing.
9.
Remove the source enclosure from the instrument.
Replacing the source assembly seals
5-83
Disassembling the source enclosure and probe adjuster
assembly
Required materials:
•
Chemical-resistant, powder-free gloves
•
4-mm Allen wrench
To dismantle the source enclosure and probe adjuster assembly
Warning: The source components can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
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
TP02657
5-84
2.
Remove the probe adjuster assembly from the source enclosure.
3.
Unscrew and remove the 3 thumbscrews that secure the source
enclosure side flange to the source enclosure.
4.
Remove the source enclosure side flange from the source enclosure.
Maintenance Procedures
Removing the seals from the source enclosure and probe
adjuster assembly
Required materials:
•
Chemical-resistant, powder-free gloves
•
3-mm Allen wrench
•
O-ring removal kit
To remove the seals from the source enclosure and probe adjuster
assembly
Warning: The source components can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
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 5-9.
Probe adjuster assembly probe seal
TP02632
Replacing the source assembly seals
5-85
2.
Use the O-ring removal kit to carefully remove the following seals from
the source enclosure:
•
Source enclosure housing seal
•
Source enclosure side flange seal
•
Probe adjuster assembly flange seal
Probe adjuster
assembly flange seal
Source enclosure
housing seal
Source side
flange seal
TP02666
Caution: Do not apply any downward force to the source
enclosure door while the door is open.
3.
5-86
Unlatch the source enclosure door handle by pulling it upward to the
horizontal position and then rotating it 90 degrees clockwise and open
the door.
Maintenance Procedures
4.
Use the O-ring removal kit to carefully remove the seal from the source
enclosure door.
Door glass retaining clip
Source enclosure door glass seal
Source enclosure door seal
TP02662
5.
Use the 3-mm Allen wrench to remove the 4 bolts securing the
glass-retaining clips to the source enclosure door.
6.
Remove the 4 glass-retaining clips from the source enclosure door.
7.
Remove the glass from the source enclosure door.
8.
Use the O-ring removal kit to carefully remove the door glass seal from
the source enclosure door.
Warning: The seals can be contaminated with biohazardous
and/or toxic materials. Ensure that they are correctly
disposed of according to local environmental regulations.
9.
Dispose of all the seals in accordance with local environmental
regulations.
Replacing the source assembly seals
5-87
Fitting the new source enclosure and probe adjuster assembly
seals
Required materials:
•
Chemical-resistant, powder-free gloves
•
3-mm Allen wrench
•
Wash bottle containing HPLC-grade (or better) 1:1 methanol/water
To fit the new source enclosure and probe seals
Warning: The source components can be contaminated with
biohazardous and/or toxic materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
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 4 glass retaining clips to the source enclosure door.
Caution: The 4 bolts securing the glass retaining clips must each
be sequentially and incrementally tightened until they are all
fully tight.
5.
Use the 3-mm Allen wrench to fit and tighten the 4 bolts 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.
5-88
Fit the new source enclosure door seal to the source enclosure door.
Maintenance Procedures
7.
Close the source enclosure door and fasten the handle by rotating it 90
degrees counterclockwise to the vertical position and then pushing it
downward.
8.
Fit the following new seals to the source enclosure:
9.
•
Source enclosure housing seal
•
Source enclosure side flange seal
•
Probe adjuster assembly flange seal
Fit the new probe adjuster assembly probe seal to the probe adjuster
assembly.
Assembling the probe adjuster assembly and source enclosure
Required materials:
•
Chemical-resistant, powder-free gloves
•
4-mm Allen wrench
To assemble the probe adjuster assembly and source enclosure
1.
Fit the source enclosure side flange to the source enclosure.
Caution: The source enclosure side flange securing thumbscrews
must each be sequentially and incrementally tightened until
they are all fully tight.
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.
Caution: The probe adjuster assembly securing screws must each
be sequentially and incrementally tightened until they are all
fully tight.
4.
Use the 4-mm Allen wrench to fit and tighten the 4 screws securing the
probe adjuster assembly to the source enclosure.
Replacing the source assembly seals
5-89
Fitting the source enclosure to the instrument
Required materials:
•
Chemical-resistant, powder-free gloves
•
5-mm Allen wrench
To fit the source enclosure to the instrument
Warning: To confirm the integrity of the source exhaust system,
perform the procedure exactly as described in this section.
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.
1.
Ensuring that the wires to the microswitch do not become trapped
between the source enclosure and the instrument’s housing, fit the
source enclosure to the housing.
Caution: The source enclosure securing screws must each be
sequentially and incrementally tightened until they are all fully
tight.
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.
Warning: The corona pin tip is sharp. To avoid puncture wounds,
handle the corona pin with care.
6.
5-90
If using ESCi mode or an IonSABRE APCI probe, carefully fit the corona
pin. See “Installing the corona pin” on page 3-5.
Maintenance Procedures
7.
Close the source enclosure door and fasten the door’s handle by rotating
it 90 degrees counterclockwise to the vertical position and then pushing
it downward.
8.
Fit the probe to the source.
9.
•
If you are fitting an ESI probe, see “Installing the ESI probe” on
page 3-2.
•
If you are fitting an IonSABRE APCI probe, see “Installing the
IonSABRE APCI probe” on page 6-3.
Start the detector. See “Starting the detector” on page 2-2.
Warning: To confirm the integrity of the source exhaust
system, a source pressure test must be performed, as
described in the Waters Micromass Source Pressure Test
Unit Operator’s Guide.
10. Perform a source pressure test, as described in the Waters Micromass
Source Pressure Test Unit Operator’s Guide.
Maintaining the detector air filters
Cleaning the air filter inside the instrument’s door
Required material: Vacuum cleaner
To clean the air filter inside the instrument’s door
Use a vacuum cleaner to clean the air filter located inside the instrument’s
door.
Maintaining the detector air filters
5-91
Air filter inside the instrument’s door
Air filter
Frame
TP02628
Replacing the air filter inside the instrument’s door
If you cannot clean the air filter by vacuuming, replace it with a new filter.
Required materials:
•
T10 TORX® driver
•
3100 detector door air filters
To replace the air filter inside the instrument’s door
1.
5-92
Use the T10 TORX driver to remove the 4 screws that secure the air
filter frame and air filter to the inside of the instrument’s door. See the
figure “Air filter inside the instrument’s door” on page 5-92.
Maintenance Procedures
2.
Remove the air filter from the air filter frame and dispose of it.
3.
Align the new air filter within the air filter frame.
4.
Use the T10 TORX driver to fit and tighten the 4 screws securing the air
filter and frame to the inside of the instrument’s door.
Cleaning the air filter inside the instrument’s lower bezel
Required materials:
•
T10 TORX driver
•
Vacuum cleaner
To clean the air filter inside the instrument’s lower bezel
1.
Use the T10 TORX driver to remove the 5 screws that secure the lower
bezel in place.
Instrument’s lower bezel
Screws
TP02636
Screws
2.
Use a vacuum cleaner to clean the air filter located inside the
instrument’s lower bezel.
Maintaining the detector air filters
5-93
Air filter inside the instrument’s lower bezel
Air filter
Frame
TP02638
3.
Reinstall the lower bezel.
Replacing the air filter inside the lower bezel
If you cannot clean the air filter by vacuuming, replace it with a new filter.
Required materials:
•
T10 TORX driver
•
3100 detector lower bezel air filter
To replace the air filter inside the lower bezel
5-94
1.
Remove the 5 screws that secure the lower bezel in place. See the figure
“Instrument’s lower bezel” on page 5-93.
2.
Use the T10 TORX driver to remove the 4 screws that secure the air
filter frame and air filter to the inside of the lower bezel.
Maintenance Procedures
Air filter inside the lower bezel
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.
Cleaning the air filter behind the source probe
Required material: Vacuum cleaner
To clean the air filter behind the source probe
1.
2.
Remove the probe from the source.
•
If you are removing an ESI probe, see “Installing the corona pin” on
page 3-5.
•
If you are removing an IonSABRE APCI probe, see “Removing the
IonSABRE APCI probe” on page 6-7.
Grasp the air filter tab, and remove the air filter frame by lifting it
toward you.
