User manual Saturn GC-MS
Contents
1. TARGET SCAN RANGE 22300 Lo mass Hi mass 58 658 AGC Editing the analysis list PAY ATTENTION E File Control Autosamp ler Util Never remove the samples that already have been Analysis List Editor measured This is essential information for the s100K TAN system operators to determine the replacement of Uitstoken sem septa 50 injections and precolumn 200 D GA TURIN METHODS WEEKS injections Select Go to the analysis screen shown on the right e a im lt 1 TE e A Analysis The screen exists of a list that el o_o has per line one sample or injection Every week a new list is made e g WEEK45 amp WEEK46 Add Expand Del UnDel DelAll PgDn File Control Autosamp ler Util Analysis List Editor D NSCHEERENNBERKOMN e With ADD or EXPAND bottom of screen ExPI2 you can expand or add to the list with EDIT ee and SELECT you can make changes to lines D SATURN HETHODS WEEK 46 6 that are already in the list yellow highlighted line is active the gray background tells which item is EDITed or EXP153 1 0_18 4 11 AA 1 008 IEXP31 2 0_18 4 11 AA 1 080 SELECTed GEXP13 2 0 18 4 11 AA 1 008 0_16 4 11 AA 1 888 STOOK 81 0_18 4 12 STOOK STOOK 1 006 Add Expand Del UnDel DelAll PgUp PgDn e Always check the PATH so the data files m File Control futosampler Util Analysis List Editor are stored in the right direction and D SCHEERE further fill in SAMPLE code of the LEON sample OPERATOR2. who is doing this analysis COMMENTS name date Varia ae concentration solvent code DATAFILE PAY ATTENTION This system contains the Old MS_DOS filename convention 8 3 this means that you OK Cancel can only use 8 positions for the data filename it is the best to use your sample code and reserve a position for a number in case you want to make multiple injections from the same vial Add Expand Del UnDel DelAll Home PgUp Press on SELECT to select Auto Sampler Method m File Control futosampler Util Analysis List Editor VIAL number GC Method and MS Method see D SCHEEREN BERKOMN screen on the right First highlight the correct line LEON with your sample and click on SELECT Ee ALWAYS insert a STOOK run after your last week E oe sample to make sure that the people that measure OK after you do not get problems like memory effects IExP31 2 010 4 B 1aa 1 eae GEXP13 2 0_16 4 11 AA AA 1 6660 1 606 or contaminations of the column At the same time the system will return to normal STANDBY situation at the end of the run 4 11 STOOK 61 0_18 4 12 STOOK STOOK 1 888 1 888 Add Expand Del UnDel DelAll PAY ATTENTION Stagt Autosampler Run PA1 Petis Tsi wai Yuen 611126 PA1 58ng ul CHC13 PA1 2 D NSA TURNNME THODS WEEK47 Varian 8160 4 eal 2 Pat 018 1 1AA aA After you have completed your analysis list start 4 STOOK 1 0_18 4 12 STOOK STOOK the analysis on one
3. OK 82 MS 724688 68 29 61 PAY ATTENTION SOHEEREN At this point you cannot extract your chromatogram Ea to a floppy disc you have to wait until the TANZANIA acquisition is completed The system gives the ZUANENBU highest priority to writing to the hard disc and OLTE ORNES there can perform no disk IO during acquisition HUAKABOK POONAM Go to e F File Manager and select the correct data file EES E Mester acai by highlighting and press ENTER cae Bc AA aon ae Tag Name Size Date e Press function key F2 and insert the desired scan Xi PA1 1 S_ 423985 11 28 01 PA1 2 MS 465687 11 20 61 area Chro Plot Range to go to the chromatogram EXPPLANT TIC EXTERNEN Chro Plot Range Plot From Scan 1 If you only have measured one sample and it has you can go directly to the TIC with C Chromatogram from the main screen On the bottom of the main screen on the right you can see the active data file Acquisition Status You always have to select your data file before you can open it in Chromatogram PAY ATTENTION S h h A are S hromatogram Plot D NGALNTHEONPA 1 2 Date 11720701 16 48 32 omment Tsi wai Yuen 611126 PA1 58ng ul CHC13 et t e system to t e cquisition tatus screen Scan No 908 Retention Time 15 66 RIc 4992 Mass Range 35 355 Plotted 245 to 1566 Range 1 to 1888 166 30761291 before you leave Otherwise the System stops after 2 the active run and the analysis list will not be completed The Mass S
