Thermo Scientific TRACE GC Ultra Programming manual

Thermo Scientific
TRACE GC Ultra
Gas Chromatograph
Maintenance and Troubleshooting
Manual
PN 31709180, Revision March 2011
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TRACE™ GC Ultra Maintenance and Troubleshooting Manual
March 2011 Edition “Original Instructions”
Part Number 317 091 80
© 2007-2010 Thermo Fisher Scientific Inc. All rights reserved.
Printed in Italy
Published by Thermo Fisher Scientific S.p.A., Strada Rivoltana, 20090 Rodano - Milan - Italy
Tel: [phone] Fax: [phone]
Printing History: First Edition, released June 1998.
Second Edition, released November 1998.
Third Edition, released June 1999.
Fourth Edition, released June 2001
Fifth Edition, released January 2002
Sixth Edition, released May 2003
Seventh Edition, released April 2004
Eight Edition, released November 2004
Ninth Edition, released September 2005
Tenth Edition, released May 2006
Eleventh Edition, released January 2007
Twelfth Edition, released May 2007
Thirteenth Edition, released July 2008
Fourteenth Edition, released April 2009
Fifteenth Edition, released November 2009
Sixteenth Edition, released May 2010
Seventeenth Edition, released March 2011
Disclaimer
Technical Information contained in this publication is for reference purposes only and is subject to change without notice. Every effort has
been made to supply complete and accurate information; however, Thermo Fisher Scientific assumes no responsibility and will not be liable
for any errors, omissions, damage, or loss that might result from any use of this manual or the information contained therein (even if this
information is properly followed and problems still arise).
This publication is not part of the Agreement of Sale between Thermo Fisher Scientific and the purchaser of a TRACE™ GC Ultra system. In
the event of any conflict between the provisions of this document and those contained in Thermo Fisher Scientific’s Terms and Conditions,
the provisions of the Terms and Conditions shall govern.
Reference to System Configurations and Specifications supercede all previous information and are subject to change without notice.
Trademarks
TRACE™ GC Ultra is a trademark of Thermo Fisher Scientific Inc., and its subsidiaries. Other brand and product names may be trademarks
or registered trademarks of their respective companies.

Maintenance and Troubleshooting Manual iii
Declaration
Manufacturer: Thermo Fisher Scientific
Thermo Fisher Scientific is the manufacturer of the instrument described in this
manual and, as such, is responsible for the instrument safety, reliability and
performance only if:
• installation
• re-calibration
• changes and repairs
have been carried out by authorized personnel and if:
• the local installation complies with local law regulations
• the instrument is used according to the instructions provided and if its opera-
tion is only entrusted to qualified trained personnel
Thermo Fisher Scientific is not liable for any damages derived from the
non-compliance with the aforementioned recommendations.

Maintenance and Troubleshooting Manual v
Contents
About This Manual.................................................................................................................................xi
Overview...................................................................................................................................xi
Conventions Used in This Manual..........................................................................................xiii
Instrument Markings and Symbols .........................................................................................xvi
Using Hydrogen .....................................................................................................................xvii
Using the Hydrogen Sensor .....................................................................................xviii
Chapter 1
Preventive Maintenance.................................................................................................................... 21
Suggested Maintenance Schedule ............................................................................................ 22
Chapter 2
Maintaining a Split/Splitless Injector ............................................................................................... 25
Split/Splitless Injector .............................................................................................................. 26
Split/Splitless Injector Maintenance ........................................................................................ 28
When replacing the septum......................................................................................... 28
When cleaning or replacing the liner .......................................................................... 28
If the glass liner breaks inside the injector.................................................................. 29
When replacing the split line tubing ........................................................................... 29
Chapter 3
Maintaining a Large Volume Splitless Injector ............................................................................... 53
Large Volume Splitless Injector...............................................................................................54
Large Volume Splitless Injector Maintenance......................................................................... 56
When replacing the septum......................................................................................... 56
When cleaning or replacing the liner .......................................................................... 56
If the glass liner breaks inside the injector.................................................................. 57
When replacing the split line tubing ........................................................................... 57
Chapter 4
Maintaining a Cold On-Column Injector for Standard Automatic Injections ............................... 79
Automated Operation Cold On-Column Injector..................................................................... 80
Cold On-Column Injector Maintenance................................................................................... 82
Replace the O-ring ...................................................................................................... 82
Possible leaks in the rotary valve................................................................................ 82
Chapter 5
Maintaining a Cold On-Column Injector Direct Narrow-Bore ........................................................ 97
Automated Operation Cold On-Column Injector..................................................................... 98

