This document provides quick and easy operational guidelines for GCMSsolu- tion
This document provides quick and easy operational guidelines for GCMSsolu- tion Ver. 2.6. Please keep this document beside your GC/MS in order to quickly confirm operational procedures. For more detailed operational procedures, please refer to the "Gas Chromatograph Mass Spectrometer GCMS-QP2010 Series Operation Guide for GCMSsolution Ver. 2.6". Quick Navigation For (GCMS-QP2010 Ultra / SE) 225-18487 Quick Navigation GPS ($.4216MUSB4& Daily Startup and Shutdown Executing Autotuning *1 Execute autotuning after creating the method file if it has not already been created. *2 Whenever autotuning is executed, calibration curves must be newly created. GCMS Data Acquisition Program GCMS Data Acquisition Program r-PBEJOH%BUB"DRVJTJUJPO$POEJUJPOT Check that the window is the [Acquisition] sub-window. Load the method file to be used. The setup parameters are sent to the instrument. The instrument is ready if the values are the set values. Open the [Tuning] sub-window. /P 0QFSBUJPO $IFDL %PVCMFDMJDL $MJDL $IFDL $MJDL %FTDSJQUJPO Turn the CRT ON. Cancel the ecology mode. /P 0QFSBUJPO 0/ $MJDL %FTDSJQUJPO *3 To check the results of autotuning, refer to the Operation Guide "2.7.3 Checking Autotuning Results". r&YFDVUJOH"VUPUVOJOH %FTDSJQUJPO Open the [Peak Monitor] sub-window. Create a new tuning file. Select the tuning mode. Select the filament as required. Start autotuning. Enter the file name. Save the tuning file. Check the report that is output.*3 /P 0QFSBUJPO $MJDL $MJDL $MJDL $MJDL $MJDL *OQVU $MJDL $IFDL 1 2 Please do not shut down GC/MS system because several hours will be required for starting-up. The PC can be switched off except during analysis. The CRT can be switched on and off whenever required. Set the method file you are going to use for the analysis. After the GC/MS system is ready for the analysis, perform autotuning.*1*2 Quick Navigation GPS ($.4216MUSB4& Creating Folders Performing Data Acquisition Files with file types in the figure on the right will be created after analysis. Create a new folder in order to save those files in the same folder. *1 For details on how to edit batch table, refer to the Operation Guide “4.3.2 Editing a Batch File”. *2 This setting can be cancelled by repeating operation 5, but always leave it set. GCMS Data Acquisition Program GCMS Data Acquisition Program Check that the window is the [Batch Table] window. Open the batch file to be used. Check and edit the batch table.*1 Overwrite and save any edits. The instrument enters the ecology mode after data acquisition ends.*2 Set the rinsing solvent and sample in place. Display the confirmation message. Start data acquisition. Cancel data acquisition. /P " 0QFSBUJPO $IFDL %PVCMFDMJDL $IFDL $MJDL $MJDL $IFDL $MJDL $MJDL $MJDL %FTDSJQUJPO Open the [Create New Project (Folder)] sub-window. Enter the folder name. Select the files to copy to the new folder. The new folder is created.*1 /P 0QFSBUJPO $MJDL *OQVU $MJDL $MJDL %FTDSJQUJPO *1 A new folder is created on the same level of the currently opened folder in Data Explorer. For detailed procedure to open the target folder, please refer to the Operation Guide "Appendix C Using Data Explorer". 3 4 Please modify the previously created batch file for easy operation. For details on how to create method files and batch files, refer to the Operation Guide “4.1 Creating a Method File”, “5.1 Creating a Method File”, “4.3.1 Creating a Batch File”and “5.2.1 Creating a Batch File”. Data file File type Icon Method file Report format file Batch file r%JTQMBZFE*DPOT BOE'JMF/BNFT " Quick Navigation GPS ($.4216MUSB4& Data Processing for Qualitative Analysis GCMS Postrun Analysis Program Display the mass spectra for chosen peak and perform library search. Register the results in the spectrum prodcess table. It allows referencing the results later or printing out the report. Select the created folder. Open the data file. Display the peak enlarged. Display the mass spectrum of the peak top. Switch to the background processing mode. Perform background subtraction. Open the [Similarity Search Results] sub-window. The searched compounds are switched. Check while comparing the compounds. Select the compound considered to be correct. Register the selected compound to the spectrum process table. Close the [Similarity Search Results] sub-window. Repeat these operations to register all target components. Open the qualitative table. Maximize the table. Select the row to edit. Edit the row (e.g. correct compound name). Close the qualitative table. Overwrite and save the data file. Create a report.