Maintaining the detector air filters
5-95
Air filter tab
Air filter tab
TP02665
3.
Use a vacuum cleaner to clean the air filter.
Air filter removed from behind the source probe
Air filter
Frame
TP02637
5-96
4.
Reinstall the air filter.
5.
Fit the probe to the source.
Maintenance Procedures
•
If you are fitting an ESI probe, see “Installing the ESI probe” on
page 3-2.
•
If you are fitting an IonSABRE APCI probe, see “Installing the
IonSABRE APCI probe” on page 6-3.
Replacing the air filter behind the source probe
To replace the air filter behind the source probe
1.
Remove the probe from the source.
•
If you are removing an ESI probe, see “Installing the corona pin” on
page 3-5.
•
If you are removing an IonSABRE APCI probe, see “Removing the
IonSABRE APCI probe” on page 6-7.
2.
Grasp the air filter tab and remove the air filter frame by lifting it
toward you. See the figure “Air filter tab” on page 5-96.
3.
Remove the air filter from the air filter frame and dispose of it.
Removing air filter from frame
Frame
Air filter
TP02640
4.
Insert the new air filter in the air filter frame.
5.
Reinstall the air filter.
6.
Fit the probe to the source.
Maintaining the detector air filters
5-97
•
If you are fitting an ESI probe, see “Installing the ESI probe” on
page 3-2.
•
If you are fitting an IonSABRE APCI probe, see “Installing the
IonSABRE APCI probe” on page 6-3.
Replacing the roughing pump oil
Change the roughing pump oil annually.
Note: This procedure is not required for an Alcatel oil-free roughing pump.
Required materials:
•
Chemical-resistant, powder-free gloves
•
8-mm Allen wrench
•
Flat-blade screwdriver
•
Container to catch used oil
•
Funnel
•
1-L container of Anderol vacuum oil, type GS 495
To replace the roughing pump oil
1.
Gas ballast the roughing pump for 1 hour to reduce the oil viscosity.
Rationale: Gas ballasting helps to circulate and mix the oil through the
pump before draining.
See “Gas ballasting the roughing pump” on page 5-20.
2.
Vent and shut-down the detector. See “Shutting down the detector” on
page 2-12.
3.
Allow the roughing pump to cool.
Warning: The roughing pump oil can be contaminated with
analyte accumulated during normal operation. Always
wear chemical-resistant, powder-free gloves when adding
or replacing oil.
Warning: To avoid burn injuries, take great care while working
with the roughing pump: it can be hot.
4.
5-98
Place the container for used oil under the pump’s drain plug.
Maintenance Procedures
5.
Use the 8-mm Allen wrench to remove the oil filler plug.
Oil filler plug
Oil-level sight glass
TP02689
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.
Warning: The roughing pump oil can be contaminated with
biohazardous and/or toxic materials. Ensure that they are
correctly disposed of according to local environmental
regulations.
8.
Dispose of the roughing pump oil in accordance with local environmental
regulations.
9.
Ensure that the O-ring on the oil drain plug is clean and properly
seated.
Replacing the roughing pump oil
5-99
Caution: Observe these precautions to avoid oil leakage when
fitting the oil drain plug to the roughing pump:
• Ensure that the plug is not cross-threaded.
• Ensure that the O-ring is not pinched.
• Do not overtighten the plug.
10. Use the 8-mm Allen wrench to fit and tighten the roughing pump’s oil
drain plug.
Tip: When the oil drain 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.
Caution: To maintain pump performance, use Anderol vacuum
oil, type GS 495.
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.
Caution: Observe these precautions 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.
14. Use the 8-mm Allen wrench to refit the oil filler plug.
15. Start the detector. See “Starting the detector” on page 2-2.
16. Gas-ballast the roughing pump. See “Gas ballasting the roughing pump”
on page 5-20.
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.
5-100 Maintenance Procedures
•
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.
Replacing the roughing pump’s oil demister element
Replace the roughing pump’s oil demister element annually.
Note: This procedure is not required for an Alcatel oil-free roughing pump.
Required materials:
•
Chemical-resistant, powder-free gloves
•
6-mm Allen wrench
•
10-mm wrench
To remove the roughing pump oil demister element
1.
Vent and shut-down the detector. See “Shutting down the detector” on
page 2-12.
2.
Allow the roughing pump to cool.
Replacing the roughing pump’s oil demister element 5-101
Warning: The pump oil can be contaminated with analyte
accumulated during normal operation. Always wear
chemical-resistant, powder-free gloves when replacing the
oil demister element.
Warning: To avoid burn injuries, take great care while working
with the roughing pump: it can be hot.
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
5-102 Maintenance Procedures
4.
Using both hands, carefully remove the exhaust flange and oil demister
element from the roughing pump.
Oil demister element
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
Replacing the roughing pump’s oil demister element 5-103
6.
Holding the oil demister element slightly elevated to prevent the loss of
the spring, remove the exhaust flange from the oil demister element.
TP02692
7.
Remove the spring from the oil demister element.
Warning: The oil demister element can be contaminated
with biohazardous and/or toxic materials. Ensure that it is
correctly disposed of according to local environmental
regulations.
8.
Dispose of the oil demister element in accordance with local
environmental regulations.
5-104 Maintenance Procedures
To fit the new oil demister element
Warning: The pump oil can be contaminated with analyte
accumulated during normal operation. Always wear
chemical-resistant, powder-free gloves when replacing the oil
demister element.
1.
Fit the spring to the new oil demister element.
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
Replacing the roughing pump’s oil demister element 5-105
4.
Ensure that the inscription “TOP” is at the top of the oil demister
element, and, using both hands, carefully fit the oil demister element
and exhaust flange to the roughing pump.
Caution: The bolts securing the source exhaust flange to the
roughing pump must each be sequentially and incrementally
tightened until they are all fully tight.
5.
Use the 6-mm Allen wrench to fit the 4 bolts securing the exhaust flange
to the roughing pump.
6.
Start the detector. See “Starting the detector” on page 2-2.
5-106 Maintenance Procedures
6
Optional APCI Mode of
Operation
This chapter describes the optional atmospheric pressure chemical
ionization (APCI) mode of operation, which uses the IonSABRE APCI
source.
Contents
Topic
Page
Atmospheric pressure chemical ionization
6-2
IonSABRE APCI probe
6-3
Installing the IonSABRE APCI probe
6-3
Installing the corona pin
6-6
Removing the corona pin
6-6
Removing the IonSABRE APCI probe
6-7
6-1
Atmospheric pressure chemical ionization
APCI, an option for the detector, 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 LC column enters
the probe, where it is pneumatically converted to an aerosol, rapidly heated,
and vaporized or gasified at the probe tip.
APCI mode
IonSABRE APCI probe
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.
6-2
Optional APCI Mode of Operation
IonSABRE APCI probe
In the IonSABRE APCI probe, the nebulized gas plume expands in a directly
heated region with a larger internal diameter. The increased aerosol
expansion gives more efficient droplet evaporation than the standard ESI
probe. The nebulizer support gas controls the droplet residence times and
positively sweeps the sample from the probe, giving optimized probe
performance. The gas flow must be maintained at all times.
Installing the IonSABRE APCI probe
Required material: Chemical-resistant, powder-free gloves
To install the IonSABRE APCI probe
Warning: The LC system connections, IonSABRE APCI probe,
and source can be contaminated with biohazardous and/or toxic
materials. Always wear chemical-resistant, powder-free gloves
while performing this procedure.
Warning: To avoid electric shock, ensure that the instrument is
suitably prepared before commencing this procedure.
1.
Prepare the instrument for working on the source. See “Preparing the
instrument for working on the source” on page 5-6.
Warning: The source can be hot. To avoid burn injuries, take
great care while working with the instrument’s access door open.
2.
Open the instrument’s access door.
IonSABRE APCI probe
6-3
3.
Ensure that the contacts on the IonSABRE APCI probe align with the
probe adjuster assembly contacts, and carefully slide the IonSABRE
APCI probe into the hole in the probe adjuster assembly.
IonSABRE APCI probe
Probe adjuster assembly
Probe adjuster
assembly contacts
TP02632
4.
