HP 5973 User manual

H
Hardware Manual
HP 5973
Mass Selective Detector

© Copyright 1998
Hewlett-Packard Company
All Rights Reserved.
Reproduction, adaptation, or
translation without prior
written permission is
prohibited, except as allowed
under the copyright laws.
Document History
Publication number
G1099-90027
First edition, 11/98
Printed in USA
Warranty
The information contained in
this document is subject to
change without notice.
Hewlett-Packard makes no
warranty of any kind with
regard to this material,
including, but not limited to,
the implied warranties of
merchantability and fitness for
a particular purpose.
Hewlett-Packard shall not be
liable for errors contained
herein or for incidental or
consequential damages in
connection with the furnishing,
performance or use of this
material.
Hewlett-Packard assumes no
responsibility for the use or
reliability of its software on
equipment that is not
furnished by Hewlett-Packard.
Instrument
Identification
Each HP 5973 Mass Selective
Detector (MSD) is identified
by a unique 10-character serial
number. This serial number is
located on a label on the lower
left side near the front of the
instrument. On CI upgrades, a
serial number is located on the
flow module.
When corresponding with
Hewlett-Packard about your
instrument, be sure to include
the model number and both
full 10-character serial
numbers.
Write the serial number of your
HP 5973 MSD here for
reference:
MSD serial #:
________________________
HP 5973 MSD version
HP 5973 MSDs are equipped
with either a diffusion pump or
a turbomolecular (turbo)
pump. Chemical Ionization is
available for the turbo MSD
only. The serial number label
displays a product number that
tells what kind of MSD you
have:
G1098A = Diffusion pump
G1099A = Turbo pump
G1999A = CI (turbo pump)
Noise Declaration
Deutsch
LpA << 70 dB am Arbeitsplatz
normaler Betrieb nach EN
27779:1991
English
LpA << 70 dB operator
position normal operation per
ISO 7779:1988
Manual Conventions
Cautions
Cautions call attention to
procedures which, if not
correctly performed or
adhered to, could result in
damage to the instrument.
Warnings
Warnings call attention to
procedures which, if not
correctly performed or
adhered to, could result in
personal injury.
Part Numbers
In this manual, Hewlett-
Packard part numbers are
generally listed in parentheses
after the name of the part or in
tables in the Parts chapter.
Most Hewlett-Packard part
numbers are either four-digit-
by-four-digit (1234-1234)
numbers or five-digit-by-five-
digit (12345-12345) numbers.
A few tools and supplies listed
have no part numbers and are
not available from Hewlett-
Packard. Most of these can be
obtained from laboratory
supply companies.
Safety Information
Safety Symbols
(on equipment)
Safety class
The HP 5973 Mass Selective
Detector (MSD) is a Safety
Class I instrument and has
been designed and tested in
accordance with IEC
Publication 1010-1 Safety
Requirements for Electrical
Equipment for Measurement,
Control, and Laboratory Use.
WAR NI NG
Connecting an MSD to a power
source which is not equipped
with a protective earth contact
creates a shock hazard for the
operator and can damage the
instrument. Likewise,
interrupting the protective
conductor inside or outside the
MSD or disconnecting the
protective earth terminal
creates a shock hazard for the
operator and can damage the
instrument.
WAR NI NG
Make sure that only fuses with
the required current rating and
of the specified type are used
for replacement. The use of
incorrect or makeshift fuses or
the short-circuiting of fuse
holders creates a shock hazard
for the operator and can
damage the instrument.
WAR NI NG
Any adjustment, maintenance
or repair of the opened
instrument while it is
connected to a power source
should be avoided if possible
and, if required, should be
carried out only by trained
persons who are aware of the
hazards involved.
Safety Information is contin-
ued on the inside of the back
cover.
;Refer to operating
instructions
=Indicates hazardous
voltage
+Indicates hot surface
3Indicates earth
(ground) terminal