*1 $MJDL %PVCMFDMJDL %SBH %PVCMFDMJDL $MJDL %PVCMFDMJDL $MJDL $MJDL $IFDL $MJDL $MJDL $MJDL 0QFSBUJPOTUP $MJDL $MJDL $MJDL $MJDL $MJDL $MJDL $MJDL Check that the window is the [Data Analysis] window in the qualitative processing mode. $IFDL Start up the [GCMS Postrun Analysis] program. /P 0QFSBUJPO %PVCMFDMJDL %FTDSJQUJPO 5 *1 For details on how to create reports, refer to the Operation Guide “4.5 Printing Qualitative Analysis Reports”. Displayed spectrum Searched compounds Searched compounds At peak top At peak tailing edge The range dragged with the mouse is displayed enlarged in the MC window. Quick Navigation GPS ($.4216MUSB4& Data Processing for Quantitative Analysis GCMS Postrun Analysis Program Create a calibration curve and calculate the concentration of target compounds. *1 For details on how to create reports, refer to the Operation Guide “5.4 Printing Quantitative Analysis Reports”. Start up the [GCMS Postrun Analysis] program. Check that the window is the [Calibration Curve] window. Select a created folder. Open the method file used for data acquisition. Check the calibration curve of the target component. Check the chromatogram of the target component.*3 Perform manual peak integration and manual identification as required.*2 Overwrite and save any corrections. /P 0QFSBUJPO %PVCMFDMJDL $IFDL $MJDL %PVCMFDMJDL $MJDL $MJDL .PEJGZ $MJDL %FTDSJQUJPO Check that the window is the [Data Analysis] window in the quantitative processing mode. Open the data file. Load the method file used for creating the calibration curve. Perform quantitative peak integration. Check the quantitative results. Select the target row. Check the chromatogram of the target component.*3 Perform manual peak integration and manual identification as required. Overwrite and save the data file. Create a report.*1 /P 0QFSBUJPO $IFDL %PVCMFDMJDL $MJDL $MJDL $MJDL $MJDL $IFDL .PEJGZ $MJDL $MJDL %FTDSJQUJPO 6 *2 For details on manual peak integration and manual identification, see page 9. *3 The peak integration and peak detection are automatically performed on the chromatogram ( peak detection marks). Detected peaks are identified based on retention times and ion ratios ( identification mark). r$IFDLJOHBOE.PEJGZJOH$BMJCSBUJPO$VSWFT r2VBOUJUBUJWF$BMDVMBUJPOPG6OLOPXO4BNQMFT Identification mark Peak detection marks Quick Navigation GPS ($.4216MUSB4& GCMS Data Acquisition Program Open the popup menu. Switch to the manual peak integration mode. Specify the start and end of the baseline. Select the baseline. The peak is integrated and identified. /P 0QFSBUJPO 3JHIUDMJDL $MJDL %SBH $MJDL $MJDL %FTDSJQUJPO Open the popup menu. Switch to the manual identification mode. The peak is identified. /P 0QFSBUJPO 3JHIUDMJDL $MJDL $MJDL %FTDSJQUJPO Open the [Vacuum Control] sub-window. Start automatic stop. [Completed.] is displayed. Close the [Vacuum Control] sub-window. /P 0QFSBUJPO $MJDL $MJDL $IFDL $MJDL %FTDSJQUJPO Appendix. Performing Maintenance "Easy sTop" is a convenient function for exchange of septum and insert. It shortens the period for stabilizing the GC/MS system after the exchange. Perform maintenance referring to the Operation Guide "Appendix D Maintenance" or MS Navigator. r4UPQQJOHUIF7BDVVN4ZTUFN Open the MS Navigator. Display the maintenance procedure for the selected part. Perform maintenance as described in the procedure. /P 0QFSBUJPO $MJDL 4FMFDU $IFDL %FTDSJQUJPO r4UBSUJOH6Q.BJOUFOBODF)FMQ Thoroughly rinse with solvent before data acquisition. Replace every 100 data acquisitions. During operation Easy sTop Easy sTop Vacuum system stopped Vacuum system stopped Vacuum system stopped Replace every 3000 hours of operation. /P .BJOUFOBODF*UFN 4ZSJOHF 4FQUVN *OTFSU $PMVNO 'JMBNFOU 0JMGPSUIFSPUBSZQVNQ 3FDPNNFOEFE3FQMBDFNFOU$ZDMF *OTUSVNFOU4UBUF r.BJO.BJOUFOBODF1BSUTBOE'SFRVFODZPG.BJOUFOBODF ·Replace when the trap current insufficient message is displayed. ·Replace burned out filaments. ·Replace according to the injection mode (split, splitless). ·Replace when the peak shape has deteriorated or peak intensity has decreased. How to Perform Manual Identification How to Perform Manual Peak Integration ·Check separation between the target component and other peaks, and replace the column with the ideal column. ·Perform maintenance when the peak shape has deteriorated or peak intensity has decreased. uploads/s1/ gcmsquickguide-shimadzu.pdf
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- Publié le Jul 27, 2021
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- Langue French
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