6-4
Secure the IonSABRE APCI probe by tightening the 2 thumbscrews
shown in the following figure.
Optional APCI Mode of Operation
IonSABRE APCI probe mounted on the source enclosure, showing the
connections to the front panel
Vernier probe adjuster
Thumbscrew
Nebulizer gas connection
Desolvation gas connection
APCI probe
electrical lead
Probe adjuster
assembly electrical
lead (not connected
when using the
IonSABRE APCI
probe)
Probe adjuster assembly
IonSABRE APCI
probe
TP02696
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.
Installing the IonSABRE APCI probe
6-5
Warning: To avoid electric shock, do not use stainless steel
tubing to connect the diverter valve to the IonSABRE APCI
probe; use the PEEK™ tubing supplied with the instrument.
8.
Using tubing of the appropriate internal diameter (ID), connect the
fluidics system’s diverter valve to the IonSABRE APCI probe. Two tubes
of differing ID are supplied with the instrument.
Requirement: If you are replacing the tubing supplied with the
instrument, minimize the length of the tube connecting the diverter
valve to the IonSABRE APCI probe. Doing so minimizes delays and
dispersion.
9.
Close the instrument’s access door.
Installing the corona pin
To install the corona pin
Refer to “Installing the corona pin” on page 3-5.
Removing the corona pin
To remove the corona pin
Refer to “Removing the corona pin” on page 3-9.
6-6
Optional APCI Mode of Operation
Removing the IonSABRE APCI probe
Required material: Chemical-resistant, powder-free gloves
To remove the IonSABRE APCI probe
Warning: The LC system connections, IonSABRE APCI probe,
and source can be contaminated with biohazardous and/or toxic
materials. Always wear chemical-resistant, powder-free gloves
while performing this procedure.
Warning: To avoid electric shock, ensure that the instrument is
suitably prepared before commencing this procedure.
1.
Prepare the instrument for working on the source. See “Preparing the
instrument for working on the source” on page 5-6.
Warning: The source can be hot. To avoid burn injuries, take
great care while working with the instrument’s access door open.
2.
Open the instrument’s access door.
3.
Disconnect the diverter valve tubing from the IonSABRE APCI probe.
4.
Disconnect the IonSABRE APCI probe’s electrical lead from the
instrument’s probe connection.
5.
Disconnect the IonSABRE APCI probe’s PTFE tube from the nebulizer
gas connection.
6.
Undo the 2 thumbscrews securing the probe to the probe adjuster
assembly.
7.
Carefully remove the probe from the probe adjuster assembly.
8.
Close the instrument’s access door.
Removing the IonSABRE APCI probe
6-7
6-8
Optional APCI Mode of Operation
A
Safety Advisories
Waters instruments display hazard symbols designed to alert you to the
hidden dangers of operating and maintaining the instruments. Their
corresponding user guides also include the hazard symbols, with
accompanying text statements describing the hazards and telling you
how to avoid them. This appendix presents all the safety symbols and
statements that apply to the entire line of Waters products.
Contents
Topic
Page
Warning symbols
A-2
Caution symbol
A-5
Warnings that apply to all Waters instruments
A-6
Electrical and handling symbols
A-13
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.
Task-specific hazard warnings
The following warning symbols alert you to risks that can arise when you
operate or maintain an instrument or instrument component. Such risks
include burn injuries, electric shocks, ultraviolet radiation exposures, and
others.
When the following symbols appear in a manual’s narratives or procedures,
their accompanying text identifies the specific risk and explains how to avoid
it.
Warning: (General risk of danger. When this symbol appears on an
instrument, consult the instrument’s user documentation for
important safety-related information before you use the instrument.)
Warning: (Risk of burn injury from contacting hot surfaces.)
Warning: (Risk of electric shock.)
Warning: (Risk of fire)
Warning: (Risk of needle puncture.)
Warning: (Risk of injury caused by moving machinery.)
Warning: (Risk of exposure to ultraviolet radiation.)
Warning: (Risk of contacting corrosive substances.)
Warning: (Risk of exposure to a toxic substance.)
A-2
Safety Advisories
Warning: (Risk of personal exposure to laser radiation.)
Warning: (Risk of exposure to biological agents that can pose a serious
health threat.)
Warnings that apply to particular instruments, instrument
components, and sample types
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.
Warning: Pressurized nonmetallic, or polymer, tubing can burst.
Observe these precautions when working around such tubing:
• Wear eye protection.
• Extinguish all nearby flames.
• Do not use tubing that is, or has been, stressed or kinked.
• Do not expose nonmetallic tubing to incompatible compounds like
tetrahydrofuran (THF) and nitric or sulfuric acids.
• Be aware that some compounds, like methylene chloride and
dimethyl sulfoxide, can cause nonmetallic tubing to swell, which
significantly reduces the pressure at which the tubing can rupture.
Mass spectrometer flammable solvents warning
This warning applies to instruments operated with flammable solvents.
Warning: Where significant quantities of flammable solvents are
involved, a continuous flow of nitrogen into the ion source is required
to prevent possible ignition in that enclosed space.
Ensure that the nitrogen supply pressure never falls below 690 kPa
(6.9 bar, 100 psi) during an analysis in which flammable solvents are
used. Also ensure a gas-fail connection is connected to the HPLC
system so that the LC solvent flow stops if the nitrogen supply fails.
Warning symbols
A-3
Mass spectrometer shock hazard
This warning applies to all Waters mass spectrometers.
Warning: To avoid electric shock, do not remove the mass
spectrometer’s protective panels. The components they cover are not
user-serviceable.
This warning applies to certain instruments when they are in Operate mode.
Warning: High voltages can be present at certain external surfaces of
the mass spectrometer when the instrument is in Operate mode. To
avoid non-lethal electric shock, make sure the instrument is in
Standby mode before touching areas marked with this high voltage
warning symbol.
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.
Warning: Waters instruments and software can be used to analyze or
process potentially infectious human-sourced products, inactivated
microorganisms, and other biological materials. To avoid infection with
these agents, assume that all biological fluids are infectious, observe
good laboratory practices and, consult your organization’s biohazard
safety representative regarding their proper use and handling. Specific
precautions appear in the latest edition of the US National Institutes
of Health (NIH) publication, Biosafety in Microbiological and
Biomedical Laboratories (BMBL).
A-4
Safety Advisories
Chemical hazard warning
This warning applies to Waters instruments that can process corrosive, toxic,
flammable, or other types of hazardous material.
Warning: Waters instruments can be used to analyze or
process potentially hazardous substances. To avoid injury
with any of these materials, familiarize yourself with the
materials and their hazards, observe Good Laboratory
Practices (GLP), and consult your organization’s safety
representative regarding proper use and handling.
Guidelines are provided in the latest edition of the National
Research Council's publication, Prudent Practices in the
Laboratory: Handling and Disposal of Chemicals.
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.
Caution: To avoid damage, do not use abrasives or solvents to clean the
instrument’s case.
Caution symbol
A-5
Warnings that apply to all Waters instruments
When operating this device, follow standard quality control procedures and
the equipment guidelines in this section.
Attention: Changes or modifications to this unit not expressly approved by
the party responsible for compliance could void the user’s authority to operate
the equipment.
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.
Achtung: Jedwede Änderungen oder Modifikationen an dem Gerät ohne die
ausdrückliche Genehmigung der für die ordnungsgemäße
Funktionstüchtigkeit verantwortlichen Personen kann zum Entzug der
Bedienungsbefugnis des Systems führen.
Avvertenza: eventuali modifiche o alterazioni apportate a questa unità e
non espressamente approvate da un ente responsabile per la conformità
annulleranno l’autorità dell’utente ad operare l’apparecchiatura.
Atencion: cualquier cambio o modificación efectuado en esta unidad que no
haya sido expresamente aprobado por la parte responsable del cumplimiento
puede anular la autorización del usuario para utilizar el equipo.
A-6
Safety Advisories
Warning: Use caution when working with any polymer tubing under
pressure:
• Always wear eye protection when near pressurized polymer tubing.
• Extinguish all nearby flames.