HP 5973
Mass Selective Detector
Hardware Manual

4
The HP 5973 Mass Selective Detector
The HP 5973 MSD is a stand-alone capillary GC detector
The HP 5973 Mass Selective Detector (MSD) is designed for use with the
HP 6890 Series Gas Chromatograph. The MSD features:
• Either a 90 L/sec vapor-diffusion or a 250 L/sec turbomolecular
high vacuum pump
• Rotary vane foreline pump
• Independently heated electron-ionization ion source
• Independently heated hyperbolic quadrupole mass filter
• High-energy dynode (HED) electron multiplier detector
• Independently heated GC/MSD interface
• Power supplies and instrument control electronics
Operator control of the MSD is through the data system
The data system features Hewlett-Packard MSD ChemStation software.
It includes programs to calibrate (tune) the MSD, acquire data, and analyze
data.
Tuning programs adjust voltages in the ion source, calibrate mass assign-
ments, and control the scanning of the analyzer.
Data acquisition programs allow you to monitor the total ion chromato-
gram (TIC), automatically storing the mass spectra of GC peaks as they
elute. This is the scan mode. Alternatively, you can monitor the concentra-
tions of particular ions. This is selected ion monitoring mode (SIM).
Data analysis programs allow you to integrate chromatograms (TIC or
SIM), view and manipulate mass spectral data, compare spectra to databas-
es of reference spectra in a library search, quantitate data, and generate
reports.

The HP 5973 Mass Selective Detector
5
An optional gauge controller is available for measuring vacuum
The HP 5973 MSD is equipped with a triode gauge tube. With an HP 59864B
Gauge Controller, the tube can be used to measure pressure (high vacuum)
in the vacuum manifold. Installation and operation of the gauge controller is
described in this manual.
The gauge controller is required for chemical ionization (CI) operation.
HP 6890 Series
Gas Chromatograph
HP 5973
Mass Selective Detector

6
In This Manual
This manual describes the operation, troubleshooting, and maintenance of
the HP 5973 Mass Selective Detector. Chapters 1 – 4 describe common
operation, troubleshooting, and maintenance tasks. Chapters 5 – 8 contain
reference material about the major systems of the MSD. Chapter 9 is a parts
reference.
• Chapter 1 shows you how to prepare and install a capillary column.
• Chapter 2 describes basic tasks such as setting temperatures, monitoring
pressures, tuning, and venting, and pumpdown.
• Chapter 3 provides a quick reference for identifying causes of poor
instrument performance or malfunctions.
• Chapter 4 features maintenance procedures.
• Chapter 5 describes operation of the components of the vacuum system.
• Chapter 6 describes the GC/MSD interface.
• Chapter 7 describes operation of the ion source, mass filter, and detector.
• Chapter 8 describes the electronics that control the MSD.
• Chapter 9 contains illustrated parts identification and part numbers.
To report errors in this manual, please send e-mail to [email protected]p.com.
For updated information, check the HP Chemical Analysis web site at
http://chem.external.hp.com/cag/main.html.
HP 5973 Mass Selective Detector Reference Collection
The two CD-ROM set includes the following multimedia resources:
• Hardware maintenance procedures for the HP 5973 MSD and
HP 6890 Series GC
• Software tutorial: hands-on training
• Mass Spectrometer Fundamentals: Mass spectrometer hardware, and
Acquiring and evaluating (mass) spectra

7
Table of Contents
Chapter 1 Installing GC Columns
To prepare a capillary column for installation, 20
To install a capillary column in a split/splitless inlet, 22
To condition a capillary column, 24
To install a capillary column without the installation tool, 26
To install a capillary column using the installation tool, 28
Chapter 2 Operating the MSD
To view MSD analyzer temperature and vacuum status, 36
To set monitors for MSD temperature and vacuum status, 38
To set the MSD analyzer temperatures, 40
To set the interface temperature from the ChemStation, 42
To monitor high vacuum pressure, 44
To measure column flow linear velocity, 46
To calculate column flow, 47
To tune the MSD, 48
To set the interface temperature from an HP 6890 GC, 49
To remove the MSD covers, 50
Upper MSD cover, 50
Lower MSD cover, 50
To vent the MSD, 52
To open the vacuum manifold, 54
To close the vacuum manifold, 56
To pump down the MSD, 58
To connect the optional gauge controller, 60
To move or store the MSD, 62
To vent the MSD without the ChemStation, 64

