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GC TCD Sop

This document provides instructions for operation of an Agilent 7890 Gas Chromatograph with a Thermal Conductivity Detector (TCD). It describes the instrument components, safety concerns, initial setup procedures, method creation, and sample analysis steps. The TCD is useful for detecting many permanent gases and other molecules down to low ppm concentrations.
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0% found this document useful (1 vote)
200 views6 pages

GC TCD Sop

This document provides instructions for operation of an Agilent 7890 Gas Chromatograph with a Thermal Conductivity Detector (TCD). It describes the instrument components, safety concerns, initial setup procedures, method creation, and sample analysis steps. The TCD is useful for detecting many permanent gases and other molecules down to low ppm concentrations.
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 6

Effective Date: 23/03/2021

Document #: SOP-GC2104
Page 1 of 6

Standard Operating Procedure

Agilent 7890 Gas Chromatograph


(Thermal Conductivity Detector)

Introduction
Gas chromatography (GC) is a separation process used to isolate the individual components of various
mixture. Gas chromatography (GC) is an analytical technique used to separate and detect and quantify
small molecular weight compounds (<1000 Da) in the gas phase. Unlike other forms of
chromatography - the mobile phase is a gas, and the components are separated as vapors. The
Thermal Conductivity Detector (TCD) is the most universal detector used with a GC. The major benefit
is it detects all molecules, and it commonly used for permanent gas analysis (O2, N2, CO, CO2, H2S,
NO, etc.). The TCD can also detect concentrations from 100% down to around 100 ppm).

Purpose
The purpose of this document is to introduce the user to the routine operation of Agilent 7890 Gas
Chromatograph with a Thermal Conductivity Detector (7890 GC-TCD). This document also outlines the
special safety concerns introduced when using the instrument.

Scope
This procedure applies to established procedures of analysis using the standard configuration (shown
below) for the 7890 GC-TCD. Individuals must complete a hands-on one-on-one training session with a
TRACES staff member.

Referenced Documents
▪ Agilent GC ChemStation: Familiarization Guide ed. 1 st (p/n 5973-1771)
▪ Agilent 7890A: GC Advanced User Guide ed.11th (p/n G3430-90015)
▪ Agilent 7890A: Operating Guide ed.3rd (p/n G3430-90011)
▪ Agilent 7890A: Quick Reference ed. 3rd (p/n G3430-90009)
▪ Agilent 7890A: Fundamentals of Gas Chromatography ed. 1st (p/n G1176-90000)
▪ Agilent 7890A: Troubleshooting ed. 6th (p/n G3430-90017)

Responsibilities
1. TRACES Users
1.1. All Users must obtain training with TRACES Staff prior to system operation. It is the responsibility
of the User to ensure they have a good understanding of the instrument and all operation
protocols.
1.2. If additional training sessions are needed it is the responsibility of the User to schedule these with
TRACES Staff.
1.3. User must ensure that the helium gas (mobile phase), GC column, and TCD are required for
impending analysis are available in TRACES*.

Approver:
T. Adamo Page 1 of 6
Effective Date: 23/03/2021
Document #: SOP-GC2104
Page 2 of 6

Standard Operating Procedure

1.4. Instrument time must be booked by the User via the online booking system prior to system
operation.

2. TRACES Staff
2.1. It is the responsibility of TRACES Staff to provide introductory and, if required, subsequent
training to all users.

Equipment (Standard Configuration)


▪ Agilent 7890A GC TCD* (Go to Initial Setup for more details)
.1. Mobile Phase: Helium Gas
.2. Detector: TCD
.3. GC Column:
.3.1. Agilent GS-CarbonPLOT 30m x 0.32mm (3.0um)
.3.2. Agilent VF-WAXms 30m x 0.25mm (1.0um)
.3.3. Agilent HP5 30m x 0.32mm (0.25um)

Safety
IMPORTANT:
▪ All the organic solvents used for GC analysis are flammable
▪ Many permanent gases are flammable
o Take the appropriate precautions
▪ Seek assistance from TRACES Staff if you have any concerns

Initial Setup
1. Ensure the carrier gas (Helium) contains MORE than 500 psi in the cylinder. If you expect a long
run time contact the TRACES Lab Manager
2. Turn the regulators to ‘OPEN’.
3. Check the gas pressures entering the GC are set to the values below (they are set by the
TRACES Staff, please DO NOT Touch)
a. Helium :60 psi
4. Power on the GC
a. Once a diagnostics test is run, “Power Successful’ should appear
5. Start the computer
a. Username/Password is given verbally by TRACES Staff
b. Click on Instrument 1 Online
6. Confirm that all the Instrument Actuals (components within the GC) * are not greyed out.

