The instrument name and description

The serial number and local asset number

 The location of the instrument

The person responsible for the instrument

The manufacturer's reference number of the instrument manual(s) and its location

A reference to the keeping of a record of any changes to the above and its location

A reference to the recording of major maintenance/changes( - not down to the level of

septum/seal/column changes  ) and the location of the record

Apart from the SOP itself ( but nothing to do with an SOP as such) it might be a local
requirement for anyone using the instrument be a trained person and a record held of that
training.

Regards

STANDARD OPERATING GAS CHROMATOGRAPHY/MASS SPECTROMETRY

MAKMAL FARMASEUTIKAL NEGERI SABAH

STANDARD OPERATING PROCEDURE FOR THE ANALYSIS OF TRICHLORONITROMETHANE

(CHLOROPICRIN) IN AMBIENT AIR USING GAS CHROMATOGRAPHY/MASS SPECTROMETRY MLD075
Revision 0.0 Northern Laboratory Branch Monitoring and Laboratory Division

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.
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

4.4.1   Temperature accuracy and stability (Detector): Herein compare selected detector set point
temperature versus actual system reading (refer to Agilent’s user manual for set temperature
recommendations). Temperature accuracy at two set temp is measured at 230° C and 100 ° C.  Actual
temperature reading should be within ±1% of the set point. The temperature stability should be ≤ 0.5 ° C.
4.4.2 Temperature accuracy and Stability (HS Sampler): Herein compare selected set point
temperature versus actual system reading (refer to Agilent’s user manual for set temperature
 recommendations). Temperature accuracy at one set temperature is measured at 70°C. Actual
temperature reading should be within ±1% of set point. The temperature stability should be ≤0.5°C.
4.4.2   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.
4.4.3   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.
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.

4.1.6 Now open the MSD-1 software located on computer‘s desktop.

4.1.7 Load the condition method for 2-3 hrs. & check the tune status.
4.1.8 If the tune report is passed (tuning performed after 2-3days). Load the analyzing method for
analysis.

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        

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.

For night: - Instrument leave on overnight method.

 Next day, load the condition method for some time & after that load analyzing method.

4.2       Shut Down after Cooling

4.2 .1 This is very critical operation and must be performed the basis of work load.
   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                                     

                                                      

4.2.4 Software will be closed automatically and now off MS & GC

4.2.5 Close the helium gas cylinder valve.

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

4.4.1   Temperature accuracy and stability: Herein compare selected detector set point temperature
versus actual system reading (refer to Agilent’s user manual for set temperature recommendations).
Temperature accuracy at two set temp is measured at 230° C and 100 ° C.  Actual temperature reading
should be within ±1% of the set point. The temperature stability should be ≤ 0.5 ° C.
 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