GCMS & GC- HS & GC-FID
- Standard
Operating Procedure
SOP on the
operation, calibration and maintenance of Gas Chromatography (FID
Detector)/Head Space
(Quality)
Lab
Code xxx
Version No.:
Effective
Date:
Review Date:
Supersedes:
Author(s):
Technical Approver
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Authorized By
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Name
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Designation
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Head of
Department / DI
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Director /
DI
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QA
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Signature
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Date
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1.
Purpose: To describe a procedure for the
operation, calibration and maintenance of Gas Chromatograph/Head Space (GC-HS).
2.
Scope: This SOP applies to the Gas
Chromatograph, GC-HS (Make: Agilent Technologies; Model: 6850/7694E located in
instruments section of analytical laboratory.
3.
References: Refer to Operating instructions manual
for the same.
4.
Procedure
The primary sources of information
for operation, maintenance and calibration
are the manufacturer's manuals. This SOP, as written, highlights the important sections of the manuals.
are the manufacturer's manuals. This SOP, as written, highlights the important sections of the manuals.
4.1 Operation
4.1.1
Ensure that the instrument is clean, free from dust and vibration.
4.1.2
Ensure that environment condition are in suitable (Temp 15-35°C) Humidity
40-60%.
4.1.3
Ensure that part of instrument and system in configuration.
4.1.4 Turn on the cylinders of nitrogen
(grey with a black top), air (grey) and hydrogen
(red) kept in the gas station
on the ground floor. Always check the
pressure level on the regulators.
4.1.5
Turn on the GC
instrument along with the HS.
4.1.3 Open the
toggle valves on the gas panel for all the three gas lines of hydrogen, air and nitrogen.
4.1.4 Click the
icon Instrument
Online placed on the desktop for invoking the GC Chemstation software. This will launch the Chemstation software for controlling the software remotely.
4.1.5 Go to method
& run control and load the desired method. This will download the entire method conditions to the GC namely oven temperature,
front inlet temperature, split
ratio, front
detector temperature, front detector hydrogen and air flow and column
carrier gas nitrogen flow.
4.1.6
Manually set the HS parameter method, Initialization time, Vial temperature,
runtime, Injection time, shaking time and purging the injection.
4.1.6 Place the
sample vial containing the sample in the HS sampler at the desired position and
given the all information in the Sample sequence. There are 18 sample
positions.
4.1.7 When the
Chemstation online and HS Manual key board shows ready (all green color) click
the ‘START’ icon on HS Key board. This will set the instrument in the run mode.
4.1.8 In the offline window one can monitor the run
by clicking the snapshot option in the
drop down menu. Further data analysis also can be performed in the same window.
4.2 Shut Down after Cooling
4.2 .1 This is very
critical operation and must be performed on a regular basis after the end of analysis.
1.2.2
The method cool.m was loaded in the Chemstation Online window. This turns off
the detector gases (both hydrogen and air). The fan inside the oven starts
cooling the capillary column until the temperature comes down to 30º C. Once
the the set temperature is achieved the system is safe to be turned off.
(Never turn off
the GC system when the column is at a temperature higher than 30º C. This can
damage the column as the packing material starts leaching out and decreases the
performance).
4.3 Calibration and Frequency
4.3.1 The IPV
(Instrument Performance Verification) is carried out by the service engineer as
a part of AMC visits on a yearly basis along with documentation report as well.
4.3.2
The frequency selected to carry out the calibration is once a year for
instrument performance. Test solutions and STD
used or recommended by vendors are acceptable if Certificates of Analysis (COAs) of these are available. Use test
solutions or STDs traceable to NIST or International
Reference if they are available.
4.3.3
Service Qualification: An analyst or a qualified service representative is
qualified for calibration. Training certifications must be provided prior to
commencing work.
4.3.4
Column: Capillary column
would be used for calibration of split and split less injector with appropriate standards.
4.4 Calibration and Validation Tests
required
4.4.3 Inlet
pressure accuracy: This test demonstrates the ability of the system to
provide accurate pressure to the head of the column. The acceptance limit
should be ≤ 1.2.
4.4.4 Detector
flow accuracy: It is determined by measuring the flows with
calibrated mass flow meter and comparing them to the test set points and the
values displayed by the GC (If applicable). The acceptance limits are as
follows:
4.4.5 Signal Noise and Drift: The base signal is recorded at the beginning of the
test, signal noise is calculated as ASTM
noise which is average peak to peak noise in a number of signal segments and
signal drift is calculated as the slope of the linear regression of the signal.
The acceptance limits are as follows:
Noise
(ASTM) ≤ 0.1 pA
Drift ≤ 2.5
4.4.6 Signal to Noise: This test uses a traceable STD
to determine signal to noise. The acceptance limit should be ≥ 300, 000.00.
4.4.7 HS
4.4.7 Injector Precision: This test uses a traceable STD to
determine injector precision. Following should be the acceptance limits,
Injector Precision (liquid) Retention time % RSD ≤ 1.0
Area % RSD ≤ 3.0
Injector Precision (Head Space)
Retention time % RSD ≤ 1.0
Area % RSD ≤ 3.0
If the test fails, arrange a service and place an
“Out of Service” sticker on the instrument.
5.
Responsibilities: It is the responsibility of the
section in charge to ensure that staff are trained in all aspects of this SOP
or deemed competent in its application. It is the responsibility of the
operator to ensure compliance with this document.
6.
References
6.1
Agilent service manuals, Part # G
6.2 Agilent 7694E Automatic Head Space Sampler
Installation Guide, Part #
7.
Appendices
8.
