Agilent Technologies 7010 Series User manual

Agilent Technologies
Agilent 7000/7010
Series Triple Quadrupole
Operating Manual

2 7000/7010 Series TQ GC/MS Operating Manual
Notices
© Agilent Technologies, Inc. 2017
No part of this manual may be reproduced in
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tronic storage and retrieval or translation
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ment and written consent from Agilent
Technologies, Inc. as governed by United
States and international copyright laws.
Manual Part Number
G7003-90046
Edition
Second edition, July 2017
Printed in USA
Agilent Technologies, Inc.
5301 Stevens Creek Boulevard
Santa Clara, CA 95051
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in future editions. Further, to the max-
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Safety Notices
CAUTION
A CAUTION notice denotes a
hazard. It calls attention to an
operating procedure, practice, or
the like that, if not correctly
performed or adhered to, could
result in damage to the product or
loss of important data. Do not
proceed beyond a CAUTION notice
until the indicated conditions are
fully understood and met.
WARNING
A WARNING notice denotes a
hazard. It calls attention to an
operating procedure, practice, or
the like that, if not correctly
performed or adhered to, could
result in personal injury or death.
Do not proceed beyond a
WARNING notice until the
indicated conditions are fully
understood and met.

7000/7010 Series TQ GC/MS Operating Manual 3
Contents
1 Introduction
Abbreviations Used 12
The 7000/7010 Series TQ GC/MS 14
7000/7010 CI MS System 15
TQ GC/MS Hardware Description 16
Important Safety Warnings 17
Hydrogen Safety 19
Safety and Regulatory Certifications 22
Intended Use 26
Cleaning/Recycling the Product 26
Accidental Liquid Spill 26
Moving or Storing the MS 26
2 Installing 7890 GC Columns
Columns 28
To Install a Capillary Column in a Split/Splitless Inlet 30
To Condition a Capillary Column 33
To Install a Capillary Column in the GC/MS Interface Using the Self
Tightening Column Nut 34
To Install a Capillary Column in the GC/MS Interface Using a
Standard Column Nut 39
To Install the Interface Tip Seal 42
The GC/MS Interface for a 7890 Series GC 44
To Calibrate the Column 46

4 7000/7010 Series TQ GC/MS Operating Manual
3 Intuvo 9000 GC Column Maintenance
Columns 50
Conditioning Intuvo columns 51
Tips and hints 51
Handling the Intuvo 9000GC Column and Bus Components 52
To Replace an Intuvo GC Column 53
To Replace an Intuvo 9000 GC Gasket 57
To Install a Column Guard or Jumper Chip 58
To Replace the 9000 GC/MS Tail 62
To Condition an Intuvo Capillary Column 66
To Install the Interface Tip Seal 68
The GC/MS Interface for a 9000 Series GC 69
4 Operating in EI Mode
Operating the MS from the Data System 72
Set the IP Address and View TQ Parameters with the WUI 73
To change the network settings of the TQ 73
Front Panel Instrument Status LED 77
Before You Turn On the MS 78
Pumping Down 79
Controlling Temperatures 79
Controlling Column Flow 80
Controlling CC Flow 80
Controlling JetClean Hydrogen Flow 80
Venting the MS 81
High Vacuum Pressure in EI Mode 82

7000/7010 Series TQ GC/MS Operating Manual 5
To Set Monitors for MS Temperature and Vacuum Status 83
To Set the MS Analyzer’s Temperatures 85
To Set the GC/MS Interface Temperature from MassHunter 87
To Configure CC Gas 88
To Set the Mode for the Optional JetClean System 89
To Set the JetClean Parameters for the Clean Only Mode 90
To Set the CC Gas Flow Rates 91
To Autotune the MS for EI Mode 92
To Open Left Side Panel for Access to the Analyzer Chambers 94
To Pumpdown the MS 95
To Vent the MS 99
To Set the Interface Temperature from the 7890 GC 101
To Save a Method on the 7890 GC 102
5 Operating in CI Mode
Setting Up Your MS to Operate in CI Mode 104
Operating the CI MS 105
High Vacuum Pressure in CI Mode 106
Other Reagent Gases 107
CI Autotune 109
The CI Flow Control Module 111
To Operate the Reagent Gas Flow Control Module 113
To Set a Reagent Gas Flow 115
To Perform a CI Autotune 116
To Pumpdown and Switch from EI to CI Mode 118

