Wednesday 25 July 2012

provide a procedure for the calibration of Gas Chromatography.

OBJECTIVE:                                                                                                                                    To provide a procedure for the calibration of Gas Chromatography.

SCOPE:  Applicable to the gas chromatography in Quality Control Department.Model              :CLARUS 500Manufacturer  : Perkin ElmerPROCEDURE: Calibration of carrier Gas Flow setting-Touch on “tool” at right hand corner of screen on instrument by using stick provided with instrument.Select option utilities.Touch on column flow calc.Enter column length, diameter, flow and column oven temperature; it will display required pressure to set by using carrier pressure knob. Column oven temperature calibration:Ware goggle and gloves while handling glass wool.Insert the calibrated digital thermometer from topside by piercing glass wool. Set column oven temperature on GC to 50°C, 100°C, 200°C, and 250°C.Allow to stabilise the set temperature for 5min and record temperature on digital thermometer at respective temperatures.Frequency - Once in three months.Detector calibration:Calibration of detectorAttach SS packed column of length 2 M x diameter 1/8 inch with stationary phase  10 % C-20 M (Ch-W/HP) 80/100 Prepare 1.0% v/v toluene solution in n-HexaneSet the chromatographic conditions as followsInjector temperature : 180°CDetector temperature : 220°CColumn flow                : 2.7 ml/minOven temperature       : 110°C (Isothermal) Run Time                     : 5 minutesInject blank and then six injections of 1.0% toluene solution in system and record chromatogram for all injectionsCalculate the RSD for the area of six 1.0 % toluene injections.The RSD should not be more than 15.0%Frequency - Once in six months.
COLUMN OVEN CALIBRATION:


Set temperature onGCOBSERVED TEMPERATURE ON DIGITAL THERMOMETERACCEPTANCE CRITERIA
50°c

        48-52°C
100°c

        98-102°C
200°c

        198-202°C
250°c

        248-252°C

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