4. User Manual varian SATURNS varian Revision C 68 Nov 2661 Thurs day 13 38 SATURNSE System operators Peter M van Galen D SCHEERENNBERKOMN EXP149 1 MS 128008 e o C NSATURNNLBRN NIST LBR 49472 Hel ene I V Amatdjais Groenen C NSATURNNPROCEDURN DEMO PRC 6 C SATURNN 6321 1B SPL 8 R Version 1 3 1 2004 02 11 23886 KB Free 295536 KB Free Please check the following before you start with the measurements e Check if there is enough solvent in the bottle besides the auto sampler and if the waste bottle is not to full please empty in a waste container e Check if the pressure of the Helium is at least 50 bars at 30 bars the operator has to replace the cylinder e Check the pressure on the GC column 14 15 PST e Check on or whether the right standby temperatures are displayed alumn 110 ector imag 4 e Check if the computer is on and the program Saturn active is normally the main menu is displayed Make a solution of 5 mg ml of your sample and inject ona GC with the most suitable column normally a HP 1 or similar column and method Gives this a good chromatogram then make the dilution from this solution Dilute in the ratio of 1 100 with preferably toluene and transfer it to the vial make sure the septum is placed in the right way with the red side down Do not use the GCMS for optimalisation Never use labels on the vial because the injection Control Adjustments Status ___Ra
5. is displayed on screen press F4 to normalize all plots to the highest peak in each plot 11 26 61 16 46 32 35 333 36761291 11 26 61 16 46 32 35 355 36761291 e The peak list or mass table Background Subtract D GALNTHEONPA1 2 Date 11 20 81 16 40 32 omment Tsi wai Yuen 611126 PA1 5 ng ul CHC13 Average of 1133 to 1137 Minus 1126 to 1138 104 39535 168 167 A mass table is available for any scan in the chromatogram by pressing F3 or on M in the T spectrum Then the mass table is shown of the scan where at the place of the cursor the active spectrum Usually but not necessary a spectrum or a mass table is taking at the top of the peak 65 77 228 51 32 135 182 199 333 46 68 88 100 126 148 168 188 200 226 248 268 288 300 328 340 368 Shp Fo bKg ass List Bkg Sub Spectrum D GALNTHEONPA1 2 Date 11 26 61 16 46 omment Tsi wai Yuen 611126 PA1 5 ng ul CHC13 Average 1133 to 1137 Minus 1126 to 1138 Mass Range 35 341 it Peaks 139 Mass of Base Peak Int 39535 Threshold 6 85 Mass Intensity zxz Base Mass Intensity z Base Mass Intensity xz Base 333 29 8 87 128 218 8 53 146 8 37 Like the table that is shown on the right the mass table is normally too big for one screen With the 1698 188 Page Down key PgDn you can scroll the table but this is not handy Often you re only interested in the most abundant peaks so instead of taking several screen dumps you can use the f
6. nges 1606 Chehk For Air Water needle could be bent when the vial gets stuck A new needle costs Checking the status of the MS Go to e I Instrument control See screen on the 108 158 208 258 300 ge LE PY y right AUTO SETUP MASS CALIB e SETUP CHECK for Air Water and nce Normalize the spectrum by clicking N next i to the Y axis AGC Control Ad justments Setup Status Ranges 124 885 305 usec The screen you see must look roughly like the one you see on the right 100 lt 4056 Air OK Water OK ratio 28 32 lt 4 1 28 width 0 8 19 18 ratio 10 otherwise there is a problem In case of a problem contact one of the system operators Control Ad justments Setup Status Ranges 1660 1243 24999 usec Then turn on the MS by clicking in the middle of the schematic view of the ion trap FILament RF and MULTiplier will be highlighted Normalize and look at the spectrum 188 158 208 258 388 608 MULT 27808 AUTO SETUP MASS CALIB TARGET SCAN RANGE 22300 Lo mass Hi mass 58 658 AGC The following values must be checked e Ionization time 24999 psec or 25 msec asa aa Tonia 24099 aise if this gives a smaller value it means the Ion trap is becoming contaminated e That the Total Ion Current TIC is low normally 2500 e That the 100 value is low a few honderd normally lower than 100 188 158 288 258 388 548 558 608 MULT Ape 2788 AUTO SETUP MASS CALIB
7. o save more than one data file at once press on T ag to select the desired data files
