sop for Operation and calibration of gas liquid chromatograph

1.0. OBJECTIVE:

The objective of this SOP is:
1.1 To lay down a procedure for the operation and calibration of Gas Chromatograph (GC).

2.0. RESPONSIBILITY:

Officer/Executive – QC

3.0. ACCOUNTABILITY:

Head – Quality Control

4.0. PROCEDURE:

4.1 Connection Of Analytical Column In Column Oven In GC:

4.1.1 For glass columns use PTFE ferrules with hexagonal nuts or O-ring seals with round nuts to be tightened by hand.
4.1.2 For metal columns use double brass ferrules and hexagonal 1/4” column fixing nuts.
4.1.3 Insert the ends of the column as required into injector and detector base body.
4.1.4 Do not use spanners to fit the glass column.
4.1.5 Check the fittings leak with soap solution.
4.1.6 Check the flow with the help of soap bubble flow meter on the detector base body.
4.1.7 For capillary columns, position the column inside the oven on the column support in such a way that the correct alignment of limbs with detector and injector us easily obtained.

4.2 Performing the Leak check of carrier gas.

4.2.1 Ensure all other gas lines are closed.
4.2.2 Ensure all exits from the Chromatograph are closed. Use blanking caps provided for the detector base body, HWD outlets and SSL valves as appropriate.
4.2.3 Adjust the carrier gas pressure to 100-200 kPa with help of regulator in instrument.
4.2.4 Turn off carrier gas supply at the cylinder or other convenient position.
4.2.5 See that the pressure of all gauges remains unchanged for at least 3 minutes. Then be sure that the system is leak tight.

4.3 Operation Of Temperature Control Unit

4.3.1 Before starting the instrument check the following carefully.
4.3.2 The correct column is properly installed and conditioned.
4.3.3 Ensure Oven temperature limit is correct see.
4.3.4 Ensure sufficient gas supply of N2 gas, H2 gas and Zero Air.
4.3.5 All external connections are plugged in.
4.3.6 Injector septum where appropriate, is in good order.
4.3.7 Switch ‘On’ the control unit powder supply.
4.3.8 Switch ‘On’ the control unit at the front and rear. Display will light after beep.
4.3.9 “PROG MEM” will appear after 5 sec. And will show the current parameter file e.g‘ PO’.
4.3.10 Keyboard of control panel can be operated by two modes 1. “Direct mode of data entry” 2. “Indirect Mode of data entry”.
4.3.11 Switch “ON” the GC from back & front on/off Switch.
4.3.12 Check the display on front panel
4.3.13 Check functioning of keyboard by entering your require program.
4.3.14 Enter OVEN Temperature in Set valve of SB ISO 1for initial temperature &* ISO 2for final temperature.
4.3.15 Enter Injector temperature in set value of ZONE 1.

4.3.16 Enter Detector Temperature in set valve of Zone 2 & Zone 3.
4.3.17 Check all temperature by pressing Actual key.
4.3.18 Adjust flow of Hydrogen 35 ml/min. and Air 350 ml/min.
4.3.19 Ignite the flame.
4.3.20 Wait for ready status of GC.
4.3.21 Start Chrom – Card Software & check Baseline in view.
4.3.22 Zero the Base line by pressing Auto zero key.
4.3.23 Open/ prepare require method in Main Menu.

4.4 Calibration:

4.4.1 Temperature Calibration:
4.4.1.1 Set the measure Oven temperature, Injector temperature & Detector temperature as per operation procedure.
4.4.1.2 Calibrate measurement temperature with help of temperature sensor and record the details in Annexure – 1.
4.4.1.3 Frequency: Six Month

4.4.2 Flow Calibration:

4.4.2.1 Connect the flow meter to the column port and operate the Gas Chromatograph as per SOP.
4.4.2.2 Check the leak test by help of soap solution.
4.4.2.3 Measure the flow by using the flow meter.
4.4.2.4 Details note in Annexure – 2
4.4.2.5 Frequency: Six month

4.4.3 Detector Calibration:

4.4.3.1 Calibrate the Detector by using of IPA (Isopropyl Alcohol).
4.4.3.2 Set the temperature of oven, injector and Detector as per Operation procedure.
4.4.3.3 Set Flow rate as per Operation procedure.
4.4.3.4 Ignite flame by help of ignite key.
4.4.3.5 Injected 0.1 µl of IPA in triplicate and note down in Annexure – 2
4.4.3.6 For above both Tolerance Limit of max. 5%
4.4.3.7 Frequency: Six Month

4.4.4 Affix a calibration status label on the instrument containing “Calibrated On”, “Due On” and “Signature”.
4.4.5 Report to Head – QC, if any discrepancy observed during calibration or operating the instrument and affix ‘Under Maintenance’ label on the instrument.

4.4.6 In case of calibration failure, follow the procedure given in SOP

5.0. REASON FOR REVISION:

The SOP is revised to specify the System suitability test and incorporating the bracketing of standard after 10 injections.

6.0 TRAINING:

Trainer — Head – Quality Control
Trainees — Quality Control Chemists and Assistants

7.0 DISTRIBUTION:
Certified Copy : Quality Control
Reference Copy : Display copy Near Gas Chromatograph
Reference Copy : File copy in Gas Chromatograph Calibration Record
Original Copy : QUALITY ASSURANCE.

8.0 ANNEXURES:

Annexure – 1 : Format For Calibration Record Of Temperature
Annexure – 2 : Format For Calibration Record Of Flow Rate and Detector

9.0 REFERENCES:

In house.