SOP for Calibration of Head Space Gas Chromatograph
1.0 OBJECTIVE
To calibrate the equipment for reliable and accurate results.
2.0 SCOPE
This procedure is applicable to calibrate Head Space Gas Chromatograph installed in Quality Control Laboratory.
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3.0 RESPONSIBILITY
3.1 Doing: Technical Assistant
3.2 Checking: Executive/Manager
4.0 ACCOUNTABILITY
Head of the Department
5.0 PROCEDURE
5.1 (I) BY MANUAL INJECTION:
Frequency: Every 3 month.
5.1.1 Install the DB-5 capillary column.
5.1.2 Set all parameters as per Annexure – I.
5.1.3 Stabilized the column for the stable baseline.
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5.1.4 Inject 1 µl of each standard solution in duplicate.
5.1.5 Calculate the ratio of Area of methanol to the internal standard.
5.1.6 Record the results in Annexure – I.
5.1.7 Calculate the linearity and correlation coefficient.
5.2 (II) FOR HEADSPACE INJECTION :
Frequency: Every 6 months.
5.2.1 Install the DB-5 capillary column.
5.2.2 Set all parameter as per Annexure – II
5.2.3 Prepare the standard solution as mentioned in Annexure – II
5.3 Check the performance for
(1) Reproducibility test
(2) Linearity test.
5.4 Reproducibility test
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5.4.1 Take 5 ml of standard preparation in 5 Head Space vial.
5.4.2 Add 1 gm of sodium sulphate (Anhydrous) in each.
5.4.3 Inject 1 ml gaseous form of the standard from each of 5 vials.
5.4.4 Record the result in Annexure – II
5.4.5 Calculate the standard deviation and related standard deviation for the respective separated solvent peak.
5.5 Linearity test
5.5.1 Take 2 ml, 5 ml and 10 ml of standard solution in Head Space Vial.
5.5.2 Add 1gm sodium sulphate (Anhydrous) make 10 ml volume by addition of required volume in respective headspace vial.
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5.5.3 Inject 1 ml Gaseous form of each standard.
5.5.4 Record the result in Annexure – II
5.5.5 Calculate the regression coefficient of the respective separated solvent peak.
5.6 After completion of Analysis, cool down the G.C.
5.7 After cooling, switch ‘OFF’ the instrument.
5.8 Switch ‘OFF’ the mains.
6.0 ABBREVIATIONS
6.1 G.C. = Gas chromatograph
6.2 ml = millimeter
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