• Do not use tubing that has been severely stressed or kinked.
• Do not use nonmetallic tubing with tetrahydrofuran (THF) or concentrated
nitric or sulfuric acids.
• Be aware that methylene chloride and dimethyl sulfoxide cause
nonmetallic tubing to swell, which greatly reduces the rupture pressure of
the tubing.
Attention: Manipulez les tubes en polymère sous pression avec precaution:
• Portez systématiquement des lunettes de protection lorsque vous vous
trouvez à proximité de tubes en polymère pressurisés.
• Eteignez toute flamme se trouvant à proximité de l’instrument.
• Evitez d'utiliser des tubes sévèrement déformés ou endommagés.
• Evitez d'utiliser des tubes non métalliques avec du tétrahydrofurane
(THF) ou de l'acide sulfurique ou nitrique concentré.
• Sachez que le chlorure de méthylène et le diméthylesulfoxyde entraînent le
gonflement des tuyaux non métalliques, ce qui réduit considérablement
leur pression de rupture.
Vorsicht: Bei der Arbeit mit Polymerschläuchen unter Druck ist besondere
Vorsicht angebracht:
• In der Nähe von unter Druck stehenden Polymerschläuchen stets
Schutzbrille tragen.
• Alle offenen Flammen in der Nähe löschen.
• Keine Schläuche verwenden, die stark geknickt oder überbeansprucht
sind.
• Nichtmetallische Schläuche nicht für Tetrahydrofuran (THF) oder
konzentrierte Salpeter- oder Schwefelsäure verwenden.
• Durch Methylenchlorid und Dimethylsulfoxid können nichtmetallische
Schläuche quellen; dadurch wird der Berstdruck des Schlauches erheblich
reduziert.
Warnings that apply to all Waters instruments
A-7
Attenzione: prestare attenzione durante l’utilizzo dei tubi di polimero
pressurizzati:
• Indossare sempre occhiali da lavoro protettivi nei pressi di tubi di polimero
pressurizzati.
• Estinguere ogni fonte di ignizione circostante.
• Non utilizzare tubi soggetti che hanno subito sollecitazioni eccessive o son
stati incurvati.
• Non utilizzare tubi non metallici con tetraidrofurano (THF) o acido
solforico o nitrico concentrato.
• Tenere presente che il cloruro di metilene e il dimetilsolfossido provocano
rigonfiamento nei tubi non metallici, riducendo notevolmente la resistenza
alla rottura dei tubi stessi.
Advertencia: se recomienda precaución cuando se trabaje con tubos de
polímero sometidos a presión:
• El usuario deberá protegerse siempre los ojos cuando trabaje cerca de
tubos de polímero sometidos a presión.
• Si hubiera alguna llama las proximidades.
• No se debe trabajar con tubos que se hayan doblado o sometido a altas
presiones.
• Es necesario utilizar tubos de metal cuando se trabaje con
tetrahidrofurano (THF) o ácidos nítrico o sulfúrico concentrados.
• Hay que tener en cuenta que el cloruro de metileno y el sulfóxido de
dimetilo dilatan los tubos no metálicos, lo que reduce la presión de ruptura
de los tubos.
A-8
Safety Advisories
Warnings that apply to all Waters instruments
A-9
Warning: The user shall be made aware that if the equipment is used in a
manner not specified by the manufacturer, the protection provided by the
equipment may be impaired.
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.
Vorsicht: Der Benutzer wird darauf aufmerksam gemacht, dass bei
unsachgemäßer Verwenddung des Gerätes unter Umständen nicht
ordnungsgemäß funktionieren.
Attenzione: l’utente deve essere al corrente del fatto che, se
l’apparecchiatura viene usta in un modo specificato dal produttore, la
protezione fornita dall’apparecchiatura potrà essere invalidata.
Advertencia: el usuario deberá saber que si el equipo se utiliza de forma
distinta a la especificada por el fabricante, las medidas de protección del
equipo podrían ser insuficientes.
A-10
Safety Advisories
Warning: To protect against fire hazard, replace fuses with those of the same
type and rating.
Attention: Remplacez toujours les fusibles par d’autres du même type et de
la même puissance afin d’éviter tout risque d’incendie.
Vorsicht: Zum Schutz gegen Feuergefahr die Sicherungen nur mit
Sicherungen des gleichen Typs und Nennwertes ersetzen.
Attenzione: per una buona protezione contro i rischi di incendio, sostituire i
fusibili con altri dello stesso tipo e amperaggio.
Advertencia: sustituya los fusibles por otros del mismo tipo y características
para evitar el riesgo de incendio.
Warnings that apply to all Waters instruments
A-11
Warning: To avoid possible electrical shock, disconnect the power cord before
servicing the instrument.
Attention: Afin d’éviter toute possibilité de commotion électrique,
débranchez le cordon d’alimentation de la prise avant d’effectuer la
maintenance de l’instrument.
Vorsicht: Zur Vermeidung von Stromschlägen sollte das Gerät vor der
Wartung vom Netz getrennt werden.
Attenzione: per evitare il rischio di scossa elettrica, scollegare il cavo di
alimentazione prima di svolgere la manutenzione dello strumento.
Precaución: para evitar descargas eléctricas, desenchufe el cable de
alimentación del instrumento antes de realizar cualquier reparación.
A-12
Safety Advisories
Electrical and handling symbols
Electrical symbols
These can appear in instrument user manuals and on the instrument’s front
or rear panels.
Electrical power on
Electrical power off
Standby
Direct current
Alternating current
Protective conductor terminal
Frame, or chassis, terminal
Fuse
Recycle symbol: Do not dispose in municipal waste.
Electrical and handling symbols
A-13
Handling symbols
These handling symbols and their associated text can appear on labels affixed
to the outer packaging of Waters instrument and component shipments.
Keep upright!
Keep dry!
Fragile!
Use no hooks!
A-14
Safety Advisories
B
External Connections
This appendix describes the detector’s external connections.
Warning: The detector is heavy. To avoid injury, Waters
recommends that the detector be lifted using suitable machinery
and the supplied harness.
Caution:
• Contact Waters Technical Service before moving the
instrument.
• If you must transport the detector, or remove it from service,
contact Waters Technical Service for recommended cleaning,
flushing, and packaging procedures.
See “Safety and handling” on page 5-5.
Contents
Topic
Page
Detector 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-25
I/O signal connectors
B-26
Connecting to the electricity source
B-31
B-1
Detector external wiring and vacuum connections
The rear panel connections for a 3100 detector system are shown below.
Detector rear panel
1
2
3
4
5
6
ACN 065444751
7
8
9
10
Analog
Out
Stop Flow
2
4
5
Out
Ground
Switch 2
1
3
Ground
Not used
Out
6
7
8
9
10
In
Inject Start
Ground
In
Event
Switch 3
Out
Ground
Switch 4
Out
Serial Number
Nitrogen inlet
Event inputs
and outputs
RS 232
API Gas
6.9 Bar Maximum
Power cord
Shielded
Ethernet
ETHERNET
V ~ 200 - 240
Hz 50 - 60
VA 900
!
Roughing pump
relay switch
PUMP
SOURCE
VENT
Source vent
Turbo vacuum
VACUUM
VACUUM
Source
vacuum
Waters Corporation
34 Maple Street Milford, MA 01757 U.S.A.
TP02591
B-2
External Connections
Connecting the oil-filled roughing pump
Note: To connect the alternative dry roughing pump, see “Connecting the
oil-free roughing pump” on page B-10.
Exhaust port flange
Oil filler plug
Oil-level sight glass
TP02689
Drain plug
Gas ballast valve
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)
Connecting the oil-filled roughing pump
B-3
To connect the roughing pump
Warning: The pump and its connections can be
contaminated with biohazardous and/or toxic materials.
Always wear chemical-resistant, powder-free gloves when
performing this procedure.
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:
Left side minimum clearance
is 15.24 cm (6 inches)
Back side minimum clearance
is 15.24 cm (6 inches)
TP02689
Front side minimum clearance
is 35.56 cm (14 inches)
Right side minimum clearance
is 15.24 cm (6 inches)
Requirement: The pump must be oriented in a way that allows easy
daily access to the gas ballast valve and oil-level sight glass.