8
Contents
Chapter 3 Troubleshooting the MSD
General symptoms, 68
GC does not turn on, 68
MSD does not turn on, 68
Foreline pump is not operating, 68
Fan for the high vacuum pump is not operating, 69
MSD is on but the status LEDs are all blinking, 69
MSD turns on but then the foreline pump shuts off, 69
Chromatographic symptoms, 70
No peaks, 70
Passes tune, 70
Does not pass tune, 71
Peaks are tailing, 71
Peaks are fronting, 71
Peaks have flat tops, 72
Peaks have split tops, 72
Baseline is rising, 72
Baseline is high, 72
Baseline is falling, 72
Baseline wanders, 73
Retention times for all peaks drift – shorter, 73
Retention times for all peaks drift – longer, 73
Poor sensitivity, 74
Poor Repeatability, 74
Mass spectral symptoms, 75
Isotopes are missing or isotope ratios are incorrect, 75
High background, 75
High abundances at m/z 18, 28, 32, and 44 or at m/z 14 and 16, 75
Mass assignments are incorrect, 76
Peaks have precursors, 76
Peak widths are inconsistent, 76
Relative abundance of m/z 502 is less than 3%, 77
Spectra look different from those acquired with other HP MSDs, 77
High mass sensitivity is poor, 78
Pressure symptoms, 79
Foreline pressure is too high, 79
Vacuum manifold pressure is too high, 79
Foreline pressure is too low, 80
Vacuum manifold pressure is too low, 80
Gauge controller displays 9.9+9 and then goes blank, 80
Power indicator on the gauge controller does not light, 81

Contents
9
Temperature symptoms, 82
Ion source will not heat up, 82
Mass filter (quad) heater will not heat up, 83
GC/MSD interface will not heat up, 83
Error messages, 84
Difficulty in mass filter electronics, 84
Difficulty with the electron multiplier supply, 84
Difficulty with the fan, 85
Difficulty with the HED supply, 85
Difficulty with the high vacuum pump, 85
Diffusion pump, 85
Turbomolecular pump, 86
Foreline pressure has exceeded 300 mTorr, 86
Internal MS communication fault, 86
Lens supply fault, 86
Log amplifier ADC error, 86
No peaks found, 86
Temperature control disabled, 87
Temperature control fault, 87
The high vacuum pump is not ready, 87
The system is in standby, 87
The system is in vent state, 88
There is no emission current, 88
There is not enough signal to begin tune, 88
Air leaks, 89
Contamination, 90

10
Contents
Chapter 4 Maintaining the MSD
Before starting 94
Maintaining the vacuum system 101
To check and add foreline pump oil, 102
To drain the foreline pump, 104
To refill the foreline pump, 106
To replace the oil trap, 108
To check the diffusion pump fluid, 110
To separate the MSD from the GC, 112
To remove the diffusion pump, 114
To replace the diffusion pump fluid, 116
To reinstall the diffusion pump, 118
To reconnect the MSD to the GC, 120
To remove the calibration vial, 122
To refill and reinstall the calibration vial, 124
To remove the foreline gauge, 126
To reinstall a foreline gauge, 128
To remove the calibration valve, 130
To reinstall a calibration valve, 132
To replace the fan for the high vacuum pump, 134
To remove the triode gauge tube, 136
To reinstall a triode gauge tube, 138
To lubricate the side plate O-ring, 140
To lubricate the vent valve O-ring, 142
Maintaining the analyzer 144
To remove the ion source, 146
To disassemble the ion source, 148
To clean the ion source, 150
To reassemble the ion source, 154
To reinstall the ion source, 156
To remove a filament, 158
To reinstall a filament, 160
To remove the heater and sensor from the ion source, 162
To reinstall the heater and sensor in the ion source, 164
To remove the heater and sensor from the mass filter, 166
To reinstall the heater and sensor in the mass filter, 168
To replace the electron multiplier horn, 170