6 7000/7010 Series TQ GC/MS Operating Manual
6 General Maintenance
Before Starting 122
Maintaining the Vacuum System 127
Maintaining the Analyzer 128
To Open the Front Analyzer Chamber 130
To Remove the EI HES 133
To Connect or Disconnect Wiring to the EI HES 135
To Remove the EI XTR Source 136
To Connect or Disconnect Wiring to the EI XTR Source 138
To Disassemble the EI HES 139
To Disassemble the EI XTR Source 142
To Clean the EI HES 145
To Clean the EI XTR Source 148
To Assemble the EI HES 151
To Assemble the EI XTR Source 156
To Install the EI HES 159
To Install the EI XTR Source 161
To Remove a Filament from the EI XTR Source 163
To Install a Filament on the EI XTR Source 165
To Remove the EI HES Filaments 166
To Install the EI HES Filaments 168
To Close the Front Analyzer Chamber 169
To Remove Left Rear Cover 170
To Open the Rear Analyzer Chamber 172
To Replace the EM Horn 175

7000/7010 Series TQ GC/MS Operating Manual 7
To Close the Rear Analyzer Chamber 177
7 CI Maintenance
General Information 180
To set up your MS for CI operation 180
To Switch from an EI XTR Source to the CI Source 181
To Remove the EI HES Radiator 182
To Connect or Disconnect EI HES Radiator Wiring 184
To Install the 7010 Series CI Source 185
To Install the 7000 Series CI Source 186
To Switch from the CI Source to the EI HES 187
To Install the EI HES Radiator 188
To Switch from the CI Source to the EI XTR Source 190
To Connect or Disconnect 7010 Series CI Source Wiring 191
To Connect or Disconnect 7000 Series CI Source Wiring 192
To Switch from the CI Source to an EI XTR Source 193
To Remove the 7000 Series CI Source 194
To Remove the 7010 Series CI Source 195
To Switch from the EI HES to the CI Source 196
To Install the CI/EI XTR Source Radiator 197
To Switch from the CI Source to the EI HES 199
To Install a CI Source Filament 200
To Remove the CI Source Radiator from the 7010 Series TQ 201
To Disassemble the CI Source 203
To Clean the CI Source 206
To Assemble the CI Source 209

8 7000/7010 Series TQ GC/MS Operating Manual
To Remove the CI Source Filament 212
To Install a CI Source Filament 214

7000/7010 Series TQ GC/MS Operating Manual 9
About This Manual
This manual contains information for operating and maintaining the Agilent
7000/7010 Series Triple Quad (TQ) Mass Spectrometer (MS) system.
1 “Introduction”
Chapter 1 describes general information about the 7000/7010 Series TQ
GC/MS, including a hardware description, general safety warnings, and
hydrogen safety information.
2 “Installing 7890 GC Columns”
Chapter 2 shows you how to prepare Agilent 7890 GC capillary columns for
use with the MS, install it in the GC oven, and connect it to the MS using the
GC/MS interface.
3 “Intuvo 9000 GC Column Maintenance”
Chapter 3 shows you how to install an Agilent Intuvo column, connect a flow
path from the column through the MS transfer line and into the ion source,
and maintain the column guard chip.
4 “Operating in EI Mode”
Chapter 4 describes routine operations in EI mode such as setting
temperatures, monitoring pressures, tuning, venting, and pumpdown.
5 “Operating in CI Mode”
Chapter 5 describes additional tasks necessary to operate in CI mode.
6 “General Maintenance”
Chapter 6 describes general maintenance procedures for the 7000/7010 Series
TQ GC/MS.
7 “CI Maintenance”
Chapter 7 describes maintenance procedures unique to CI MS.

10 7000/7010 Series TQ GC/MS Operating Manual
Hardware User Information
Accompanying your hardware and software is a comprehensive collection of
manuals, videos, user applications, and method development tools. These are
located on the:
•Agilent GC and GC/MS User Manuals and Tools DVD set
•Agilent GC/MS Software Information and Manuals memory stick
See the Agilent 7000/7010 Series TQ GC/MS System Quick Start document for
information on finding and installing the documentation located on this USB
and DVDs.
To Install Your Hardware Library
Insert the disk into your DVD drive and follow the prompts.
This can be installed by anyone who has authority to copy
information onto the receiving computer.
To Install Your Software Library
Insert the memory stick into a USB port and follow the prompts.
This can be installed by anyone who has authority to copy
information onto the receiving computer.

