Getting Started May 2007.book
Getting Started May 2007.book
Getting Started May 2007.book
TRACE GC Ultra
Gas Chromatograph
Getting Started
PN 31709230, Revision May 2007
HOME
TRACE™ GC Ultra Getting Started
May 2007 Edition
Part Number 317 092 30
© 2007 Thermo Fisher Scientific Inc. All rights reserved.
Printed in Italy
Published by Thermo Electron S.p.A., Strada Rivoltana, 20090 Rodano - Milan - Italy
Tel: +39 02 95059373 Fax: +39 02 95059388
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 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.
Declaration
Manufacturer: Thermo Electron S.p.A.
Thermo Electron S.p.A. 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
Thermo Italia S.p.A. is not liable for any damages derived from the non-
compliance with the aforementioned recommendations.
Chapter 1
Configuring the Instrument .................................................................................................................15
Getting Ready........................................................................................................................... 16
Navigating TRACE GC Ultra Menus ...................................................................................... 18
Viewing a Submenu .................................................................................................... 18
Editing a Menu Item ................................................................................................... 20
Chapter 2
Working with Detectors........................................................................................................................21
Installing Detectors .................................................................................................................. 21
Getting the Most from the Detector ......................................................................................... 23
Chapter 3
Operating the
TRACE GC Ultra....................................................................................................................................25
Setting Up an Analysis............................................................................................................. 26
Example ...................................................................................................................... 27
Injecting a Test Mixture ........................................................................................................... 28
Chapter 4
Automating Your Analyses ..................................................................................................................35
Developing an Analytical Method ........................................................................................... 35
Autosampler Sequence Basics ................................................................................................. 37
Appendix A
Customer Communication...................................................................................................................39
How To Contact Us.................................................................................................................. 39
Reader Survey ............................................................................................................. 40
Glossary ................................................................................................................................................45
Index ......................................................................................................................................................51
Getting Started v
Contents
vi Getting Started
About This Manual
Overview
The TRACE GC Ultra Getting Started manual offers step-by-step instructions for
making your first analysis with the TRACE GC Ultra a success. If you follow the
procedures provided, by the end of the guide you will have:
• checked the TRACE GC Ultra’s software configuration to make sure it
matches the hardware configuration and your purchase order
• installed the detectors, if necessary
• analyzed a standard test mixture
• gained an understanding of the possibilities for automating analyses
This guide is written for users with some experience in gas chromatography. Less
experienced users are encouraged to explore additional sources of information. If
you would like more instruction, ask your customer service representative about
Thermo Fisher Scientific training courses in basic gas chromatography.
WARNING! Before using this guide, you must have already prepared your workspace and installed the
TRACE GC Ultra in accordance with the TRACE GC Ultra Site Preparation and Installation
Manual.
Chapter 1, Configuring the Instrument, explains how to check and modify the
TRACE GC Ultra’s configuration by examining and editing the software menus.
The Glossary contains definitions of terms used in this guide and the help
diskette. This also includes abbreviations, acronyms, metric prefixes, and
symbols.
The Index contains an alphabetical list of key terms and topics in this guide,
including cross-references and the corresponding page numbers.
Getting Started ix
About This Manual Conventions Used in This Manual
x Getting Started
Instrument Markings and Symbols About This Manual
Symbol Description
Direct Current
Alternating Current
Equipotentiality
On (Supply)
Off (Supply)
Getting Started xi
About This Manual Instrument Markings and Symbols
Symbol Description
Equipment protected throughout by DOUBLE
INSULATION or REINFORCED INSULATION
(Equivalent to Class II of IEC 536)
Instruction manual symbol affixed to product. Indicates
that the user must refer to the manual for specific
Warning or Caution information to avoid personal injury
or damage to the product.
Caution, risk of electric shock
The TRACE GC Ultra has been configured to your specifications at the factory.
Now you will check your purchase order against the instrument settings.