vi Maintenance and Troubleshooting Manual
Contents
Cold On-Column Injector Maintenance ................................................................................ 100
Possible leaks in the rotary valve ............................................................................. 100
Chapter 6
Maintaining a Cold On-Column Injector...........................................................................................111
Manual Cold On-Column Injector......................................................................................... 112
Cold On-Column Injector Maintenance ................................................................................ 114
Possible leaks in the rotary valve ............................................................................. 114
Chapter 7
Maintaining a Packed Column Injector ............................................................................................121
Packed Column Injector ........................................................................................................ 122
Packed Column Injector Maintenance................................................................................... 124
When replacing the septum ...................................................................................... 124
Chapter 8
Maintaining a Purged Packed Column Injector ...............................................................................129
Purged Packed Column Injector ............................................................................................ 130
Purged Packed Column Injector Maintenance ...................................................................... 132
When replacing the septum ...................................................................................... 132
When replacing the liner........................................................................................... 132
Chapter 9
Maintaining a PTV Injector ................................................................................................................141
PTV Injector .......................................................................................................................... 142
PTV Injector Maintenance..................................................................................................... 144
When replacing the septum ...................................................................................... 144
When cleaning or replacing the liner........................................................................ 145
If a liner breaks inside the injector ........................................................................... 146
Adjusting the quartz wool packing........................................................................... 146
PTV Troubleshooting ............................................................................................................ 171
Sensitivity ................................................................................................................. 171
Discrimination .......................................................................................................... 171
Large Volume PTV .................................................................................................. 171
Troubleshooting the PTV Injector............................................................................ 172
Chapter 10
Ensuring Tightness............................................................................................................................179
Keeping Leaks under Control................................................................................................ 180

Contents
Maintenance and Troubleshooting Manual vii
DCC-equipped systems............................................................................................. 180
Leak Check ............................................................................................................... 180
Multiple systems .......................................................................................... 188
Chapter 11
Maintaining a FID............................................................................................................................... 191
Flame Ionization Detector (FID)............................................................................................192
FID Maintenance.................................................................................................................... 194
FID Troubleshooting.............................................................................................................. 214
Change in Sensitivity ................................................................................... 214
Gases ............................................................................................................ 214
Flame Ignition.............................................................................................. 215
Contamination.............................................................................................. 217
Chapter 12
Maintaining an Electron Capture Detector ...................................................................................... 219
Electron Capture Detector (ECD) .......................................................................................... 220
ECD Maintenance .................................................................................................................. 222
Wipe Test ............................................................................................................................... 223
Wipe Test Certificate ................................................................................................ 224
ECD Troubleshooting ............................................................................................................235
Change in Sensitivity ................................................................................................235
Temperature ................................................................................................. 235
Gases ............................................................................................................ 235
Contamination........................................................................................................... 236
Troubleshooting the ECD .........................................................................................237
Chapter 13
Maintaining a Nitrogen Phosphorus Detector ................................................................................ 239
Nitrogen Phosphorus Detector (NPD) ...................................................................................240
NPD Maintenance .................................................................................................................. 242
Thermionic source..................................................................................................... 242
NPD Troubleshooting ............................................................................................................264
Sensitivity .................................................................................................... 264
Gases ............................................................................................................ 264
Troubleshooting the NPD .........................................................................................266