Revision History
SOP No.
|
Supersedes No. & Date
|
Changes made (in brief)
|
END
OF THE DOCUMENT
==================================================
Standard Operating
Procedure
SOP on the operation, calibration and
maintenance of Gas Chromatograph/Mass Spectroscopy [Agilent-7890A/5975C]
(Quality)
Document No …
Version No.:
Effective Date:
Review Date:
Supersedes:
Author(s):
Technical
Approver
|
Authorized
By
|
||
Name
|
|||
Designation
|
Head of Department
|
Director
|
QA
|
Signature
|
|||
Date
|
|||
1.
Purpose: To describe a procedure for the
operation, calibration and maintenance of Gas Chromatograph/Mass spectroscopy
(GC/MS).
2. Scope:
This SOP applies to
the Gas Chromatograph/Mass spectroscopy, GC/MS (Make: Agilent Technologies;
Model: 7890A/5975C) located in instruments section of analytical laboratory.
3.
References: Refer to Operating instructions manual
for the same.
4.
Procedure
The primary sources of information
for operation, maintenance and calibration
are the manufacturer's manuals. This SOP, as written, highlights the important sections of the manuals.
are the manufacturer's manuals. This SOP, as written, highlights the important sections of the manuals.
4.1 Operation
4.1.1 Ensure
that Instrument is clean , free from dust and vibration
|
4.1.2 Ensure
that Environment conditions are in suitable (Temp. 15 -35 °C) Hum. 40 – 60 %
|
4.1.3 Ensure
that all part of Instrument and system is on.
|
4.1.4 Now open
the Helium gas (99.9995% purity) Cylinder valve & regulate the pressure
of gas 6 bar.
|
4.1.5 ‘ON’ the
GC & ‘ON’ the MS, wait for some time till turbo pump speed is 100% of
full.
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4.1.6 Now open
the MSD-1 software located on computer‘s desktop.
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4.1.7 Load the
condition method for 2-3 hrs. & check the tune status.
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4.1.8 If the
tune report is passed (tuning performed after 2-3days). Load the analyzing
method for analysis.
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4.1.9 For run
the sample :- Click on method , Click
on run method, a window will display , gave the sample information and, Click
OK & RUN method
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4.2.0 After
complete the run time & post run
time , the data file of unknown sample is compare with std curve data file (
on data analysis) , & take print.
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For night: -
Instrument leave on overnight method.
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Next day, load
the condition method for some time & after that load analyzing method.
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4.2 Shut Down after Cooling
4.2 .1 This is very critical operation
and must be performed the basis of work load.
4.2.2
For Close the instrument :- Click on view, Click on tune & vacuum control, Click on vacuum, Click on vent
4.2.3
Wait for some time till , turbo pump speed >50%, MS
Source temp > 100°C, MS Quad temp > 100 °C
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4.2.4 Software
will be closed automatically and now off MS & GC
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4.2.5 Close
the helium gas cylinder valve.
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4.2.6 Shutdown
the computer and off the electric supplies.
|
4.3
.Calibration and Frequency
4.3.1 Daily Tuning of MS is required before work or after
25 injections of samples by the Auto tuning with the PFTBA.
The IPV
(Instrument Performance Verification) is carried out by the service engineer as
a part of AMC visits on a yearly basis along with documentation report as well.
4.3.2
The frequency selected to carry out the calibration is once a year for
instrument performance. Test solutions and STD
used or recommended by vendors are acceptable if Certificates of Analysis (COAs) of these are available. Use test
solutions or STDs traceable to NIST or International
Reference if they are available.
4.3.3
Service Qualification: An analyst or a qualified service representative is
qualified for calibration. Training certifications must be provided prior to
commencing work.
4.3.4
Column: Capillary column
would be used for calibration of split and splitless injector with appropriate standards.
4.4 Calibration
and Validation Tests required
4.4.2
MS Mass Calibration:
for this purpose we have used PFTBA calibrant as a automatic calibration system
by the auto tuning for mass 69, 219 and 512.
4.4.3 Inlet pressure decay: This test
demonstrates the pressure integrity of the GC inlet (with a valve controlled
injection system, if applicable) and all flows controlled by GC inlet
pneumatics. The acceptable limit for pressure change should be ≥ -2.0 and
<0.5 psi/5min.
4.4.4 Inlet
pressure accuracy: This test demonstrates the ability of the system to
provide accurate pressure to the head of the column. The acceptance limit
should be ≤ 1.2.
4.4.5 Signal Noise and Drift: The base signal is recorded at the beginning of the
test, signal noise is calculated as ASTM
noise which is average peak to peak noise in a number of signal segments and
signal drift is calculated as the slope of the linear regression of the signal.
The acceptance limits are as follows:
Noise
(ASTM) ≤ 0.1 pA
Drift ≤ 2.5
4.4.6 Signal to Noise: This test uses a traceable STD
to determine signal to noise. The acceptance limit should be ≥ 300, 000.00.
4.4.7 Injector Precision: This test uses a traceable STD to
determine injector precision. Following should be the acceptance limits,
Injector Precision (liquid) Retention time % RSD ≤ 1.0
Area % RSD ≤ 3.0
Injector Precision (Head Space)
Retention time % RSD ≤ 1.0
Area % RSD ≤ 3.0
If the test fails, arrange a service and place an
“Out of Service” sticker on the instrument.
5.
Responsibilities: It is the responsibility of the
section in charge to ensure that staff are trained in all aspects of this SOP
or deemed competent in its application. It is the responsibility of the
operator to ensure compliance with this document.
6.
References
6.1
Agilent service manuals, Part # G 1530-90220
6.2 Agilent 6890 Automatic Liquid Sampler
Installation Guide, Part # G2612- 90107
7.
Appendices
8.
Revision History
SOP
No.
|
Supersedes
No. & Date
|
Changes
made (in brief)
|
END OF THE DOCUMENT