11
Agilent 7000/7010 TQ GC/MS
Operating Manual
Agilent Technologies
1
Introduction
Abbreviations Used 12
The 7000/7010 Series TQ GC/MS 14
TQ GC/MS Hardware Description 16
Important Safety Warnings 17
Hydrogen Safety 19
Safety and Regulatory Certifications 22
Intended Use 26
Cleaning/Recycling the Product 26
Accidental Liquid Spill 26
Moving or Storing the MS 26
This section provides general information about the 7000/7010 Series Triple
Quad (TQ) Gas Chromatograph (GC) / Mass Spectrometer (MS), including a
hardware description, general safety warnings, and hydrogen safety
information.

12 7000/7010 Series TQ GC/MS Operating Manual
1Introduction
Abbreviations Used
The abbreviations in Table 1 are used in discussing this product. They are
collected here for convenience.
Table 1 Abbreviations
Abbreviation Definition
AC Alternating current
ALS Automatic liquid sampler
BFB Bromofluorobenzene (calibrant)
CC Collision cell
CI Chemical ionization
CID Collision induced dissociation
CSB Ceramic source board
DC Direct current
DFTPP Decafluorotriphenylphosphine (calibrant)
DIP Direct insertion probe
EI Electron impact
EM Electron multiplier (detector)
EMV Electron multiplier voltage
EPC Electronic pneumatic control
eV Electron volt
GC Gas chromatograph
HED High-energy dynode (refers to detector and its power supply)
HES High Efficiency Source
id Inside diameter
Inert Standard EI source constructed of inert materials
Inert+ MS model equipped with an EI XTR source
LAN Local Area Network

Introduction 1
7000/7010 Series TQ GC/MS Operating Manual 13
LCP Local control panel
m/z Mass to charge ratio
MFC Mass flow controller
MRM Multiple reaction monitoring
MS Mass spectrometer
MS1 Front quadrupole
MS2 Rear quadrupole
NCI Negative chemical ionization
OFN Octafluoronaphthalene (sample)
PCI Positive chemical ionization
PFDTD Perfluoro-5,8-dimethyl-3,6,9-trioxydodecane (calibrant)
PFTBA Perfluorotributylamine (calibrant)
Quad Quadrupole mass filter
RF Radio frequency
RFPA Radio frequency power amplifier
Torr Unit of pressure, 1 mm Hg
TQ Triple Quad (Quadrupole)
Turbo Split flow turbomolecular vacuum pump
XTR EI Extractor source
Table 1 Abbreviations (continued)
Abbreviation Definition

14 7000/7010 Series TQ GC/MS Operating Manual
1Introduction
The 7000/7010 Series TQ GC/MS
The 7000/7010 Series TQ GC/MS is a standalone capillary GC detector for use
with the Agilent 7890 Series GC. (See Figure 1 on page 16.) The TQ GC/MS
features:
•One split flow turbomolecular vacuum pump
•Rotary vane foreline pump
•A choice of two independently MS heated high sensitivity EI sources
•An optional JetClean system for cleaning the ion source in place under
vacuum
•CI and EI modes available (PCI/NCI/EI)
•Two independently MS heated hyperbolic Quads
•Single hexapole CC
•HED EM
•Independently GC heated GC/MS interface with interface tip seal
•Independently GC controlled CC gas flows
Physical description
The 7000/7010 Series TQ GC/MS is a rectangular box, approximately 47 cm
high, 35 cm wide, and 86 cm deep. The weight is 59 kg for the turbo pump
mainframe. The attached foreline (roughing) pump weighs an additional
21.5 kg.
The basic components of the instrument are:
•Frame/cover assemblies
•Vacuum system
•GC/MS interface
•Ion source
•Electronics
•GC
•Detector
•Front and rear analyzers

