1.1To lay down the procedure for operation of gas chromatograph (SHIMADZU GC-2010 with AOC-5000) system.
3.1Assistant – QC
3.2Executive – QC
4.0ACCOUNTABILITY:
4.1 Manager – QC
5.0PROCEDURE:
5.1GC System Configuration :
5.1.1Shimadzu GC System, GC-2010
5.1.2AOC 5000 Head Space Sampler and auto injector
5.1.3GC Solution Software.
5.2Ensure that the working bench and area is clean.
5.3 Always ensure gas line pressure is maintained above 4kg/cm2 in all gas supply lines.
5.4 Check for constant flow of carrier gas in the system.
5.5 Switch on the instrument.
5.6 Open the oven door and connect the required column.
5.7 Fixing the Capillary Column:
5.7.1 Insert the column end into the column nut and ferrule.
5.7.2 Ensure that the column ends do not have jagged edges or graphite contamination. If observed, cut the column ends using column cutter. Inspect the end for a clean break.
Position the column so that it extends above the end of the ferrule by 3 cm at inlet or injector side and 7 cm at detector.
5.7.4 Insert the column in the inlet and finger tighten the column nut, until it starts to grab the column. Then tighten the column nut-using wrench with gentle pressure, so that it cannot be pulled from the fitting.
5.7.5 After the column is installed at both inlet and detector, establish a flow of carrier gas through inlet.
5.7.6 Close the oven door properly; heat the oven, inlet and detector to the operating temperature.
5.7.7 Ensure oven door is always closed, when temperature is applied
5.8Switch on AOC-5000, CPU, and monitor.
5.9Wait for initialization and double click on the GC Real Time analysis icon.
5.10Double click on the LC solution icon, select the user ID and enter the password.
5.11Connecting the instrument ” shall be displayed with a beep sound and Real time analysis window appears
5.12To Create a new method:
5.12.1Click <File>,<Method>,<New> and current method is displayed with <Untitled .met>.
5.12.2Select the Advanced button in instrument parameter view.
5.12.3Click <SPL1>tab to display the (Injection unit).
5.12.4Enter injector temperature and select Injection mode as split mode.
5.12.5Select <Flow control mode> as Linear velocity and enter carrier gas pressure and split ratio. (Total flow and column flow will be recalculated and displayed based on these settings)
5.12.6 Select purge flow and enter the flow rate.
5.12.7 Click <Column oven >tab and set the initial temperature and sampling rate.
5.12.8 Enter the temperature programme in column oven temperature program.
5.12.9Stop time shall be displayed based on the time programme setting.
5.12.10Click <Redraw> to diplay the set temperature data on the graph.
5.12.11Click <Detector>tab and set the detector temperature.
5.12.12 Click <General> tab and enable <auto flame on >to ignite the detector flame automatically when the system gets into ready position.
5.12.13Enter the column length and ID dimensions in configuration of inlet
5.12.14Select open file in main tool bar and save method file with name.
5.12.15 Click down load method to proceed for analysis.
5.13 To install Head space syringe:
5.13.1Select <Menu> and press <F1/changsyr.>and injection unit moves to installation location.
5.13.2Place the plunger holder into the injection unit.
5.13.3 Place the syringe in the appropriate syringe adapter and pull the black plunger.
5.13.3If necessary, loosen the plunger screw in the red plunger holder.
5.13.4Move the syringe installed in the heated syringe adapter partially into the injection unit guide the needle first into the lower needle guide.
5.13.5Place the black plunger button into the red plunger holder. Press the syringe adapter against the syringe carrier until it sits flush on the carrier.
5.13.6Tighten the plunger screw against the plunger button.
5.13.7 Press “HOME” to return syringe into normal position.
5.14 To create Head space injector Method:
5.14.1 Press menu and select the method.
5.14.2Select <F2/insrt.meth.>and enter the new method name using rotating knob.
5.14.3Press the <F4/enter>tab and select cycle HS-Inj.
5.14.4Specifiy the syringe to be used in the method.
5.14.5Scroll and assign parameter values according to the application requirements.
5.14.6Press <F4/Home function> key
5.15 To create Job Queue:
5.15.1 Select <F2/Add Job> and select insert mode Append.
5.15.2 Select the tray name.
5.15.3 Enter the first and last sample number for this job.
5.15.4 Select and enter the sample processing method for this job
5.15.5Press the F4/ Home function key
5.16 Preparation of sample (For HSS):
5.16.1Transfer specified quantity of sample/sample preparation into the vial.