1.
Place the PTFE drip tray on the floor, within 5 feet of the instrument.
Warning: The roughing pump is heavy. To avoid injury, at least
two people must lift the pump.
2.
B-4
Place the pump on the PTFE drip tray.
External Connections
3.
Attach the NW25 tee, included in the startup kit, to the inlet of the
pump using the NW25 center ring, and then secure the connection with
a clamp.
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 detector’s rear panel.
Secure the hose ends with clamps supplied in the startup kit; install 2
clamps on each hose end.
Connecting the oil-filled roughing pump
B-5
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).
6.
Connect an approximately 36.4-cm (2.5-inch) length of 12.7-mm clear
PVC exhaust tubing to the roughing pump exhaust port NW25 nozzle
fitting. Secure the tubing with a hose clamp.
Caution: To prevent condensation from draining backward and
damaging the pump, the exhaust tubing must be installed with
an exhaust trap bottle; the bottle must be positioned at or below
the roughing pump exhaust port.
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
Exhaust trap bottle
TP02800
B-6
External Connections
Caution: To avoid gas leaks, use the sharp knife to cut the PVC
exhaust tubing squarely (that is, perpendicular to its horizontal
axis).
8.
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.
9.
Secure the exhaust trap bottle in a conspicuous location.
Caution: The instrument requires two separate exhaust systems:
one for nitrogen, the other for the roughing pump. Vent them to
atmosphere through separate exhaust lines. Oil mist can
seriously damage the instrument if the nitrogen exhaust line
connects with the roughing pump exhaust line. Your warranty
does not cover damage caused by routing exhaust lines
incorrectly.
10. Route the open end of the exhaust tubing to a suitable exhaust vent.
11. Check the oil level in the pump.
Caution: To ensure correct operation of the roughing pump, do
not operate the pump with the oil level at less than 30% of the
MAX level.
See “Checking the roughing pump oil level” on page 5-23, and, if needed,
“Adding oil to the roughing pump” on page 5-23.
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.
Connecting the oil-filled roughing pump
B-7
Making the electrical connections for a roughing pump with an
external relay box
Roughing pump connections with an external relay box
Detector rear panel
1
2
3
4
5
6
ACN 065444751
7
8
9
10
Analog
Out
Ground
Stop Flow
2
4
5
Out
Ground
Switch 2
1
3
Not used
Out
6
7
8
9
10
Inject Start
In
Ground
Event
Switch 3
In
Out
Ground
Switch 4
Out
Serial Number
Roughing pump main
power connector
RS 232
API Gas
6.9 Bar Maximum
ETHERNET
V ~ 200 - 240
Hz 50 - 60
VA 900
!
PUMP
SOURCE
VENT
VACUUM
VACUUM
Waters Corporation
34 Maple Street Milford, MA 01757 U.S.A.
Relay box
To power source
To make the electrical connections for a roughing pump with an external
relay box
1.
B-8
Connect the power cable from the roughing pump relay box connector to
the relay box.
External Connections
2.
Connect the relay cable from the relay box to the pump connector on the
detector’s rear panel.
3.
Connect the relay box power connector to the main power source.
Making the electrical connections for a roughing pump without an
external relay box
Roughing pump connections without an external relay box
Detector rear panel
1
2
3
4
5
6
ACN 065444751
7
8
9
10
Analog
Out
Stop Flow
2
4
5
Out
Ground
Switch 2
1
3
Ground
Not used
Out
6
7
8
9
10
Inject Start
In
Ground
Event
Switch 3
In
Out
Ground
Switch 4
Out
Serial Number
Roughing pump d.c. connector
Roughing pump main
power connector
RS 232
API Gas
6.9 Bar Maximum
ETHERNET
V ~ 200 - 240
Hz 50 - 60
VA 900
!
PUMP
SOURCE
VENT
VACUUM
VACUUM
Waters Corporation
34 Maple Street Milford, MA 01757 U.S.A.
To power source
Connecting the oil-filled roughing pump
B-9
To make the electrical connections for a roughing pump without an external
relay box
1.
Connect the roughing pump power cord to the main power source.
2.
Connect the relay cable from the roughing pump d.c. connector to the
pump connector on the detector’s rear panel.
Connecting the oil-free roughing pump
The oil-free roughing pump is an optional alternative to the standard oil-filled
roughing pump. To connect the oil-filled roughing pump, see “Connecting the
oil-filled roughing pump” on page B-3.
The noise reduction cover must be installed over the pump to minimize
operating noise, unless the pump is installed in a cabinet that includes sound
dampening and ventilation.
Exhaust port
flange
Noise reduction
cover
Inlet flange
TP02995
Required materials:
B-10
•
Chemical-resistant, powder-free gloves
•
7-mm nut driver
•
8-mm Allen wrench
External Connections
•
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)
•
NW25 full nipple (included in the Alcatel pump kit)
•
DN25 reducing nipple (included in the Alcatel pump kit)
•
NW40 center rings (included in the Alcatel pump kit)
•
NW40 clamps (included in the Alcatel pump kit)
•
DN40 full nipple flange (included in the Alcatel pump 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)
•
Isolation valve (included in the Alcatel pump kit)
•
External silencer (included in the Alcatel pump kit)
•
Noise reduction cover (included in the Alcatel pump kit)
To install the noise reduction cover
1.
Remove the clamp and blank flange from the pump inlet.
2.
Attach the DN40 nipple to the top of the inlet filter and o-ring assembly
and then secure the connection with a clamp.
3.
Attach the DN25 nipple to the outlet fitting and secure the connection
with a clamp.
4.
Connect the gray pump control cable to the rear of the pump.
Connecting the oil-free roughing pump
B-11
5.
Connect the power cord to the rear of the pump.
6.
Install the noise reduction cover.
DN 25 nipple
DN 40 nipple
Clamps
TP02996
B-12
External Connections
To connect the oil-free roughing pump
Warning: The pump and its connections can be
contaminated with biohazardous and/or toxic materials.
Always wear chemical-resistant, powder-free gloves when
performing this procedure.
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:
Left side minimum clearance
is 15.24 cm (6 inches)
Back side minimum clearance
is 15.24 cm (6 inches)
TP02995
Front side minimum clearance
is 35.56 cm (14 inches)
Right side minimum clearance
is 15.24 cm (6 inches)
.
Warning: The roughing pump is heavy. To avoid injury, at least
two people must lift the pump.
1.
Place the pump on the floor, within 1.5 m (5 feet) of the instrument.
Connecting the oil-free roughing pump
B-13
2.
Attach the isolation valve, NW25 tee, and elbows to the DN40 nipple on
the pump inlet, and then secure these connections with clamps, as
shown in the figure below.
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. 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 detector’s rear panel.
Secure the hose ends by installing 2 clamps supplied in the startup kit
on each hose end.
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.
B-14
Attach the DN25 elbow to the DN25 nipple on the pump exhaust outlet
and secure the connection with a clamp.
External Connections
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. Secure the tubing
with a hose clamp.
Caution: To prevent condensation from draining backward and
damaging the pump, the exhaust tubing must be installed with
an exhaust trap bottle; the bottle must be positioned at or below
the roughing pump exhaust port.
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).
External silencer
Exhaust port
TP02997
Elbow
Exhaust trap bottle
TP02800
TP02996
Connecting the oil-free roughing pump
B-15
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.
B-16
External Connections
Making the electrical connections for an oil-free roughing pump
Roughing pump connections
Detector rear panel
1
2
3
4
5
6
ACN 065444751
7
8
9
10
Analog
Out
Stop Flow
2
4
5
Out
Ground
Switch 2
1
3
Ground
Not used
Out
6
7
8
9
10
Inject Start
In
Ground
Event
Switch 3
In
Out
Ground
Switch 4
Out
Serial Number
RS 232
API Gas
6.9 Bar Maximum
ETHERNET
Roughing pump
control cable
V ~ 200 - 240
Hz 50 - 60
VA 900
!
PUMP
SOURCE
VENT
VACUUM
VACUUM
Waters Corporation
34 Maple Street Milford, MA 01757 U.S.A.
To power source
To make the electrical connections for a oil-free roughing pump
1.
