Calibration Of Gas Chromatograph

Instrument :  Gas Chromatograph

       

        Make           :  Shimadzu

       

        Model          :  GC-2010

       

        Date of calibration         : 

       

        Next calibration due on  :

       

        A.  UPKEEP OF INSTRUMENT:

       

        Instrument is clean and free from dust

CHROMATOGRAPHIC CONDITIONS

Parameters	Test condition
Column	Rtx 624 (30m × 0.53mm, 3µm) or equivalent
Oven temp. program	40 ºC-3min-@30 ºC/min-220 ºC-6 min
Detector Temperature	220 ºC
Injector Temperature	240 ºC
Head Pressure	20 Kpa
Linear velocity	31.0 cm/sec
Injection Volume	1 ml Gaseous phase
Equilibration Temperature	105 ºC
Transfer line Temperature	110 ºC
Equilibration Time	20 minutes
Run Time	15 minutes
Split Ratio	1 : 10

I)            (a)  Retention Time repeatability :   

                                                                                           

Run #	Observed Retention Time (RT)		Acceptance criteria
	Iso Propyl Alcohol (IPA)	Tetrahydrofuran (THF)
Run-1			(% RSD: NMT 1.5 %)
Run-2
Run-3
Run-4
Run-5
Mean
% RSD

     

Conclusion:

  (b)  Area Repeatability:

Run #	Iso Propyl Alcohol (IPA)	Tetrahydrofuran (THF)	Acceptance criteria
Run-1			(% RSD: NMT 15 %)
Run-2
Run-3
Run-4
Run-5
Mean
% RSD

         

      

               Conclusion :

II)          Linearity :

Make triplicate injection of each injection volume. Draw the linearity curve as concentration vs. area.

      For Isopropyl alcohol (IPA)

Area	Concentrations(ppm)
	500	400	300	200	100
Area 1
Area 2
Area 3
Mean

 Result:

Coefficient of correlation :

Limit: Not less than 0.99

Conclusion:

For Tetrahydrofuran (THF)

Area	Concentrations(ppm)
	72.0	57.5	43.1	28.7	14.4
Area 1
Area 2
Area 3
Mean

      Result:

Coefficient of correlation:

Limit: Not less than 0.99

     Conclusion:

II)                Temperature calibration for GC

         Following parts will be calibrated at the temperature points indicated.

a)    Column Oven Temperature :

Set Temp.  (ºC)	Measured Temp.(ºC)	Limit(ºC)	Remarks
50		±3.2
100		±4.2
200		±5.5
300		±5.5

            

b)       Injector Port Temperature:    

Set Temp.  (ºC)	Measured Temp.(ºC)	Limit (ºC)	Remarks
100		±4.2
200		±5.5
300		±5.5

c)       Detector Port Temperature:

Set Temp.  (ºC)	Measured Temp. (ºC)	Limit (ºC)	Remarks
100		±4.2
200		±5.5
300		±5.5

   

d)    HT 200HT Incubator Temperature:    

Set Temp.  (ºC)	Measured Temp. (ºC)	Limit (ºC)	Remarks
50		±3.2
100		±4.2
150		±5.5

         

Acceptance criteria: The temperature should be within the specified limit.

Carrier gas flow calibration:  

    Flow will be calibrated using digital flow meter at room temperature.

a) Column flow for packed column:    

Set column flow in ml/min	Measured column flow in ml/min	Limit in ml/min	Acceptance criteria
20.0		18.0 to 22.0	For 20 and 30ml/min limit is ±10% For 50ml/min limit is±20%
30.0		27.0 to 33.0
50.0		40.0 to 60.0

Conclusion:

b) Column flow for capillary column:   

Set column flow in ml/min	Measured column flow in ml/min	Limit in ml/min	Acceptance criteria
2.5		2.25 to 2.75	±10%
5.0		4.5 to 5.5

Conclusion:

c) Split flow for capillary column:

Set split ratio	Set column flow in ml/min	Total flow in ml/min	Measured flow in ml/min	Limit of flow in ml/min	Acceptance criteria
1:5	2.0ml/min	10.0ml/min		8.0 to 12.0	±20%
1:10	10.0ml/min	100.0ml/min		80.0 to 120.0

Conclusion :

Calibration Status: Satisfactorily/ Not Satisfactoril

Remark: Hence the instrument stands/does not stands calibrated w.r.t.

1.     Detector Precision.

2.     Detector linearity.

3.     Temperature Calibration.

Flow Calibration