viii Maintenance and Troubleshooting Manual
Contents
Chapter 14
Maintaining a Flame Photometric Detector .....................................................................................269
Flame Photometric Detector (FPD)....................................................................................... 270
FPD Maintenance .................................................................................................................. 272
FPD Troubleshooting............................................................................................................. 310
Sensitivity.................................................................................................... 310
Gases............................................................................................................ 310
Troubleshooting the FPD.......................................................................................... 312
Chapter 15
Maintaining a Photoionization Detector...........................................................................................315
Photoionization Detector (PID) ............................................................................................. 316
PID Maintenance ................................................................................................................... 318
Leaks............................................................................................................ 318
PID Troubleshooting ............................................................................................................. 334
Sensitivity ................................................................................................................. 334
Lamp............................................................................................................ 334
Contamination ............................................................................................. 334
Troubleshooting the PID .......................................................................................... 335
Chapter 16
Maintaining a Thermal Conductivity Detector .................................................................................337
Thermal Conductivity Detector (TCD) ................................................................................. 338
TCD Maintenance.................................................................................................................. 340
TCD Troubleshooting............................................................................................................ 341
Sensitivity ................................................................................................................. 341
Baseline drift............................................................................................................. 341
Negative peaks.......................................................................................................... 341
Troubleshooting the TCD......................................................................................... 342
Chapter 17
Maintaining Detectors in Stack Configuration ................................................................................345
ECD adapted for Stack Configuration................................................................................... 346
Guidelines for Maintenance................................................................................................... 348
Troubleshooting Guidelines................................................................................................... 386
Incorrect installation of the column............................................................ 386

Contents
Maintenance and Troubleshooting Manual ix
Chapter 18
Regenerating Carrier and Split Lines Filters................................................................................... 387
Chapter 19
Analytical Troubleshooting............................................................................................................... 391
Appendix A
Customer Communication 401
How To Contact Us................................................................................................................ 401
Reader Survey ........................................................................................................... 402
Appendix B
Reagents Safety Information 403
ACETONE ................................................................................................... 403
METHANOL ............................................................................................... 404
TOLUENE ................................................................................................... 404
Glossary ..............................................................................................................................................405

x Maintenance and Troubleshooting Manual
Contents

Maintenance and Troubleshooting Manual xi
About This Manual
Overview
This manual reports information and operating sequences for the maintenance and
the troubleshooting of the TRACE GC Ultra and its components.
This manual is organized as follows:
Chapter 1, Preventive Maintenance, gives a schedule for preventive maintenance
of your TRACE GC Ultra.
Chapter 2, Maintaining a Split/Splitless Injector, reports information and
maintenance sequences for the Split/Splitless injector.
Chapter 3, Maintaining a Large Volume Splitless Injector, reports information and
maintenance sequences for the Large Volume Splitless injector
Chapter 4, Maintaining a Cold On-Column Injector for Standard Automatic
Injections, reports information and maintenance sequences for the Cold On-
Column injector for TriPlus autosampler.
Chapter 5, Maintaining a Cold On-Column Injector Direct Narrow-Bore, reports
information and maintenance sequences for the Cold On-Column injector for
direct injection into capillary column with the TriPlus autosampler.
Chapter 6, Maintaining a Cold On-Column Injector, reports information and
maintenance sequences for the Cold On-Column injector.
Chapter 7, Maintaining a Packed Column Injector, reports information and
maintenance sequences for the Packed Column injector.
Chapter 8, Maintaining a Purged Packed Column Injector, reports information
and maintenance sequences for the Purged Packed Column injector.
Chapter 9, Maintaining a PTV Injector, reports information and maintenance
sequences for the Programmable Temperature of Vaporization injector.
Chapter 10, Ensuring Tightness, reports instructions for identifying and correcting
leaks.