Route the cables through the opening in the rear of the noise reduction
cover.
2.
Connect the gray pump control cable to the pump connector on the
detector’s rear panel.
3.
Connect the power cable and power-on the instrument.
Connecting the oil-free roughing pump
B-17
Connecting to the nitrogen gas supply
Required materials:
•
Chemical-resistant, powder-free gloves
•
Sharp knife
•
Wrench
•
6-mm PTFE tubing (included in the Waters Rough Pump Connect Kit)
To connect the nitrogen gas supply
Caution: To avoid gas leaks, use the sharp knife to cut the PTFE
tubing squarely (that is, perpendicular to its horizontal axis).
B-18
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.
External Connections
Nitrogen gas supply, and exhaust connections
1
2
3
4
5
6
ACN 065444751
7
8
9
10
Analog
Out
Stop Flow
2
4
5
Out
Ground
Switch 2
1
3
Ground
Not used
Out
6
7
8
9
10
In
Inject Start
Ground
In
Event
Switch 3
Out
Ground
Switch 4
Out
Serial Number
Nitrogen inlet
RS 232
API Gas
6.9 Bar Maximum
ETHERNET
V ~ 200 - 240
Hz 50 - 60
VA 900
!
PUMP
SOURCE
VENT
Source vent
Turbo vacuum
VACUUM
VACUUM
Source
vacuum
Waters Corporation
34 Maple Street Milford, MA 01757 U.S.A.
TP02591
5.
Attach a nitrogen regulator (not provided) to the nitrogen supply.
6.
Install the 6-mm stud into the regulator outlet.
7.
Connect the free end of the long piece of 6-mm PTFE tubing to the 6-mm
stud.
Connecting to the nitrogen gas supply
B-19
Connecting the nitrogen exhaust line
Required materials:
•
Chemical-resistant, powder-free gloves
•
Sharp knife
•
10-mm and 12-mm PTFE tubing (included in the Waters Rough Pump
Connect Kit)
•
snoop® (or equivalent) leak detector liquid
To connect the nitrogen exhaust line
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: The instrument requires two separate exhaust systems: one
for nitrogen, the other for the roughing pump. Vent them to
atmosphere through separate exhaust lines. Oil mist can seriously
damage the instrument if the nitrogen exhaust line connects with the
roughing pump exhaust line. Your warranty does not cover damage
caused by routing exhaust lines incorrectly.
1.
B-20
Locate the exhaust trap bottle in an accessible area below the
instrument. See the figure “Exhaust trap bottle” on page B-22.
External Connections
Caution: To avoid gas leaks, use the sharp knife to cut the PTFE
tubing squarely (that is, perpendicular to its horizontal axis).
2.
Cut a length of 12-mm tubing long enough to connect the instrument to
the exhaust trap bottle.
3.
Connect one end of the tubing to the exhaust port on the rear panel.
Connect the other end to one of two ports on the exhaust trap bottle.
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.
Warning: To confirm the integrity of the source exhaust
system, the following leak test must be performed.
Caution: To avoid damage to the instrument, snoop (or its
equivalent) leak detector liquid must be used only for the
purpose described in the following step. It must not be used on
any other part of the instrument.
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.
Connecting the nitrogen exhaust line
B-21
Exhaust trap bottle
From instrument
exhaust connection
(12-mm OD)
B-22
External Connections
To laboratory
exhaust port
(10-mm OD)
Connecting the liquid waste line
Required material: Chemical-resistant, powder-free gloves
To connect the liquid waste line
Warning: The waste line and connection can be contaminated
with biologically hazardous materials. Always wear
chemical-resistant, powder-free gloves while performing this
procedure.
1.
Place a suitable waste container below the detector.
Caution: To avoid distorting the drip tray or causing the drain
cup to leak, restrain the drain cup when attaching or removing
the waste line.
2.
Slide a drain line over the barbed fitting of the drain (located at the
bottom of the detector).
Drain cup
Barbed fitting
TP02684
Drain line
Connecting the liquid waste line
B-23
Warning: To prevent leakage of biologically hazardous
materials, ensure that the
• drain line does not crimp or bend. A crimp or bend can
impede flow to the waste container.
• waste container is emptied before the lower end of the
drain tube is covered by waste solvent.
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.
Positioning of drain tube
Correct
Incorrect
TP01807
B-24
External Connections
Connecting the workstation
Before connecting the workstation to the instrument, set up the workstation
according to its accompanying instructions. Locate the workstation within
5 meters (16 feet) of the instrument.
Requirement: Shielded network cables must be used with the detector to
ensure compliance with FCC limits.
To connect the workstation
1.
Connect the monitor to the PC.
2.
Connect one end of the shielded network cable to the appropriate port on
the rear panel of the detector.
3.
Connect the other end of the shielded network cable to the port labeled
instrument LAN on the workstation rear panel.
To connect the instrument to the power source
Caution: Do not connect the instrument’s power supply cord until you
complete the installation procedures in the previous sections.
1.
Select the correct power cord for your location.
2.
Connect the female end of the power cord to the power port on the rear
panel of the instrument.
Connecting Ethernet cables
Requirement: Shielded Ethernet cables must be used with the detector to
ensure compliance with FCC limits.
To make Ethernet connections
1.
Connect one end of one shielded Ethernet cable to the network switch,
and then connect the other end to the Ethernet card on the
preconfigured workstation.
Tip: On preconfigured systems, the Ethernet card is identified as the
Instrument LAN card.
Connecting the workstation
B-25
2.
Connect one end of the other shielded Ethernet cable to the back of the
detector, and then connect the other end to the network switch.
I/O signal connectors
Warning: To avoid electric shock, all electrical connections to the rear
panel must be separated from hazardous voltages by double or
reinforced insulation. Circuits of this type are classified as safety extra
low voltage (SELV). Examples of circuits that are typically SELV
include contact closure inputs and outputs for auto-samplers, and UV,
RI, and fluorescence detector signal outputs for LC/MS systems. The
electrical connections on the rear panel of this mass spectrometer are
all SELV.
To avoid electric shock and damage to the instrument, do not apply
more than
• ±30 V d.c. to the Analog (Out) connection.
• 30 V d.c. to the Stop Flow (Out), Inject Start (In), Switch 2 (Out),
Switch 3 (Out), and Switch 4 (Out) connections.
The detector’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.
B-26
External Connections
I/O signal connectors
Connector I
1 +
2 −
3
4
5
6
7
8
9
10
Analog (Out)
Analog (Out)
Ground
Not Used
Not Used
Stop Flow (Out)
Stop Flow (Out)
Ground
Switch 2 (Out)
Switch 2 (Out)
Connector II
1
2
3
4
5
6
7
8
9
10
+
−
+
−
+
−
+
−
Inject Start (In)
Inject Start (In)
Ground
Event (In)
Event (In)
Switch 3 (Out)
Switch 3 (Out)
Ground
Switch 4 (Out)
Switch 4 (Out)
I/O signal connectors
B-27
Signal connections
Detector analog-out/event-in connections
Signal connections
Description
Analog (Out)
Used for analog chart output functionality. The
output voltage range is 0 to 2 V. The resolution of
the voltage output is 12 bits.
Stop Flow (Out)
Used to stop the solvent flow if the nitrogen gas
supply fails. Maximum 30 V, 0.5 A, 10 W.
Inject Start (In)
Signals the start of an injection. Maximum 30 V.
Event (In)
Allows an external device to start data acquisition.
Maximum 30 V.
Switch 2 (Out)
Used to send time-based contact closure signals to
external devices. Maximum 30 V, 0.5 A, 10 W.
Switch 3 (Out)
Used to send time-based contact closure signals to
external devices. Maximum 30 V, 0.5 A, 10 W.
Switch 4 (Out)
Used to send time-based contact closure signals to
external devices. Maximum 30 V, 0.5 A, 10 W.
Requirement: To meet the regulatory requirements of immunity from
external electrical disturbances, you must install connection covers over the
signal connectors.
To make signal connections
1.
