CALIBRAITON PROCEDURE FOR GAS CHROMATOGRAPH CLARUS 500 WITH HEAD SPACE (Perkin Elmer)

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CALIBRAITON PROCEDURE FOR GAS CHROMATOGRAPH CLARUS 500 WITH HEAD SPACE (Perkin Elmer)

OBJECTIVE : To lay down the procedure for calibration of  GC  Clarus 500 with head space (Perkin Elmer )

SCOPE : This SOP shall be applicable for the GC Clarus 500 with head space (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
  • Acceptance criteria for 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 air flow 0 ml/min by GC control panel.
  • Note the flow of Carrier gas.
  • Repeat this process at 20ml/min and 50 ml/min.
  • Acceptance criteria for 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 air flow 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 0 ml/min by GC control panel.
  • Note the flow of zero air gas.
  • 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 Isopropyl alcohol, 200 mg methylene chloride and 200 mg of ethyl acetate in 100 ml volumetric flask containing 20ml 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 head space vial & seal
Linearity solution 25 ppm

Take 1.25 ml of solution(A), make the volume with purified water, take 1ml in HS vial & seal.
Linearity solution 50 ppm Take 2.5 ml of solution(A), make the volume with purified water, take 1 ml in  HS vial & seal.
Linearity solution 100 ppm Take 5 ml of solution(A) , make the volume with purified water, take 1 ml in

HS vial & seal
Linearity solution 200 ppm Take 10 ml of solution(A) , make the volume with purified water, take 1 ml in

HS vial & seal.
Linearity solution 300 ppm Take 15 ml of solution(A) , make the volume with purified water, take 1 ml in

 HS vial & seal

After conditioning the column set the system on the above parameters and inject 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

Correlation coefficient between concentration in ppm and 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 Isopropyl alcohol, 200 mg methylene chloride and 200 mg of ethyl acetate in 100 ml volumetric flask containing 20ml Dimethyl sulfoxide and dilute up to mark with purified water.

Take 1 Nos of 100 ml volumetric flasks previously cleaned and dried and mark 100 ppm.

Blank preparation                                       :              1 ml purified water in head space 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 :

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:

% Carry over =(area of solvent in blank / mean area of solvent in six repeatability injections) x 100

Acceptance criteria:

% Carry over for each solvent is not more than 0.01%

Record the observations in Annexure-I.

If instrument goes under maintenance, after service the calibration of the instrument to be conducted.

In case out of calibration display “OUT OF ORDER “ label and make an entry in instrument down time log book.

ANNEXURE I

CALIBRATION OF GAS CHROMATOGRAPH 

INSTRUMENT CALIBRATION FORMAT – GAS CHROMATOGRAPH CLARUS 500 WITH HEAD SPACE

LOCATION   CALIBRATION PROCEDURE NO.
MANUFACTURED BY   INSTRUMENT ID. NO.
MODEL NO.  

EFFECTIVE DATE

CLEANLINESS OF EQUIPMENT / INSTRUMENT BEFORE CALIBRATION:

SATISFACTORY/ NOT SATISFACTORY

 1. OVEN TEMPERATURE 

Sr.No. Set temperature Observations
Average
 Acceptance Criterion
Probe-1 Probe-2
1 50°C ± 2° C
    2 100°C ± 2° C
   3 200°C ± 2° C

 STATUS: ­­­­­­­­­­­­­­­­ PASS/ FAIL 

2.FLOW RATE ACCURACY:

CARRIER GAS

Sr.No. Flow rate Set

     ( ml/min )

 Observations  Acceptance Criterion
1 5 ml/min  

± 2 % of set value
    2 20 ml/min  

± 2 % of set value
   3 50 ml/min  

± 2 % of set value

HYDROGEN GAS 

Sr. no. Set Value Observation Aceptence Criteria
1 40 ml /min ± 2 % of set value

ZERO AIR

Sr. no. Set Value

Observation

 Aceptence Criteria
1 400 ml /min ± 2 % of set value

STATUS: ­­­­­­­­­­­­­­­­ PASS/ FAIL

3.Linearity test

Standard stock solution:

________mg ethnol, ________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
25 ppm r ≥0.99
50 ppm
100 ppm
200 ppm
300 ppm

STATUS: ­­­­­­­­­­­­­­­­ PASS/ FAIL

  1. Repeatibility 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
1
2
3
4
5
6
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: Checked by: Approved by:
Date      :  Date       :   Date           :

 

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