Introduction 1
7000/7010 Series TQ GC/MS Operating Manual 15
Vacuum gauge
The 7000/7010 Series TQ GC/MS is equipped with two ion vacuum gauges. The
Agilent MassHunter GC/MS Acquisition software can be used to read the
pressure (high vacuum) in the vacuum manifold and at the turbomolecular
vacuum pump discharge.
7000/7010 CI MS System
In this manual, the term “CI MS” refers to the 7000/7010 Series TQ GC/MS CI
source system. It also applies, unless otherwise specified, to the mass flow
controller (MFC) for these instruments.
The 7000/7010 Series TQ GC/MS CI source system upgrade kit adds to the
7000/7010 TQ MS:
•EI/CI GC/MS interface
•CI source
•Reagent gas MFC system
•JetClean option available that shares the same MFC system
•HED with high sensitivity electronics
•Bipolar HED power supply for PCI and NCI operation
A required methane/isobutane gas purifier is provided. It removes oxygen,
water, hydrocarbons, and sulfur compounds.
The CI MS system has been optimized to achieve the relatively high source
pressure required for CI while still maintaining high vacuum in the CC,
quadrupoles, and detector. Special seals along the flow path of the reagent gas
and very small openings in the ion source keep the source gases in the
ionization volume long enough for the appropriate reactions to occur.
The CI interface has special plumbing for reagent gas. A spring-loaded
insulating seal fits onto the tip of the interface.
Switching back and forth between CI and EI sources takes about 1 hour,
however, a 1- to 2-hour wait is required to purge the reagent gas lines and bake
out water and other contaminants. Switching from PCI to NCI requires about
2 hours for the ion source to cool.

16 7000/7010 Series TQ GC/MS Operating Manual
1Introduction
TQ GC/MS Hardware Description
Figure 1 7000/7010 Series TQ GC/MS
ALS
7000/7010 Series
TQ MS
MS power
switch
7890B
series GC
Drawer
GC power switch
Front panel
LED

Introduction 1
7000/7010 Series TQ GC/MS Operating Manual 17
Important Safety Warnings
There are several important safety notices to always keep in mind when using
the MS.
Many internal parts of the MS carry dangerous voltages
If the MS is connected to a power source, even if the power switch is off,
potentially dangerous voltages exist on:
•The wiring between the MS power cord and the AC power supply
•The AC power supply itself
•The wiring from the AC power supply to the power switch
With the power switch on, potentially dangerous voltages also exist on:
•All electronics boards in the instrument
•The internal wires and cables connected to these boards
•The wires for any heater (oven, detector, inlet, or valve box)
Electrostatic discharge is a threat to MS electronics
The printed circuit boards in the MS can be damaged by electrostatic
discharge (ESD). Do not touch any of the boards unless it is absolutely
necessary. If you must handle them, wear a grounded wrist strap and take
other antistatic precautions.
WARNING
All these parts are shielded by covers. With the covers in place, it should be difficult
to accidentally make contact with dangerous voltages. Unless specifically
instructed to, never remove a cover unless the detector, inlet, and oven are turned off.
WARNING
If the power cord insulation is frayed or worn, the cord must be replaced. Contact
your Agilent service representative.

18 7000/7010 Series TQ GC/MS Operating Manual
1Introduction
Many parts are dangerously hot
Many parts of the GC/MS operate at temperatures high enough to cause
serious burns. These parts include, but are not limited to the:
•Inlet
•Oven and its contents
•Valve box
•Detectors
•Column nuts attaching the column to an inlet or detector
•Foreline pump
•GC/MS transfer line
•Quadrupole
•Ion source
Always cool these areas of the system to room temperature before working on them.
They will cool faster if you first set the temperature of the heated zone to room
temperature. Turn the zone off after it has reached the setpoint. If you must perform
maintenance on hot parts, use a wrench and wear gloves. Whenever possible, cool the
part of the instrument that you will be maintaining before you begin working on it.
The oil pan under the foreline pump can be a fire hazard
Oily rags, paper towels, and similar absorbents in the oil pan could ignite and
damage the pump and other parts of the MS.
WARNING
Be careful when working behind the instrument. During cool-down cycles, the GC
emits hot exhaust that can cause burns.
WARNING
The insulation around the inlets, detectors, valve box, and the insulation cups is
made of refractory ceramic fibers. To avoid inhaling fiber particles, we recommend
the following safety procedures: ventilate your work area; wear long sleeves,
gloves, safety glasses, and a disposable dust/mist respirator; dispose of insulation
in a sealed plastic bag in accordance with local regulations; wash your hands with
mild soap and cold water after handling the insulation.
WARNING
Combustible materials (or flammable/nonflammable wicking material) placed
under, over, or around the foreline (roughing) pump constitute a fire hazard. Keep
the pan clean, but do not leave absorbent material such as paper towels in it.