B-28
Reference the signal connection location from the silk-screened label for
inject start or any other input/output connection you plan to use from
Connector I or II on the rear panel of each instrument.
External Connections
2.
To make the signal connections, attach the positive and negative leads of
the signal cable to the connector.
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
I/O signal connectors
B-29
5.
Insert the connector with the signal cable into the connection cover, and
position the clamp over the cable leads. Tighten the clamp into place
with the second self-tapping screw.
Cable leads
Clamp
TP02587
6.
Place the second connection cover over the first cover, and snap it into
place.
Signal connector
Connection cover
TP02588
B-30
External Connections
Connecting to the electricity source
The detector requires a separate, grounded electricity source. The ground
connection in the electrical outlet must be common and connected near the
system.
To connect to the electricity source
Recommendation: Use a line conditioner or an uninterruptible power supply
(UPS) for optimum long-term input voltage stability.
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 detector.
2.
Connect the male end of the detector power cord to a suitable 200 to
240 V a.c. wall outlet.
3.
Connect the power cord from the roughing pump relay box to a 200 to
240 V a.c. wall outlet.
The system software controls electrical power to the pump.
Connecting to the electricity source
B-31
B-32
External Connections
C
Materials of Construction and
Compliant Solvents
Warning: To confirm the integrity of the source exhaust
system, you must address any safety issues raised by the
contents of this Appendix.
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.
Items exposed to solvent
The items that appear in the following table can be exposed to solvent. You
must evaluate the safety issues if the solvents used in your application differ
from the solvents normally used with these items. See “Solvents used to
prepare mobile phases” on page C-3 for details about the most common
ingredients used to prepare mobile phases.
Items exposed to solvent
C-2
Item
Material
Autotune reservoirs
High-density polyethylene
Corona discharge pin mounting
contact
PEEK™
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
®
Materials of Construction and Compliant Solvents
Items exposed to solvent
Item
Material
Trap bottle
Polypropylene
Trap bottle push-in fittings
Nitrile butadiene rubber, stainless
steel, polybutylene terephthalate,
and polyoxymethylene
Solvents used to prepare mobile phases
These solvents are the most common ingredients used to prepare mobile
phases for reverse-phase LC/MS (API):
•
Water
•
Methanol
•
Acetonitrile
•
Formic acid (<0.1%)
•
Acetic acid (<0.1%)
•
Trifluoroacetic acid (<0.1%)
•
Ammonium acetate (<10 mM)
•
Ammonium formate (<10 mM)
These solvents are not expected to cause any problems with the materials
identified in “Items exposed to solvent” on page C-2.
Solvents used to prepare mobile phases
C-3
C-4
Materials of Construction and Compliant Solvents
D
Preparing Samples for LC/MS
System Check with Empower
software
This appendix describes the procedure for preparing a sulfadimethoxine
standard for use with the LC/MS System Check projects supplied for
Empower software.
Contents:
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 detector.
•
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.
Preparing the sulfadimethoxine standard
The target mass of sulfadimethoxine on the HPLC column is 100 pg. Because
the supplied LC/MS System Check methods specify an injection volume of
10 µL, you must prepare a 10 pg/µL sulfadimethoxine solution.
To dilute the stock solutions to the final standard concentration:
1.
Pour 1 mL of the stock solution into one of the 100-mL volumetric flasks.
2.
Dilute to the 100 mL mark with solvent.
Result: The flask contains a 10 ng/µL sulfadimethoxine solution.
3.
Into a second 100-mL volumetric flask, pour 1 mL of the solution created
in step 2.
4.
Dilute to the 100 mL mark with solvent.
Result: The flask contains a 100 pg/µL sulfadimethoxine solution.
5.
Into the 10-mL volumetric flask, pour 1 mL of the solution created in
step 4.
6.
Dilute to the 10 mL mark with solvent.
Result: The flask contains the 10 pg/µL sulfadimethoxine standard
solution.
D-2
Preparing Samples for LC/MS System Check with Empower software
Storing the solutions
Store each of the solutions in an appropriate container. Waters recommends
using the following sample bottles:
•
For the stock solution, a 15-mL sample bottle.
•
For the 10 ng/µL solution, a 125-mL sample bottle.
•
For the 100 pg/µL solution, a 125-mL sample bottle.
•
For the final sulfadimethoxine standard solution, a 15-mL sample
bottle.
Using the solution in an LC/MS System Check run
The final sulfadimethoxine standard solution is ready for use in an LC/MS
System Check run with the Empower software.
To use the solution in an LC/MS System Check run:
1.
Pour 1 mL of the sulfadimethoxine standard solution into the 2-mL
sample vial.
2.
If you use an Alliance HPLC system, place the vial in position 1. If you
use an Alliance High Throughput System, place the vial in position 1:A,1
of a 48-vial tray.
3.
Run LC/MS System Check, as described in the detector’s online Help.
Storing the solutions
D-3
D-4
Preparing Samples for LC/MS System Check with Empower software
Index
Numerics
3100 detector
overview 1-2
A
air filter
cleaning
behind source probe 5-95
inside door 5-91
inside lower bezel 5-93
replacing
behind source probe 5-97
inside door 5-92
inside lower bezel 5-94
Alliance HPLC system D-3
analog signal connection B-28
APCI 1-5, 6-2
APCI probe
cleaning tip 5-4, 5-65
installing 6-3
replacing capillary 5-4, 5-65
replacing heater 5-4, 5-74
APPI 1-6
assembling
cone gas assembly 5-32
probe adjuster 5-89
source enclosure 5-89
source ion block assembly 5-46
B
biohazard warning A-4
burst warning A-3
C
cables, network B-25
calibrating 2-4
calibration, guidelines vii
caution symbol A-5
checking, roughing pump oil level 5-3,
5-23, 5-100
chemical hazard warning A-5
cleaning
air filter
behind source probe 5-95
inside door 5-91
inside lower bezel 5-93
APCI probe tip 5-4, 5-65
corona pin 5-4, 5-73
ESI probe tip 5-3, 5-57
extraction cone 5-35
gas cone 5-25, 5-29
hexapole assembly 5-51, 5-52
instrument case 5-3, 5-10
ion block 5-35
isolation valve 5-35
sample cone 5-25, 5-29
source components 5-3, 5-25
source hexapole assembly 5-53
clearances, roughing pump B-4, B-13
closing source isolation valve 5-7
combined position, of fluidics system
diverter valve 2-10
comments ii
complete shutdown 2-13
compliant solvents C-1
cone gas assembly
assembling 5-32
disassembling 5-28
handling guidelines 5-32
connecting
electricity source B-31
Ethernet B-25
exhaust trap bottle B-7, B-16
Index-1
liquid waste line B-23
nitrogen exhaust B-20
nitrogen supply B-18
NW25 tee B-5, B-14
relay box B-8
roughing pump B-3, B-10
signal connections B-28
vacuum B-2
workstation B-25
construction materials C-1
contamination, preventing C-2
corona pin
cleaning 5-4, 5-73
installing 3-7
mounting contact blanking plug
installing 3-10
removing 3-6
removing 3-9
replacing 5-4, 5-73
covers, for signal connectors B-28
customer comments ii
D
demister element, replacing 5-4, 5-101
detector
calibrating 2-4
compliant solvents C-1
door air filter 5-91
external wiring B-2
I/O signal connectors B-26
materials of construction C-1
operate LED 2-5
power LED 2-5