Chapter at a Glance…
Getting Ready.......................................................................................................16
Navigating TRACE GC Ultra Menus...................................................................18
Getting Started 15
Chapter 1
Configuring the Instrument Getting Ready
Getting Ready
If a Thermo Fisher Scientific customer service engineer installed your instrument,
your detectors probably have been installed. If not, you will check the
configuration and install the detectors accordingly. For instance, if the LEFT
DETECTOR menu specifies an FID (flame ionization detector), you will install an
FID at the left detector position.
CAUTION Before turning on the TRACE GC Ultra, check to see which detectors were ordered
with your instrument. If an ECD (electron capture detector) will be used, do not turn
on the power until it has been installed. If these detectors are configured but not
installed, the TRACE GC Ultra could shut down. For installation instructions, see
Working with Detectors on page 21.
After the ECD detectors are installed, turn on the power switch.
16 Getting Started
Chapter 1
Getting Ready Configuring the Instrument
Figure 1-1 below shows the TRACE GC Ultra keypad. To check the
configuration, you will use the keypad to call up the appropriate menus.
LEFT
CARRIER
Getting Started 17
Chapter 1
Configuring the Instrument Navigating TRACE GC Ultra Menus
To see the configuration settings for your instrument, press CONFIG. The
CONFIGURATION main menu appears. Each item in the CONFIGURATION main
menu leads to a submenu.
Viewing a Submenu
When you press CONFIG, the CONFIGURATION main menu appears. Use the
following procedure to examine the configuration submenus.
1. Press to move through the menu. The cursor (<) moves as you scroll.
3. To return to the main menu or the next higher level menu, press CLEAR.
Figure 1-2 below shows how the OVEN submenu display might look.
OVEN ↓
Temp 40 40 <
Initial time 0.00
Ramp 1 Off
Table 1-1 shows the CONFIGURATION main menu and explains what to check for.
18 Getting Started
Chapter 1
Navigating TRACE GC Ultra Menus Configuring the Instrument
Getting Started 19
Chapter 1
Configuring the Instrument Navigating TRACE GC Ultra Menus
1. To select a menu item, use the key to scroll through the menu until the
cursor (<) points to the item you want to edit.
2. To display the selected field’s range and options, press the INFO/DIAG key
once. If the field cannot be edited, no information will appear. Press CLEAR to
return to the menu.
• If the field cannot be filled with on/off, yes/no, or a number, press ENTER
or MODE/TYPE to display a submenu of choices. In the submenu, you
might use the keypad, or you might select an item by scrolling with the
arrow keys. While you are editing a numeric field, a blinking asterisk (*)
appears to the right of the menu item.
4. When you have entered the proper information in the field, press ENTER to
load the new setpoint. The blinking asterisk disappears and the cursor
advances to the next menu item.
5. Use the key to scroll to the next item you want to edit.
20 Getting Started
Working with Detectors
2
This chapter explains how to install a detector on the TRACE GC Ultra. It also
contains detector parameters and operating tips.
Chapter at a Glance…
Installing Detectors...............................................................................................21
Getting the Most from the Detector......................................................................23
The FID (Flame Ionization Detector), NPD (Nitrogen Phosphorus Detector), FPD
(Flame Photometric Detector), PID (Photoionization Detector), TCD (Thermal
Conductivity Detector) and PDD (Pulsed Discharge Detector) are already
installed on the TRACE GC Ultra according to your requirements. Due to Local
Regulations of radioactive materials, the ECD (Electron Capture Detector) is sent
separately from the GC unit.
If you need to install other detectors, do so in accordance with the configuration
settings. For example, if the left detector is specified as an ECD, install the ECD
on the left side.
Installing Detectors
The detector base body allows you to easily install or exchange detectors. Use the
following procedure to install a detector.
1. Remove the TRACE GC Ultra cover plate from the top of the instrument.
Getting Started 21
Chapter 2
Working with Detectors Installing Detectors
Figure 2-1 shows how an ECD would fit into the detector base body.