About This Manual Overview
xii Maintenance and Troubleshooting Manual
Chapter 11, Maintaining a FID, reports information and maintenance sequences
for the Flame Ionization (FID) detector.
Chapter 12, Maintaining an Electron Capture Detector, reports information and
maintenance sequences for the Electron Capture (ECD) detector.
Chapter 13, Maintaining a Nitrogen Phosphorus Detector, reports information
and maintenance sequences for the Nitrogen Phosphorus (NPD) detector.
Chapter 14, Maintaining a Flame Photometric Detector, reports information and
maintenance sequences for the Flame Photometric (FPD) detector.
Chapter 15, Maintaining a Photoionization Detector, reports information and
maintenance sequences for the Photoionization (PID) detector.
Chapter 16, Maintaining a Thermal Conductivity Detector, reports information
and maintenance sequences for the Thermal Conductivity (TCD) detector.
Chapter 17, Maintaining Detectors in Stack Configuration, reports information
and maintenance sequences for detectors if installed in stack configuration.
Chapter 18, Analytical Troubleshooting, is a guide to troubleshoot the instrument
when its analytical response indicates a problem.
Appendix A, Reagents Safety Information, reports chemical safety information
concerning reagents used in the operating sequences.
Appendix B, Customer Communication, contains contact information for Thermo
Fisher Scientific offices worldwide. Use the Reader Survey in this section to give
us feedback on this manual and help us improve the quality of our documentation.
The Glossary contains definitions of terms used in this guide. This also includes
abbreviations, acronyms, metric prefixes, and symbols.

Conventions Used in This Manual About This Manual
Maintenance and Troubleshooting Manual xiii
Conventions Used in This Manual
The following symbols and typographical conventions are used throughout this
manual.
Bold Bold text indicates names of windows, menus, dialog boxes,
buttons, and fields.
Italic Italic indicates cross references, first references to important
terms defined in the glossary, and special emphasis.
Monospace Monospace, or Courier, indicates filenames and filepaths, or
to indicate text the user should enter with the keyboard.
Monospace
Bold
Monospace Bold indicates messages or prompts displayed on
the computer screen or on a digital display.
»This symbol illustrates menu paths to select, such as
File»Open….
KEY NAME Bold, uppercase sans serif font indicates the name of a key on
a keyboard or keypad, such as ENTER.
.CAUTION This symbol alerts you to an action or procedure that, if
performed improperly, could damage the instrument.
NOTE This symbol alerts you to important information related to the
text in the previous paragraph.
WARNING! This symbol alerts you to an action or procedure that, if
performed improperly, could result in damage to the
instrument or possible physical harm to the user. This symbol
may be followed by icons indicating special precautions that
should be taken to avoid injury.
This symbol indicates electric shock hazard.

About This Manual Conventions Used in This Manual
xiv Maintenance and Troubleshooting Manual
This symbol indicates danger from hazardous chemicals.
This symbol indicates danger from high temperature surfaces
or substances.
This symbol indicates a fire hazard.
This symbol indicates an explosion hazard.
This symbol indicates a toxic hazard.
This symbol indicates the presence of flammable materials.
This symbol indicates the presence of radioactive material.
This symbol indicates an operation or procedure that must
NOT be performed by the user. A Thermo Fisher Scientific
authorized Customer Support Engineer must perform this
procedure.
This symbol indicates all metal objects, such as watches and
jewelry, must be taken off.
This symbol indicates an eye hazard. Eye protection must be
worn.
This symbol indicates the user must wear a protective screen
when performing the procedure.

Conventions Used in This Manual About This Manual
Maintenance and Troubleshooting Manual xv
This symbol indicates the user must wear protective shoes
when performing the procedure.
This symbol indicates the user must wear protective clothing
when performing the procedure.
This symbol indicates the user must wear gloves when
performing the procedure.