Contents
11
Maintaining the GC/MSD interface 172
To remove the GC/MSD interface heater and sensor, 173
To reinstall the GC/MSD interface heater and sensor, 175
Maintaining the electronics 177
To adjust the RF coils, 179
To replace the primary fuses, 181
Chapter 5 Vacuum System
Diffusion pump MSD vacuum system, 186
Turbo pump MSD vacuum system, 187
Diffusion pump vacuum manifold, 188
Turbo pump vacuum manifold, 189
Side plate, 190
Vacuum seals, 192
Face seals, 192
KF (NW) seals, 192
Compression seals, 192
High voltage feedthrough seal, 193
Foreline pump, 194
Foreline gauge, 196
Diffusion pump and fan, 198
Turbomolecular pump and fan, 202
Calibration valve and vent valve, 204
Calibration valve, 204
Vent valve, 204
Triode gauge tube, 206
Gauge controller, 208
Chapter 6 GC/MSD Interface

12
Contents
Chapter 7 Analyzer
Ion source, 218
Ion source body, 218
Filaments, 219
Filament selection, 219
Emission current, 220
Electron energy, 220
Filament care, 221
Magnet, 221
Repeller, 221
Drawout plate and cylinder, 222
Ion focus, 222
Entrance lens, 222
Entrance lens offset, 222
Entrance lens gain, 222
Mass filter, 223
AMU gain, 223
AMU offset, 224
219 width, 224
DC polarity, 225
Mass (axis) gain, 225
Mass (axis) offset, 225
Quadrupole maintenance, 226
Detector, 227
Detector focus lens, 227
High energy dynode, 227
Electron multiplier horn, 227
Analyzer heaters and radiators, 230

Contents
13
Chapter 8 Electronics
Side board, 236
Electronics module, 237
Main board, 238
Signal amplifier board, 239
HP-IB/MS control card, 240
AC board, 241
Pumpdown safety shutdown, 242
Power supplies, 243
Low voltage (ac-dc) power supply, 243
High voltage (HED) power supply, 243
Toroid transformer, 244
Back panel and connectors, 245
Remote start connector, 245
I/O (HP-IB) connector, 245
HP-IB address switch, 245
High vacuum signal (HIVAC SIGNAL) connector, 246
High vacuum power (HIVAC POWER) connector, 246
Power cord receptacle, 246
Foreline pump power cord receptacle, 246
Primary fuses, 246
Interfacing to external devices, 248
Remote control processor, 248
Remote start signals, 248
System ready, 249
Start run input, 249
Status display and power switch, 250
Power status LED, 250
Analyzer status LED, 250
Cal valve status LED, 250
Power switch, 250
Turbo pump controller, 252

14
Contents
Chapter 9 Parts
Electronics, 256
Vacuum system, 260
Analyzer, 268
GC/MSD interface, 274
Consumables and maintenance supplies, 276

1
Installing GC Columns
How to connect GC columns to the MSD
To prepare a capillary column for installation, 20
To install a capillary column in a split/splitless inlet, 22
To condition a capillary column, 24
To install a capillary column without the installation tool, 26
To install a capillary column using the installation tool, 28

16
Installing GC columns
Before you can operate your GC/MSD system, you must select, condition,
and install a GC column. This chapter will show you how to install and
condition a column. For correct column and flow selection, you must know
what type of vacuum system your MSD has. The serial number tag on the
lower front of the left side panel shows the model number.
Many types of GC columns can be used with the MSD but there are
some restrictions
During tuning or data acquisition the rate of column flow into the MSD
should not exceed 2.0 milliliters per minute for the diffusion pump MSD,
or 4.0 milliliters per minute for the turbomolecular pump MSD. Therefore,
there are limits to column length and flow.
• Narrow-bore columns (0.20 mm id or 0.25 mm id) can be installed
directly into the GC/MSD interface. Do not exceed recommended column
flow.
• Wide-bore columns (0.32 mm id), and megabore columns (0.53 mm id)
at least 100 meters long, can be installed directly into the GC/MSD
interface of the turbo pump MSD. Flow restrictions apply. Wide-bore and
megabore columns cannot be used with the diffusion pump MSD.
This information is summarized in Table 1. The dimensions listed are nomi-
nal values. The velocities and flows listed are calculated values at 70°C.
Actual values can vary from column to column and vary greatly with oven
temperature, unless the electronic pneumatic control (EPC) on the GC is
set for constant flow. See To measure column flow linear velocity
(page 46) for instructions on how to measure actual flow in your column.
0RGHOQXPEHU 9DFXXPV\VWHP 6RIWZDUHYDFXXPPRQLWRU
HP G1098A Diffusion pump Foreline pressure
HP G1099A Turbo pump Turbo speed

