Tuesday, December 14, 2010

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



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