5.16.2 Ensure that the headspace vials do not have jagged edges, to avoid leakage of vapour.
5.16.2Seal the vials with crimp caps tightly and confirm that caps do not rotate after crimping.
5.17 To install Liquid syringe:
5.17.1 Select <Menu> and press <F1/changsyr.>and injection unit moves to installation location.
5.17.2Place the plunger holder into the injection unit.
5.17.3Move the syringe installed in the heated syringe adapter partially into the injection unit guide the needle first into the lower needle guide.
5.17.4 Place the blue plunger holder into the injection unit.
5.17.4Place the syringe in the appropriate syringe adapter pull the plunger. If necessary, loosen the plunger retaining screw in the red plunger holder.
5.17.5Move the syringe installed in the syringe adapter partially into the injection unit. Guide the needle first into the upper needle guide and the into the lower needle guide.
5.17.6Place the plunger button into the plunger holder. Allow the syringe adapter to dick into place by magnetic force, against the syringe carrier.
5.17.7Tighten the plunger retaining screw against the plunger button.
5.17.8Press “HOME” to return syringe into normal position.
5.18 To create Liquid injector Method:
5.18.1 Press menu and select the method.
5.18.2 Select <F2/insrt.meth.>and enter the new method name using rotating knob.
5.18.3Press the <F4/enter>tab and select cycle GC-Inj.
5.18.4Specifiy the syringe to be used in the method.
5.18.5Scroll and assign parameter values according to the application requirements.
5.18.6Press <F4/Home function> key
5.19Preparation of sample (Liquid injector):
5.19.1Transfer specified quantity of sample / sample preparation into the vial and close with screw cap.
5.19.2Position the sample vials to be injected only in the vial tray labeled from 1 to 98.
5.19.3Ensure rinsing solvent is filled in another vial, where mostly diluent is used.
5.19.4Position the rinsing solvent vial in Wash1 in the wash station. If the second rinsing is required, then position the vial containing second rinsing solvent in the Wash 2.
5.19.5Place empty vials in waste1 and waste2 wash station.
5.20Procedure to create and run Batch file:
5.20.1Click <Batch processing> icon and select <Batch table Wizard> icon to display batch table wizard Screen.
5.20.2Click<new batch table>, select required method file and then click <Next>tab.
5.20.3Select the number of sample groups and click <Next>tab.
5.20.4Select the calib levels, Repetitions, Vial, Sample name, sample ID and then click Next button.
5.20.5Select the Data file name, Report file name then click Next button.
5.20.6Click Finish button. Appear prepared batch table if any changes required made changes and then go to main tool bar, open File and select save batch file.
5.20.7 Place the sample vials in specified tray and click start icon. Simultaneously press AOC-5000 auto injector F4/Start function key.
5.21To acquire single run:
5.21.1Click <single run> icon, and sample login screen shall appear.
5.21.2Enter the sample name, sample ID, specify the data file, vial number and click <OK>.
5.21.3Inject required quantity in the injection port and press <START> button on key board menu of the GC .
5.22 Post run analysis:
5.22.1 Click on [Data Analysis] icon on the [Acquisition] page of the Assistant Bar.
5.22.2The <GC Data Analysis> window in the <GC Postrun> program shall be displayed with the previously obtained data file loaded.
5.22.3In the <GC Data Analysis> window, open the data file created from the analysis using the [File] menu or <Data Explorer>.
5.22.4When the data file is opened, the chromatogram shall be displayed.
5.22.5Right click on the chromatogram and select [Data Analysis Parameters] menu.
5.22.6Select <Integration> tab and enter the values of width, slope, drift, TDBL, Minimun area/Height to optimize the integration parameters.
5.22.7 Click <apply> and the chromatogram gets integrated with optimized parameters.
5.22.8Save the integration parameters as a part of the method file < click Apply to Method in the Assistant bar>. Make sure the method file is not used for analyses in the real-time and run is going.
5.23 After completion of analysis load cool method to cool oven temperature, injector temperature, detector temperature, vials temperature and syringe temperature to room temperature.
Gas chromatograph, tighten, injection, magnetic force