22 Getting Started
Chapter 2
Getting the Most from the Detector Working with Detectors
Getting Started 23
Chapter 2
Working with Detectors Getting the Most from the Detector
WARNING! Because of its radioactive source, an ECD has special handling and reporting
requirements.
24 Getting Started
Operating the
3
TRACE GC Ultra
This chapter contains instructions to run an analysis. With all components
installed and configured, you are ready to make the first run, probably a simple
manual injection of a test mixture. You will need to have your data system or
integrator connected and turned on to see the chromatogram. Save the first
chromatogram to compare future performance and to help resolve service issues.
Chapter at a Glance…
Setting Up an Analysis .........................................................................................26
Injecting a Test Mixture........................................................................................28
Getting Started 25
Chapter 3
Operating the TRACE GC Ultra Setting Up an Analysis
Setting Up an Analysis
1. Choose the text mixture or standard you will inject. Your choice will depend
on your intended applications and standard laboratory practice.
3. If you want to make changes to any menu, follow the procedures outlined in
Editing a Menu Item on page 20.
26 Getting Started
Chapter 3
Setting Up an Analysis Operating the TRACE GC Ultra
Example
Menu settings to run the Thermo Fisher Scientific Calibration Mixture for an
FID (PN 338 190 20) with a splitless injection might look like those in the
following figure:
Mkup (N2) 30 30
Figure 3-2. Menu Settings for Thermo Fisher Scientific Calibration Mixture for an FID
Getting Started 27
Chapter 3
Operating the TRACE GC Ultra Injecting a Test Mixture
To analyze the Calibration Mixture for an FID, you will need a 10-µL syringe
with a 51 mm needle. The column and liner shipped with your TRACE GC Ultra
are appropriate for this analysis.
Table 3-1 lists three columns: TRACE GC Ultra Status, Manual Control, and
Automated Control. The first column describes how the TRACE GC Ultra Status
LEDs look during each stage in a run. The second column, Manual Control,
describes the steps and decisions you would face in manually operating the
TRACE GC Ultra. The third column describes automated control options you
might consider.
Once you have prepared a syringe for injection, follow the instructions listed
under Manual Control in Table 3-1. In the case of the calibration mixture for an
FID, you would draw a 1-µL sample and inject this amount, including the mixture
remaining in the needle.
28 Getting Started
Chapter 3
Injecting a Test Mixture Operating the TRACE GC Ultra
NOTE The STATUS key is useful during NOT READY to see a list of conditions which are
preventing the instrument from going to STANDBY.
Getting Started 29
Chapter 3
Operating the TRACE GC Ultra Injecting a Test Mixture
30 Getting Started
Chapter 3
Injecting a Test Mixture Operating the TRACE GC Ultra
Getting Started 31
Chapter 3
Operating the TRACE GC Ultra Injecting a Test Mixture
32 Getting Started
Chapter 3
Injecting a Test Mixture Operating the TRACE GC Ultra
If you analyzed the calibration mixture for an FID, the resulting chromatogram
should resemble the one shown in Figure 3-3 below.
400
1 2 3
318.2
236.4
(mV)
154.6
72.8
-9.001
0.0 1.6 3.2 4.8 6.4 8.0
(min)
Figure 3-3. Chromatogram for Thermo Fisher Scientific Calibration Mixture for an FID Detector
1. dodecane
2. tetradecane
3. hexadecane
Getting Started 33
Chapter 3
Operating the TRACE GC Ultra Injecting a Test Mixture
34 Getting Started
Automating Your
4
Analyses
This chapter discusses the basics of automation in analytical methods and
autosampler sequences. After you have confirmed the TRACE GC’s proper
operation, you will probably want to automate many features.
