Step by step GCMS operating manualWord文档下载推荐.docx

1、 load the latest calibration file.Block 2.Create and save sample list.Block 3.Run the analysis.Block 4.Switch the machine into Stand by mode; switch off MS tune window. Block 5Analysis of chromatograms and data collecting.Block 6. Dont do.Block 1 Open/create project.When you start you can open your

2、existing project or create a new one. To open existing project do to File Open. Project is like a folder where your information will be stored.When creating new one go to File - Project Wizard.For new project fill in the Project name and press Next.Confirm Create new project and press Finish.Block 1

3、 Inlet methodOne the main window the bottom Shortcut should be pressed. You should see the following view with blue icons on the left.Press first icon Inlet method. It manages with chromatography part in GC-MS.Press on the icon with bottle （Inlet parameters）. You obtain the following window.Press th

4、e tab “Oven temperature ramp”Set up necessary parameters for chromatography （for capillary column）. Maximum temperature should not excide 280-300 C and be higher than boiling point of your analyte. If boiling point of your analyte is higher than maximum of capillary column your analyte wont come up

5、from the column and may even block the capillar. Use rump function when necessary. Maximum oven temperature is 325 C. Recommended starting temperature is 40-60C to cut off your solvent. Good solvent for the column are : hexane, benzene, THF, chloroform, DCM. Not acceptable solvents are water, acids

6、and alkalis （complete damage of the column）, DMF, DMSO.Then press the tab Back Injector. Confirm Gas saver Enabled; Flow 15 mL/min; time 6 min; Injector On. Set up temperature of injector （should be enough to evaporate your analyte should be higher than boiling point of analyte） and should not be hi

7、gh enough to destroy the analyte. Maximum possible injector temperature is 230-250C.Then go to File and Save as. Save the method with extension .h68. Inlet method should be saved in the folder ACQUDB in your project folder. All folders into your project folder are created automatically when you crea

8、te a new project. You can add “Inlet method” words in the name of Inlet method saved file for convenience.Block 1 - MS methodPress blue icon MS method. MS method manages with the work of mass detector （mass spectrometry part in GC-MS. If there is a blue line click blue line twice. You can see MS win

9、dow. If there is no blue line click type of method of mass detector MS scan. In the drop up window you should set up: start and end of mass scanning （recommended from 50 up to 600 Da. Time min: Start means time when your detector starts scanning. It starts not from 0 min but from 3.5-4 min because w

10、e need to avoid work of detector when solvent comes out. High concentration of solvent can damage detector. Therefore it start after 4 min when all solvent already came out from the column. End analysis should correspond to your Run time. You take this value （end of your analysis） from the tab of In

11、let method Oven temp rump （see above）. To see the end time your need click the bottom Run time. Inlet Method window can be closed after saving the Inlet file. In our case the length of analysis is 19 min. Ionization mode is E+; data processing Centroid; Scan time is 0.6 secs; Inter-Scan delay is 0.0

12、7 secs. After that press OK bottom （see below）. As a result you should see the window as shown below. Then go to Option Solvent delay.Reconfirm the delay time when your solvent come out from the column. It should correspond to the start of the analysis （see two pictures below）. In our case it is 4 m

13、in. Press OK.Then go to File and Save as the MS method with the extension .exp in the folder ACQUDB in your project folder （see below）. You can add MS method words in the name of MS method saved file for convenience.Block 1 MS Tune windowNext press MS tune blue icon at the left side of the main wind

14、ow. The windows as below is appeared.MS method window can be closed after saving the file. Now the machine is on Stand by mode. Press the bottom Press to Operate （right bottom corner）. Red color should be changed into green one （see below） Check Filament Current （A）. If it is close to zero press Rei

15、nitialize Filament bottom. The value of filament current should be about 5 A in normal condition （below）. Check whether computer can see the machine. Go to the Option Communication status. If the machine is “Not present” go to Option and click Reinitialize.Then load the latest calibration file. Go t

16、o File Open and choose the highlighted below file from drop up window 220711_MS1.ipr. （Should be in your subfolder ACQUDB in your project folder）. MS tune window should be all time open when doing analysis! Block 2. Sample list in the main window.You need to fill in File Name. Sample ID and File tex

17、t cells up to you （may be empty）. Click on the cell under MS method. Choose the MS file from drop up window.Highlight and confirm pressing Open bottom （Or just click twice on file name）. The cell of MS method in the line of your sample should be filled in like shown below. Do the same with Inlet met

18、hod. Click twice on the empty cell under Inlet method and choose the correct file from drop up window.The cell of Inlet method in the line of your sample should be filled in like shown below. Fill in the vial number in Bottle cell （number of your sample in the carousel autosampler）, and put 10 for I

19、nject volume cell. This is all information that is needed for analysis. You may insert necessary amount of lines clicking on the existing line and to choose Insert or Add.Or you can go to Sample tab and choose necessary command as well. When finishing sample list you need to save it. Go to File Save

20、 as. Block 3. Run the analysis.Check whether everything is ready. Highlight the lines of samples which you want to analyze （just clicking on it or clicking and dragging if many）. Then press icon Start up （Blue triangle）. Machine will ask to reconfirm or change the amount of sample in drop up window.

21、 Check the thick should be in Acquire Sample Data, and press OK.Machine will start analysis. Green color should appear on running sample line. Block 4. Switch the machine into Stand by mode; switch off MS tune window.When the machine is finish analyses press “Press to Standby” bottom. Green color sh

22、ould turn into red and Press to Standby should be changed into Press to operate.When you see the following picture （below） you can close the MS tune window. It will take some time （up to 10-20 seconds）. Block 5. Data analysis.Highlight the line of necessary sample （click on it once）. See below.Click

23、 on Chromatogram bottom and window with chromatogram of your sample is appeared.Right mouse click on the peak you want to analyze. Vertical line is appeared and you can see mass-spectrum window. Click on the library icon on the mass spectrum window to identify your chemical using library of mass spe

24、ctra. The following window is appeared automatically. You can see a list of chemicals that fit to you sample mass spectrum. The first one from the top in the list has all time the highest probability of fitting. Block 6. Dont do.Nota bene!Never close the main window of GC-MS （below）!Any other windows may be closed without interrupting GC-MS activity. Only MS Tune window can not be closed when analysis is running. And MS Tune window can be closed only after transferring into Stand by mode （red color window at the right bottom corner and no filament current or close to zero current value）.