Calibration procedure for gas chromatograph clarus 500 with headspace (Perkin Elmer)
OBJECTIVE
To lay down the procedure for calibration of GC Clarus 500 with headspace (Perkin Elmer )
SCOPE
This SOP shall be applicable for the GC Clarus 500 with headspace (Perkin Elmer).
RESPONSIBILITY
Quality Control Executive/Officer.
ACCOUNTABILITY
Head Quality Control.
CALIBRATION PARAMETERS
- Oven temperature
- Carrier gas flow rate
- Hydrogen & Zero air gas flow rate
- Linearity test
- Repeatability test
Oven temperature:
- Set GC oven temperature to 50°c
- Set probe-I & probe-II of RTD in the GC oven & close the door.
- After 10 minutes note the temperature.
- Repeat the process at 100°C and 200°C
- The acceptance criteria for the GC oven is ± 2°c.
Carrier Gas Flow rate:
- Install capillary column G43 / (DB-624, 30 M X 0.53 mm X 3µm)
- Set carrier flow 5ml / min by GC control panel
- Set electronic flow meter input in the collector assembly.
- Set Hydrogen & zero airflows 0 ml/min by GC control panel.
- Note the flow of Carrier gas.
- Repeat this process at 20ml/min and 50 ml/min
- The acceptance criteria for the carrier flow rate is ± 2% of the set value.
Hydrogen and Zero air flow rate:
- Install capillary column G43 / (DB-624, 30 M X 0.53 mm X 3µm)
- Set carrier flow & zero airflows 0 ml/min by GC control panel.
- Set electronic flow meter input in the collector assembly.
- Note the flow of hydrogen gas.
- Set carrier flow & hydrogen flow to 0 ml/min by GC control panel.
- Note the flow of zero air gas
- The acceptance criteria for hydrogen & zero air gas flow rate is ± 2% of the set value.
LINEARITY TEST:
GC PARAMETERS
- Column: G43 / (DB-624, 30 M X 0.53 mm X 3µm)
- Initial oven temperature:45°c
- Initial hold time: 12 minutes.
- Rate: 45°c
- Final oven temperature: 220°c
- Final hold time: 2.0 minutes
- Injector temperature: 150°c
- Detector temperature: 250°c
- Range: 1
- Attenuation: 2
- Carrier flow (nitrogen): 2 psi
- Split flow: 20 ml/min.
HS PARAMETERS
- Oven temperature: 80°c
- Needle temperature: 90°c
- Transfer line temperature: 100°c
- Thermostatting time: 20 minutes
- Pressurization time: 3.0 minutes
- Withdrawal time: 0.2 minute
- Injection time: 0.1 minute
- GC cycle time: 25 minutes
- Column pressure: 9.5 psi
Linearity solution preparation:
Solution (A)
Take 200 mg of ethanol, 200 mg of Isopropyl alcohol, 200 mg of methylene chloride, and 200 mg of ethyl acetate in a 100 ml volumetric flask containing 20 ml Dimethyl sulfoxide and dilute up to mark with purified water.
Take 5 Nos of 100 ml volumetric flasks previously cleaned and dried and mark 25 ppm, 50 ppm, 100 ppm, 200 ppm & 300 ppm.
Blank preparation: 1 ml purified water in headspace vial & seal
Linearity solution 25 ppm: Take 1.25 ml of solution(A), make the volume with purified water, take 1 ml in an HS vial & seal.
Linearity solution 50 ppm: Take 2.5 ml of solution(A), make the volume with purified water, take 1 ml in an HS vial & seal.
Linearity solution 100 ppm: Take 5 ml of solution(A) , make the volume with purified water, take 1 ml in an HS vial & seal.
Linearity solution 200 ppm: Take 10 ml of solution(A) make the volume with purified water, take 1 ml in an HS vial & seal. Linearity solution 300 ppm: Take 15 ml of solution(A) make the volume with purified water, take 1 ml in an HS vial & seal.
After conditioning, the column set the system on the above parameters and injects the linearity solutions in the following sequence.
Blank → LIN SOL (25 ppm) → LIN SOL (50 ppm) → LIN SOL (100 ppm) → LIN SOL (200 ppm) → LIN SOL (300 ppm)
Acceptance criteria
The correlation coefficient between concentration in ppm and the response of each solvent should be ≥ 0.99
% CARRY OVER and REPEATABILITY TEST :
GC PARAMETERS
- Column: G43 / (DB-624, 30 M X 0.53 mm X 3µm)
- Initial oven temperature: 45°c
- Initial hold time: 12 minutes.
- Rate: 45°c
- Final oven temperature: 220°c
- Final hold time: 2.0 minutes
- injector temperature:150°c
- detector temperature: 250°c
- range :1
- attenuation: 2
- carrier flow (nitrogen): 2 psi
- split flow: 20 ml/min.