Chapter at a Glance…
Developing an Analytical Method........................................................................35
Autosampler Sequence Basics..............................................................................37
Getting Started 35
Chapter 4
Automating Your Analyses Developing an Analytical Method
You can store the methods you develop in the TRACE GC’s memory or in the
data system. The TRACE GC Ultra can hold up to 10 saved methods.
Figure 4-1 shows the keys you could use in developing a method. Pressing a key
brings up a menu of choices related to the key name.
When you have set the parameters you want, store the method as follows:
1. Press METHOD.
2. Enter a number between 1 and 10 to denote the memory location where the
method is to be saved.
3. Press STORE.
36 Getting Started
Chapter 4
Autosampler Sequence Basics Automating Your Analyses
Figure 4-2 shows the keys you would use to develop and run a sequence.
NOTE The EDIT/ACTIVE key allows you create and edit methods and sequences while a
sequence is running. Your changes do not affect the current run.
When you have set the parameters you want, save the method as follows:
1. Press SEQ.
2. Enter a number between 1 and 5 to denote the memory location where the
method is to be saved.
3. Press STORE.
Getting Started 37
Chapter 4
Automating Your Analyses Autosampler Sequence Basics
38 Getting Started
Customer
A
Communication
Thermo Fisher Scientific provides comprehensive technical assistance worldwide
and is dedicated to the quality of our customer relationships and services.
How To Contact Us
This appendix contains contact information for Thermo Fisher Scientific office.
Use the list reported in Customer Communication to contact your local Thermo
Fisher Scientific office or affiliate.
Getting Started 39
Appendix A
How To Contact Us
Reader Survey
Product: TRACE GC Ultra
Manual: Getting Started
Part No.: M31709230
Please help us improve the quality of our documentation by completing and returning this survey.
Circle one number for each of the statements below.
Strongly Strongly
Agree Agree Neutral Disagree Disagree
If you would like to make additional comments, please do. (Attach additional sheets if necessary.)
________________________________________________________________________________________
________________________________________________________________________________________
________________________________________________________________________________________
________________________________________________________________________________________
Fax or mail this form to:
Thermo Electron S.p.A.
Strada Rivoltana km 4
20090 Rodano (MI)
ITALY
Fax: 39 02 95059388
40 Getting Started
Appendix A
How To Contact Us
Getting Started 41
Appendix A
How To Contact Us
42 Getting Started
Glossary
This section contains an alphabetical list and descriptions of terms used in this guide and the help
diskette. This also includes abbreviations, acronyms, metric prefixes, and symbols.
A
A ampere
ac alternating current
ADC analog-to-digital converter
B
b bit
B byte (8 b)
baud rate data transmission speed in events per second
C
ºC Celsius
CIP Carriage and Insurance Paid To
cm centimeter
CPU central processing unit (of a computer)
CSE Customer Service Engineer
D
d depth
DAC digital-to-analog converter
dc direct current
DS data system
Getting Started 45
Glossary
E
ECD Electron Capture Detector
EMC electromagnetic compatibility
ESD electrostatic discharge
F
ºF Fahrenheit
FID Flame Ionization Detector
FOB Free on Board
FPD Flame Photometric Detector
ft foot
G
g gram
GC gas chromatograph
GND electrical ground
H
h height
h hour
harmonic A high-frequency disturbance that appears as distortion of the
distortion fundamental sine wave.
HV high voltage
Hz hertz (cycles per second)
46 Getting Started
Glossary
I
IEC International Electrotechnical Commission
impulse See transient
in. inch
I/O input/output
K
k kilo (103 or 1024)
K Kelvin
kg kilogram
kPa kilopascal
L
l length
l liter
lb pound
LAN Local Area Network
LED light-emitting diode
M
m meter (or milli [10-3])
M mega (106)
µ micro (10-6)
min minute
mL milliliter
mm millimeter
Getting Started 47
Glossary
N
n nano (10-9)
NPD Nitrogen Phosphorous Detector
O
Ω ohm
P
p pico (10-12 )
Pa pascal
PCB printed circuit board
PDD Pulsed Discharge Detector
PID Photo Ionization Detector
psi pounds per square inch
R
RAM random access memory
RF radio frequency
ROM read-only memory
RS-232 industry standard for serial communications
S
s second
sag See surge
slow average A gradual, long-term change in average RMS voltage level,
with typical durations greater than 2 s.