Introduction 1
7000/7010 Series TQ GC/MS Operating Manual 19
Hydrogen Safety
Hydrogen is a commonly used GC carrier gas, detector fuel gas, and reactive
cleaning gas for the optional JetClean system. Hydrogen is potentially
explosive and has other dangerous characteristics.
•Hydrogen is combustible over a wide range of concentrations. At atmospheric
pressure, hydrogen is combustible at concentrations from 4% to 74.2% by volume.
•Hydrogen has the highest burning velocity of any gas.
•Hydrogen has a very low ignition energy.
•Hydrogen that is allowed to expand rapidly from high pressure can self-ignite.
•Hydrogen burns with a nonluminous flame, which can be invisible under
bright light.
Dangers unique to GC/MS operation
Hydrogen presents a number of dangers. Some are general, others are unique
to GC or GC/MS operation. Dangers include, but are not limited to:
•Combustion of leaking hydrogen
•Combustion due to rapid expansion of hydrogen from a high-pressure cylinder
•Accumulation of hydrogen in the GC oven and subsequent combustion. See
your GC documentation and the label on the top edge of the GC oven door.
•Accumulation of hydrogen in the MS and subsequent combustion
WARNING
The use of hydrogen as a GC carrier gas, detector fuel gas, or in the optional
JetClean system, is potentially dangerous.
WARNING
When using hydrogen (H2) as the carrier gas or fuel gas, be aware that hydrogen
gas can flow into the GC oven and create an explosion hazard. Therefore, ensure that
the hydrogen supply is turned off until all connections are made, and ensure that the
inlet and detector column fittings are either connected to a column or capped at all
times when hydrogen gas is supplied to the instrument.
Hydrogen is flammable. Leaks, when confined in an enclosed space, may create a
fire or explosion hazard. In any application using hydrogen, leak test all
connections, lines, and valves before operating the instrument. Always turn off the
hydrogen supply at its source before working on the instrument.

20 7000/7010 Series TQ GC/MS Operating Manual
1Introduction
Hydrogen accumulation in an MS
All users should be aware of the mechanisms by which hydrogen can
accumulate, and know what precautions to take if they are certain or suspect
that hydrogen has accumulated. (See Table 2.) Note that these mechanisms
apply to all MSs.
WARNING
The MS cannot detect leaks in inlet or detector gas streams. For this reason, it is
vital that column fittings should always be either connected to a column or have a
cap or plug installed.
WARNING
The MS cannot detect leaks in the valves for the optional JetClean system. It is
possible that hydrogen can leak into the MS from this cleaning system. Always turn
off the JetClean system and close the manual hydrogen shutoff valve to the JetClean
MFC and ensure good vacuum before venting the MS.
Table 2 Hydrogen accumulation mechanisms
Mechanism Results
MS turned off A MS can be shut down deliberately. It can also be shut down accidentally by an
internal or external failure. A MS shutdown does not shut off the flow of carrier gas. As
a result, hydrogen may slowly accumulate in the MS.
MS automated shutoff
valves closed
The MSs are equipped with automated shutoff valves for the calibration vial, optional
JetClean system, and the reagent gases. Deliberate operator action or various failures
can cause the shutoff valves to close. Shutoff valve closure does not shut off the flow of
carrier gas. As a result, hydrogen may slowly accumulate in the MS.
GC off A GC can be shut down deliberately. It can also be shut down accidentally by an internal
or external failure. Different GCs react in different ways. If a 7890 Series GC equipped
with Electronic Pressure Control (EPC) is shut off, the EPC stops the flow of carrier gas.
If the carrier flow is not under EPC control, the flow increases to its maximum. This flow
may be more than some MSs can pump away, resulting in the accumulation of hydrogen
in the MS. If the MS is shut off at the same time, the accumulation can be fairly rapid.
Power failure If the power fails, both the GC and MS shut down. The flow of carrier gas, however, is
not necessarily shut down. As described previously, in some GCs a power failure may
cause the carrier gas flow to be set to maximum. As a result, hydrogen may accumulate
in the MS.