preparing for working on the source
5-6
rear panel B-2
rebooting 2-11
signal connectors B-26
specifications 1-2
Index-2
starting 2-2
tuning 2-4
vacuum connections B-2
verifying state of 2-4
disassembling
cone gas assembly 5-28
ion block assembly 5-37
probe adjuster 5-84
source enclosure 5-84
diverter valve positions 2-8
door glass, tightening guidelines 5-88
drain tube positioning B-24
drip tray, installing 2-6
E
electrical symbols A-13
electricity source, connecting B-31
electrospray ionization 1-5
emergency shutdown 2-14
emptying
exhaust trap bottle 5-3, 5-15
liquid trap bottle 5-3, 5-16
equipment guidelines vii, 6
error messages, viewing 2-4
ESCi 1-5
ESI probe
capillary, replacing 5-3, 5-58
installing 3-2
removing 3-11
tip
cleaning 5-3, 5-57
replacing 5-57
Ethernet, connecting B-25
event signal connection B-28
exhaust system
checking for leaks 5-16, B-21
requirements B-20
exhaust systems, separation of B-7,
B-20
exhaust trap bottle B-22
connecting B-7, B-16
emptying 5-3, 5-15
experiment methods 4-7
external connections B-1
extraction cone
cleaning 5-35
handling guidelines 5-43
extraction tool, cone gas assembly 5-28
F
fans 2-14
flammable solvents v, A-3
flow path diagrams 2-8
flow states 1-12, 1-13
fluidics system
diverter valve positions
combined 2-10
home 2-8
infusion 2-9
LC 2-9
waste 2-10
operating from Instrument Console
1-10, 1-11
operating from sample list 1-11
operating from Tune window 1-11
G
gas ballasting, roughing pump 5-3,
5-20
gas cone, cleaning 5-25, 5-29
guidelines
calibration vii
demister element nut tightening
5-105
door glass tightening 5-88
probe adjuster screw tightening
5-89
quality control viii
thumbscrew tightening 5-89
H
handling
extraction cone 5-43
hexapole assembly 5-52, 5-55 I
waste liquid 5-16
handling symbols A-14
hazards
flammable solvents v
high temperature v
high voltage vi
solvent leakage iv
heater cartridge assembly
replacing 5-77
hexapole assembly
cleaning 5-51, 5-52
handling 5-52, 5-55
high temperature hazard v
high voltage hazard vi
home position, of fluidics system
diverter valve 2-8
I
I/O signal connectors B-26
in vitro diagnostic applications vii
infusion position, of fluidics system
diverter valve 2-9
infusion syringe, purging 2-11
inject start signal connection B-28
inlet, overview 1-7
installing
APCI probe 6-3
APCI probe sample capillary 5-69
corona pin 3-7
corona pin mounting contact
blanking plug 3-10
drip tray, solvent manifold 2-6
ESI probe 3-2
low-volume vials 2-7
reservoir bottles 2-7
Index-3
solvent manifold drip tray 2-6
instrument
case, cleaning 5-3, 5-10
LAN card B-25
set-up parameters 4-3
shutdown 2-13
Instrument Console, operating fluidics
system from 1-10, 1-11
integral reservoirs 1-3, 1-9
IntelliStart
configuring 2-4
operating 1-10
overview 1-3, 1-9
intended use vii
ion block
cleaning 5-35
disassembling 5-37
grub screw 5-48
heater cartridge assembly,
replacing 5-77
removing 5-35
ion optics 1-6
ionization modes 3-2
APCI 1-5, 6-1
APPI 1-6
ESI 1-4
IonSABRE APCI probe 6-2
IP addresses 2-2
isolating source from instrument 5-7
isolation valve, cleaning 5-35
IVD authorized representative ix
L
LAN card B-25
LC, position of fluidics system diverter
valve 2-9
LC/MS System Check D-1
leaks, checking for 5-16, 5-63, 5-70,
B-21
Index-4
LED
monitoring 2-4
operate 2-5
power 2-2, 2-5
status 2-2
liquid trap bottle, emptying 5-3, 5-16
liquid waste line, connecting B-23
lower bezel air filter
cleaning 5-93
replacing 5-94
low-volume vials, installing 2-7
M
maintenance
safety 5-5
schedule 5-3
mass spectrometer shock hazard A-4
MassLynx software 1-4
materials of construction C-1
mobile phases, solvents used in
preparation of C-3
mode
scanning 1-7
selected ion recording 1-7
monitoring, system instrument LEDs
2-4
MS operating modes 1-7
multi-mode ESCi source 1-2
N
network cables B-25
nitrogen
exhaust, connecting B-20
supply
connecting B-18
pressure requirements v, 2-2
NW25 tee, connecting B-5, B-14
O
oil, roughing pump
adding 5-24
changing 5-4
checking level 5-3, 5-23, 5-100
replacing 5-98
opening source isolation valve 5-8
operate LED 2-5
operating modes, MS 1-7
operating source isolation valve 5-7
O-ring removal kit 5-9
O-rings, removing 5-9
overview 1-2
P
PEEK terminal block, removing 5-40,
5-79
photomultiplier detection system 1-6
power LED 2-2, 2-5
power supply, connecting to B-25
powering-on 2-2
precipitation of salts, preventing 2-12
pressure test, performing 5-81, 5-91
preventing contamination C-2
probe adjuster
assembling 5-89
disassembling 5-84
probe capillary
replacing 5-4
pump, gas ballasting 5-3
purging infusion syringe 2-11
Q
quality control guidelines viii
R
rear panel B-2
rebooting detector 2-11
relay box, connecting B-8
removing
APCI probe sample capillary 5-65
corona pin 3-9
corona pin mounting contact
blanking plug 3-6
ESI probe 3-11
ion block assembly 5-35
I
O-rings 5-9
PEEK terminal block 5-40, 5-79
seals 5-9
replacement parts 5-5
replacing
air filter
behind source probe 5-97
inside door 5-92
inside lower bezel 5-94
APCI probe heater 5-4, 5-74
corona pin 5-4, 5-73
demister element 5-4, 5-101
ESI probe capillary 5-3, 5-58
ESI probe tip 5-57
ion block heater cartridge assembly
5-77
sample capillary 5-65
source assembly seals 5-4, 5-81
requirements
exhaust system B-20
nitrogen supply pressure v, 2-2
reservoir bottles, installing 2-7
reservoirs, integral 1-3, 1-9
reset button 2-11
roughing pump 1-7
clearances B-4, B-13
connecting B-3, B-10
gas ballasting 5-3, 5-20
oil
adding 5-24
checking level 5-3, 5-23, 5-100
replacing 5-98
replacing demister element 5-4,
5-101
setting up B-4, B-13
Index-5
site requirements B-4, B-13
S
safety advisories A-1
safety procedures, maintenance 5-5
salts, preventing precipitation of 2-12
sample 5-65
sample bottles D-3
sample capillary, replacing 5-65
sample cone, cleaning 5-25, 5-29
sample inlet, overview 1-7
sample tune 4-6
scan speed 1-2
scanning mode 1-7
seals, removing 5-9
selected ion recording (SIR) mode 1-7
shutdown
complete 2-13
emergency 2-14
signal connections, connecting B-28
site requirements, roughing pump B-4,
B-13
solvent leakage hazard iv
solvent manifold drip tray, installing
2-6
solvent vapor leakage, avoiding 5-81
solvents
compliant C-1
exposure of detector components to
C-2
use in mobile phases C-3
source
cleaning 5-3, 5-25
enclosure
assembling 5-89
disassembling 5-84
seals, replacing 5-81
hexapole assembly
cleaning 5-53
Index-6
ion block assembly, assembling
5-46
isolation valve
closing 5-7
opening 5-8
operating 5-7
preparing for work on 5-6
pressure test 5-91
replacing assembly seals 5-4
types 1-2
source probe air filter
cleaning 5-95
replacing 5-97
spare parts 5-5
specifications 1-2
standby mode 2-13
starting, detector 2-2
status LED 2-2
stop flow signal connection B-28
sulfadimethoxine standard D-1
switch signal connection B-28
symbols
caution A-5
electrical A-13
handling A-14
warning A-2
system
set-up 4-2
verification 4-10
System QC 4-10
T
thumbscrews, tightening 5-89
tightening
demister element nut 5-105
thumbscrews 5-89
trademarks ii
trap bottle
connecting B-22
emptying 5-15
Tune window, operating fluidics
system from 1-11
tuning 2-4
turbomolecular pump 1-7, 2-13
I
V
vacuum
connections B-2
system 1-7
valve
diverter 2-8
source isolation 5-7
venting, automatic 2-13
W
warning symbols A-2, A-6
waste
bottle, emptying 5-16
line, connecting B-23
liquid, handling 5-16
waste position, of fluidics system
diverter valve 2-10
wiring, external B-2
workstation, connecting B-25
Z
ZSpray source 1-2
Index-7
Index-8
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