48 Getting Started
Glossary
T
TCD Thermal Conductivity Detector
transient A brief voltage surge of up to several thousand volts, with a
duration of less than 50 µs.
U
UFM Ultra Fast Module
V
V volt
V ac volts, alternating current
V dc volts, direct current
VGA Video Graphics Array
W
w Width
W Watt
Getting Started 49
Index
A I
analysis 25–33 INFO/DIAG 20
analytical method 35–36 Initial Temp LED 30
automation 28–32, 35–38 injecting a sample 28
autosampler 19 inlet
autosampler sequence 37 on column 19
auxiliary detector 19 Inlet menu 27
auxiliary devices 19 installing detectors 21–22
C K
Carrier menu 27 key
column select valve 19 CONFIG 18
CONFIG 18 DOWN ARROW 20
configuration 15–20 EDIT/ACTIVE 37
Configuration menu 18–19 INFO/DIAG 20
Cool LED 32 LOAD 29
MODE/TYPE 18, 20
D OFF/NO 20
detector 19 ON/YES 20
applications 23 STORE 36, 37
auxiliary 19 keypad 17
base body 21
ECD (Electron Capture Detector) 16, 23, 24 L
FID (Flame Ionization Detector) 23 LOAD 29
installation diagram 22
NPD (Nitrogen-Phosphorus Detector) 23 M
operating suggestions 23–24 manual operation 28–32
Detector menu 27 menu
detectors Carrier 27
installing 21–22 Configuration 18–19
DOWN ARROW 20 Detector 27
editing 20
E Inlet 27
ECD (Electron Capture Detector) 16, 22, 23, 24 navigation 18
EDIT/ACTIVE 37 Oven 18, 27
editing a menu 20 sample settings for analysis 27
external devices 19 Signal 27
method 35–36
F MODE/TYPE 18, 20
FID (Flame Ionization Detector) 23
calibration mix 27–28, 33 N
Final Temp LED 31 Not Ready LED 29
NPD (Nitrogen-Phosphorus Detector) 23
H
hydrogen sensor 19
Title 51
Index
O
OFF/NO 20
ON/YES 20
on-column inlet 19
operating instructions 25–33
automated 28–32
manual 28–32
oven cryogenic options 19
Oven menu 18, 27
P
Post Run LED 32
Prep Run LED 29
pressure ramps 31
R
Ramp LED 31
ramps
pressure 31
temperature 31
Ready-to Inject LED 30
S
sequence 37
Signal menu 27
signal polarity 19
status LEDs 28–32
STORE 36, 37
submenu 18
syringe 28
T
temperature ramps 31
V
valve 19
column select 19
valve oven 19
52 Title
List of Figures
Figure 1-1. TRACE GC Ultra Keypad............................................................................................17
Figure 1-2. Oven Menu Display......................................................................................................18
Figure 2-1. Detector Installation Diagram ...................................................................................... 22
Figure 3-1. Zone and Device Keys to Set Run Parameters .............................................................26
Figure 3-2. Menu Settings for Thermo Fisher Scientific Calibration Mixture for an FID ............. 27
Figure 3-3. Chromatogram for Thermo Fisher Scientific Calibration Mixture for an FID Detector33
Figure 4-1. Keys Used in Developing an Analytical Method .........................................................36
Figure 4-2. Keys Used in Developing an Autosampler Sequence ..................................................37
List of Tables
Table 1-1. Main Configuration Menu ............................................................................................19
Table 2-1. Detector Options, Sensitivities, and Tips .....................................................................23
Table 3-1. Steps in a TRACE GC Ultra Run .................................................................................29