HS PARAMETERS
- Oven temperature: 80°c
- Needle temperature: 90°c
- Transfer line temperature: 100°c
- Thermostatting time: 20 minutes
- Pressurization time: 3.0 minutes
- Withdrawal time: 0.2 minute
- Injection time: 0.1 minute
- GC cycle time: 25 minutes
- Column pressure: 9.5 psi
Repeatability solution preparation:
Solution (A)
Take 200 mg of ethanol, 200 mg of Isopropyl alcohol, 200 mg of methylene chloride, and 200 mg of ethyl acetate in a 100 ml volumetric flask containing 20 ml Dimethyl sulfoxide and dilute up to mark with purified water.
Take 1 No of 100 ml volumetric flasks previously cleaned and dried and mark 100 ppm.
Blank preparation :1 ml purified water in headspace vial & seal
Repeatability solution 100 ppm : 5 ml of solution(A) , make the volume with purified water
Take six headspace vials and take 1 ml repeatability solution in each vial and seal immediately.
After conditioning the column set the system on the above parameters and load vials in HS magazine in the following sequence.
Blank (one vial) → repeatability (six vials) → air blank (one vial) → blank (one vial)
Acceptance criteria
The relative standard deviation of six replicate injections for the area and RT of each solvent should not be more than 10% and 2.0% respectively
Calculate the % age of carry over each solvent in the last blank vial by the following formula:
% Carryover =(area of solvent in blank / mean area of solvent in six repeatability injections) x 100
Acceptance criteria
- % Carryover for each solvent is not more than 0.01%
- Record the observations in Annexure-I.
- If the instrument goes under maintenance, after service the calibration of the instrument is to be conducted.
- In a case out of calibration display the “OUT OF ORDER “ label and make an entry in the instrument downtime log book.
Forms and Records (Annexures)
Calibration procedure for gas chromatograph Clarus 500 – Annexure – 1
Distribution
Master copy – Quality Assurance
Controlled copies- Quality Assurance, Production, Quality Control. engineering
Annexure – 1
Calibration procedure for gas chromatograph clarus 500
- LOCATION
- CALIBRATION PROCEDURE NO.
- MANUFACTURED BY
- INSTRUMENT ID. NO.
- MODEL NO.
- EFFECTIVE DATE
- CLEANLINESS OF EQUIPMENT / INSTRUMENT BEFORE CALIBRATION: SATISFACTORY/ NOT SATISFACTORY
OVEN TEMPERATURE
Set temperature: 50°C / 100°C /200°C
Observations: Probe-1 & Probe-2, Average
Acceptance Criterion : ± 2° C
STATUS: PASS/ FAIL
FLOW RATE ACCURACY:
CARRIER GAS
Flow rate Set ( ml/min ):5 ml/min ,20 ml/min,50 ml/min.
Observations :
Acceptance Criterion: ± 2 % of the set value
HYDROGEN GAS
Set Value: 40 ml /min
Observation:______
Acceptance Criteria:± 2 % of the set value
ZERO AIR
Set Value: 400 ml /min
Observation:
Acceptance Criteria: ± 2 % of the set value
STATUS: PASS/ FAIL
Linearity test
Standard stock solution:
________mg ethanol, ________mg isopropyl alcohol, _________mg dichloromethane & __________mg ethyl acetate in 100 ml water containing 20 ml DMSO.
- Dilutions:-
- 25ppm :-
- 50ppm:-
- 100 ppm:-
- 200 ppm:-
- 300 ppm:-
- Concentration
- Response of Ethanol
- Response of Isopropyl alcohol
- Response of Dichloromethane
- Response of Ethyl Acetate
- Correlation Coefficient
- Acceptances Criteria: r ≥0.99
Repeatability Test
100 ppm:- Dilute________ml standard stock solution in 100 ml water.
Replicate injection
- Response of Ethanol
- RT of Ethanol
- Response of Isopropyl Alcohol
- RT of Isopropyl Alcohol
- Response of Dichloromethane
- RT of Dichloromethane
- Response of Ethyl Acetate
- RT of Ethyl Acetate
- Mean % RSD
% CARRY OVER
% carry over =( response of solvent in blank/average response of solvent in six repeatability injections) x 100
- Sr. No.
- Response of Ethanol in Blank
- % Carry Over
- Response of Isopropyl Alcohol in Blank
- % Carry Over
- Response of Dichloromethane in Blank
- % Carry Over
- Response of Ethyl Acetate in Blank
- % Carry Over
- STATUS: PASS/ FAIL
OPINION: INSTRUMENT IS SUITABLE/ NOT SUITABLE FOR USE.
NEXT CALIBRATION DUE ON: ——————-
Calibrated by/Date:_______ Approved by/Date:______Checked by/Date:______
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