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.

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.
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

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.

Related: Calibration of Gas Chromatography (GC)

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.

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

ANNEXURE-I

QUALITY CONTROL LABORATORY

CALIBRATION  CHECK REPORT OF

GAS CHROMATOGRAPH

CALIBRATION DATE	DATE OF LAST CALIBRATION DONE	NEXT DUE FOR CALIBRATION

INSTRUMENT DETAILS
INSTRUMENT NAME	INSTRUMENT MAKE	INSTRUMENT IDENTIFICATION NO.

OBSERVATION

(I)  FOR  MANUAL INJECTION
G.C. Parameters:
Column                    : DB-5 Capillary (0.32mm X 30meter X 0.25micron)                   
Range                      : 2
Oven Temp.            : 30⁰C
Split Ratio               : 1:20
Detector Temp        : 180⁰C
Nitrogen                  : 100 kPa
Inj. Temp.               : 140⁰C
Carrier                    : 25Kpa (Helium)
Inj. Volume             : 1.0μl
Hydrogen                : 55Kpa
Air                          : 85 Kpa

Preparation of internal Standard: 25 ml Ethanol è 1000 ml with water
Test preparation : 1 ml, 2 ml, 3 ml, 4 ml, 5 ml Methanol 100 ml with Internal Std.

Methanol (% v/v)	Ratio of Methanol/Ethanol	Mean Ratio
1.0	(1)
	(2)
2.0	(1)
	(2)
3.0	(1)
	(2)
4.0	(1)
	(2)
5.0	(1)
	(2)

               Correlation coefficient :___________ (Not less than 0.9900)

PERFOMED BY			CHECKED BY
NAME	SIGN.	DATE	NAME	SIGN.	DATE

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