GC Setup Section

Approver:
T. Adamo Page 2 of 6
Effective Date: 23/03/2021
Document #: SOP-GC2104
Page 3 of 6

Standard Operating Procedure

Figure 1

7. Load a Method
a. Click on Method and Load a method from the list provided
i. Should include ‘TCD’ in the method name
ii. If you wish to use this loaded method (skip to #10)
iii. To create a new method, use the loaded method as a template (go to #8)
8. Click on the Instrument Actuals window (Figure 1)
a. Manual Injection (using 250uL gas-tight syringe)
i. Remove the ALS
1. This procedure will be done by TRACE Staff members
2. ALS will be greyed out (skip to #8c)
b. ALS
i. Trays: Set by program, do not change
ii. Sample Overlay: Used particularly when runs are long
1. Apply when using isothermal runs
iii. Injector
1. Set to Back Injector
2. Set the injector volume between 1-5 uL
3. Set the number of washes and pumps per injection
c. MM Inlet
1. Set Points for:
a. Temperature
b. Pressure
2. Septum Purge flow
a. Rate: 3 mL/min (MINIMUM)
b. Mode: Standard
3. Mode
a. Split (standard)
b. Splitless (low level)
c. Pulsed (maximize transfer)
d. PTV (Large Volume Injections)
d. Column
i. Control Mode: On
1. Set the control mode. The remaining parameters will be defaulted once
this is identified.
a. Constant pressure or flow
b. Programmable pressure or flow
ii. GC Column will be loaded by the TRACES staff

Approver:
T. Adamo Page 3 of 6
Effective Date: 23/03/2021
Document #: SOP-GC2104
Page 4 of 6

Standard Operating Procedure

e. Oven
i. Temperature set
1. Ramped
2. Isothermally
ii. Check with the TRACES Manager for the Maximum Oven Temperature
f. Detector
i. TCD-Back
1. Set (DEFAULT: Do not change without consulting TRACES Staff)
a. Heater temperature
b. Reference flow (He): 20 mL/min
c. Makeup flow (He): 2 mL/min
d. Column + Makeup: computer generated
g. Events
i. Setting time events during the analysis run
1. AO signal range
2. Inlet septum purge

h. Signals
i. Back Signal (TCD) in the #1 Slot
1. Data Rate :50 Hz/0.004 min (default)
2. Zero is checked (AO at injection)
3. Save is checked (save the signal)
9. Method>Save
a. Use an exclusive method name
b. Loading a previous method and making changes
i. Save ‘new’ method using an exclusive method name

GC Analysis Section
10. Single Sample/Manual Injection
a. Select Run Control from the Task Bar
i. Set the subdirectory (if necessary, a new one must be created)
ii. Select the file name using the format; Course/PI/Student_DDMMYY
1. Counter set to value between 0001 and 9999
iii. Enter the vial location
iv. Enter the sample name and comment if required
b. Run the sample from the Task Bar or the Run Method icon in ChemStation
11. Sequence
a. Sequence Parameter
i. Set a new subdirectory for EVERY new sequence
1. The data may be overwritten
2. Change to prefix/counter and set a base name to id samples
3. Sequence output: As specified by method

b. Sequence Table
ii. Populate the sections below for each sample:

Approver:
T. Adamo Page 4 of 6
Effective Date: 23/03/2021
Document #: SOP-GC2104
Page 5 of 6

Standard Operating Procedure

1. Vial number
2. Sample name
3. Method*
4. Injections/Vial
5. Sample Type: Set to sample
iii. Fill-down Wizard can be used
iv. Press Okay
c. Press Run Sequence (i.e. Analyze samples)
i. Under the Run Control menu
ii. On the Sampling Diagram

Data Evaluation Section


12. Click Instrument Offline
13. Select Data Analysis tab
14. Click on File>Load Signal
a. This will load the data file of interest
15. Reports
a. Print Report
i. Press Okay to print to the default printer
ii. If the need is to auto print the Report go to #15(c)(i)
iii. If the Report is unsatisfactory go to #15(b) and alter accordingly
b. Specify Report
i. Determine Qualitative Results Info
1. Calculate: Percent
2. Based On: Area
3. Sorted by: Signal
ii. Report Style: Short
1. Add Chromatogram Output box checked
iii. Report Layout for Uncalibrated Peaks
1. With Calibrated Peaks box checked
c. Destination
i. Printer box checked
1. Reports are auto printed at the end of a run
a. Ensure a default printer is available
ii. Screen box checked
1. Reports are shown on the screen at the end of run where they can be
printed
2. The subsequent run report will remove the preceding run report from the
screen

iii. File box checked


1. File Setting
a. Check the Unique pdf file box

Approver:
T. Adamo Page 5 of 6
Effective Date: 23/03/2021
Document #: SOP-GC2104
Page 6 of 6

Standard Operating Procedure

b. Check the desired file format


i. Files are saved in the *.D files
16. Integration*
a. Using the CS Integrator
i. Integrate Manually
1. Using Integration Events
ii. Auto Integrate
17. Calibration*
a. Calibration Table
i. Set the Analyte Name, Level and Concentration
ii. Calibrate
18. Method>Save
a. This will transform the Report/Integration/Calibration Results, lock it to the method for
successive analysis that use this method will contain the default values saved

*The TRACES Manager will provide full details during hands-on training.

Approver:
T. Adamo Page 6 of 6

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