About This Manual Instrument Markings and Symbols
xvi Maintenance and Troubleshooting Manual
Instrument Markings and Symbols
The following table explains the symbols used on Thermo Fisher Scientific
instruments. Only a few of them are used on the TRACE GC Ultra.
Symbol Description
Direct Current
Alternating Current
Both direct and alternating current
3
Three-phase alternating current
Earth (ground) terminal
Protective conductor terminal
Frame or chassis terminal
Equipotentiality
On (Supply)
Off (Supply)

Using Hydrogen About This Manual
Maintenance and Troubleshooting Manual xvii
Using Hydrogen
The use of hydrogen as a carrier gas or as fuel for certain flame detectors requires
the operator’s strict attention and compliance with special precautions due to the
hazards involved.
Hydrogen is a dangerous gas, particularly in an enclosed area when it reaches a
concentration corresponding to its lower explosion level (4% in volume). When
mixed with air it can create an explosive mixture. An explosion hazard could
develop in the GC oven when hydrogen is used as a carrier gas if oven elements
are not perfectly connected to each other, or if the connection materials are worn
out, broken, or otherwise faulty.
Equipment protected throughout by DOUBLE
INSULATION or REINFORCED INSULATION
(Equivalent to Class II of IEC 536)
Caution, risk of electric shock
Caution, hot surface
Caution (refer to accompanying documents)
In-position of a bistable push control
Out-position of a bistable push control
Symbol in compliance to the Directive 2002/96/EC on
Waste Electrical and Electronic Equipments (WEEE)
placed on the european market after August, 13, 2005.
Symbol Description

About This Manual Using Hydrogen
xviii Maintenance and Troubleshooting Manual
Use the following safety precautions when using hydrogen:
• Ensure that all hydrogen cylinders comply with the safety requirements for
proper use and storage. Hydrogen cylinders and delivery systems must
comply with local regulations.
• Make sure the gas supply is turned completely off when connecting hydrogen
lines.
• Perform a bubble test to ensure that the hydrogen lines are leak-tight before
using the instrument. Perform the bubble test after performing the pressure
test described in the Performing a Manual System Leak Check operating
procedure on page 66 of the Operating Manual.
• Ensure your GC column oven has a hydrogen sensor. A hydrogen sensor con-
tinuously monitors the hydrogen level in the GC column oven.
If your GC oven does not have a hydrogen sensor already installed, contact
your Thermo Fisher Scientific sales representative. To comply with
instrument safety requirements, a Thermo Fisher Scientific CSE or authorized
service technician should install the sensor
If you plan to use a sensor other than the sensor recommended by Thermo
Fisher Scientific, you must verify its ability to perform the functions listed
above before installing it. It must comply with your local safety regulations,
or with the IEC 10101regulations if local regulations do not exist.
Using the Hydrogen Sensor
The lower limit of the hydrogen sensor is 0.5% in volume. You should adjust the
detection threshold to 1% in volume, which is 25% of the hydrogen lower limit of
explosion (4% in volume).
In cases where the connections begin to leak or the column breaks, the sensor
alerts the operator. Then it automatically cuts off the gas supply and heating to the
active zones, and sweeps the column oven with forced air ventilation.
1. IEC 1010-1, First Edition, September 1990; IEC 1010-1, Amendment 1, September 1992; IEC 1010-1, Amendment 2,
June 1995.

Using Hydrogen About This Manual
Maintenance and Troubleshooting Manual xix
If the sensor detects anomalies or leaks during GC operation due to instrument
malfunction, the operator must immediately:
• close the hydrogen supply
• switch off the gas chromatograph
• air out the room
The reliability of the sensor depends on careful maintenance. After the sensor is in
use, you must periodically check its operating performance and calibration as
recommended by the manufacturer. Refer to your hydrogen sensor’s instruction
manual for maintenance guidelines.
WARNING! Never use hydrogen in your TRACE system unless your GC oven has a hydrogen
sensor installed.
NOTE Thermo Fisher Scientific CSEs are not authorized to install or repair any instrument using
hydrogen as a carrier gas unless the instrument is equipped with the appropriate sensor.