1Installing GC Columns
17
Table 1 GC column information
Column diameter
(mm)1Column length
(meters)1Head pressure (psi) Column flow (ml/min)2
0.100 10 100 1.83
0.200 60 58.8 2.0
30 37.3 2.0
15 22.0 2.0
15 30.3 4.0
0.250 60 32.3 2.0
30 18.5 2.0
15 8.8 2.0
15 18.5 4.03
0.32360 25.9 4.03
(wide-bore) 30 14.0 4.03
15 5.6 4.03
0.533100 4.41 4.03
(megabore) 75 1.8544.0
1 Nominal dimensions
2 Calculated values at 70°C with vacuum compensation turned on
3 Acceptable for turbo pump MSD only
4 Notacceptable–flowtoohighorheadpressuretoolowforaccurate
control

18
1Installing GC Columns
Conditioning a column before it is installed into the GC/MSD
interface is essential
A small portion of the capillary column stationary phase is often carried
away by the carrier gas. This is called column bleed. Column bleed deposits
traces of the stationary phase in the MSD ion source. This decreases MSD
sensitivity and makes cleaning of the ion source necessary.
Column bleed is most common in new or poorly cross-linked columns. It is
much worse if there are traces of oxygen in the carrier gas when the column
is heated. To minimize column bleed, all capillary columns should be condi-
tioned before they are installed in the GC/MSD interface.
Conditioning ferrules is also beneficial
Heating ferrules to their maximum expected operating temperature a few
times before they are installed can reduce chemical bleed from the ferrules.
Tips and hints
• Note that the column installation procedure is different from that for all
other Hewlett-Packard mass spectrometers and MSDs. Using the
procedure from another instrument will not work.
• For optimal sensitivity performance, install your caapillary column
without using the installation tool.
• You can remove old ferrules from column nuts with an ordinary push pin.
• Always use carrier gas that is at least 99.999% pure.
• Because of thermal expansion, new ferrules may loosen after heating and
cooling a few times. Check for tightness after two or three heating cycles.
• Always wear clean gloves when handling columns, especially the end that
will be inserted into the GC/MSD interface.

1Installing GC Columns
19
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20
1Installing GC Columns
To prepare a capillary column for installation
To prepare a capillary column for installation
Materials needed: Capillary column
Column cutter (5181-8836)
Ferrules
0.27-mm id, for 0.10-mm id columns (5062-3518)
0.37-mm id, for 0.20-mm id columns (5062-3516)
0.40-mm id, for 0.25-mm id columns (5181-3323)
0.47-mm id, for 0.32-mm id columns (5062-3514)
0.74-mm id, for 0.53-mm id columns (5062-3512)
Gloves, clean
large (8650-0030)
small (8650-0029)
Inlet column nut (5181-8830)
Magnifying glass
Septum (may be old, used inlet septum)
1Slide a septum, column nut, and conditioned ferrule onto the free end of
the column.
The tapered end of the ferrule should point away from the column nut.
2Use the column cutter to score the column 2 cm from the end.
3Break off the end of the column.
Hold the column against the column cutter with your thumb. Break the column
against edge of the column cutter.
4Inspect the end for jagged edges or burrs.
If the break is not clean and even, repeat steps 2 and 3.
5Wipe the outside of the free end of the column with a lint-free cloth
moistened with methanol.