8. of the following ways CONTROL Start Auto sampler Run if you want to start a new series of runs CONTROL Continue Acquisition Run if there s ada Expand Det Unbet perar PgDn Ena still a analysis running they must be finished before you can start another According to our policy it is prohibited to start a new series of runs when there is already a series running SATURN Tasker Revision H Background acquisition is inactive Please use the Acquisition Sequence Editor to start a background acquisition any key to continue You can view the STATUS of a running analysis by clicking on AQUISITION STATUS in the main screen of the SATURN program or with U Acqu Status Than a screen is shown on which you can see what analysis is running and how long it still has to run When a series of analysis have to be measured always set the system on this screen before you leave Otherwise the System stops after the active run and the analysis list will not be completed Manage the results from the chromatogram TIC Total Ion Current During acquisition it is possible to look at the File Manager Default D NSATURNSDATANDEMO MS Date 10 19 92 Comment Demo Data 86 PPB Organics In Water Purge amp Trap 6 53 mm DB results of the measurement you can derive mass ESNE Search Path D SATURNNDATAN Tag Name Size Date spectra from the chromatogram TIC and RUTJES DENO MS 54484 18 19 92 eventual ly print them Ea STO
9. pectrum of a peak can be retrieved on two different ways 1 Go to the top or near the top of a peak with the arrow keys and press function key F1 The Aoo n spectrum that is displayed is not corrected a 388 6668 988 1266 for background 5 88 18 88 15 88 28 88 F1 Spee r2 GRE F3 MSA r4 Monn FS DESRISSaReH F PESH Fs PEE F10 MaA 2 Go to the top of the peak and at the same time press the control key B The spectrum that then is displayed is automatically corrected for background You can also correct the spectrum for background hromatogran Plot D GALYTHEONPAI Z Tsi wai Yuen 611126 PAI 5 ng ul CHC13 1135 18 55 153243 manually this is useful when there are shoulder peaks SASAE 1 to 1888 present or when the peaks are close together Go to the top of the peak and press control key B now select the beginning and the ending of the peak Then select the area to be used for the background subtraction If there are many peaks it is not always clear which onment Tei wai Yuen 611128 Pal S ng gt ul CHC13 872 14 32 5279 peak is the main product then you can make a plot of Sr a the chromatogram together with expected ions from your compound as follows e Press D Display and select the desired scan area e g 45 to 1500 see left screen in the header e Insert the desired numbers of traces ions plus TIC e g 4 respectively TIC 93 105 en 228 expected MH auto CI effect of the Ion trap e After the plot
10. unction keys at the bottom of the screen e g Fl 1 th Threshold of 1 cut off peaks lt 1 ECEE 0 10 i F5 5 th Threshold of 5 cut off peaks lt 5 F6 init sort Sort initial table on mass peak intensity F9 bkg sub Subtract backgroundspectrum Library Search Library Search D GALNTHEONPA1 2 Acquired 26 Nov 2661 16 46 32 18 54 A sometimes handy tool in the search after the Soane a e o maltersttee e 18807 87 identity of an unknown component is a library search Because the reference spectra are impure EI spectra and the Saturn generates spectra with substantial auto CI character this is usually not 9 very valuable Furthermore the library is limited to 65 77 go 195 ra 728 40 000 compounds while on modern systems 46 66 86 166 126 146 166 186 266 226 246 266 286 306 326 346 library s often contain 150 000 compounds This sare cone near et i P Purity Search L Select Library Search Libr NIST and the fact that in a synthesis lab usually new and F Fit Search D Delete Mass Peak Search Type Purity R Reverse Fit Search W Mol Weight Range Mol Wt Limit 8 2808 not yet published compounds are produced the I Init Search Params X Sample Mass Range Sample Range 38 343 N Local Normalization M Minimum to Search Min Search 56 library will not be used often Fi Search Scan List F2 Scan List Results Local Norm Off lt Cr gt Start Search Scans inList 1 There are several
11. ways to perform the search Purity Fit and Reverse fit The meaning of these terms can be revealed with the Help key plot gain 2 4 plot gain 2 help Chromatogram Backup Because the limited size of the hard disk it is the best to backup your data after the measurements ona floppy disk Most data files are several of hundreds of KB so it is common to reduce the files by saving only the important part of the chromatogram Selecting an extraction range can do this Chose the EXTRACTion range by pressing E in the Chromatogram screen Select the desired area by setting the cursor left of the desired area and pressing the spacebar Set the cursor right of the desired area and again press on the spacebar Then the parameter menu pops up to change the parameters press P Give the extracted chromatogram a different name put X in front of the sample name e g STOOKO1 becomes XSTOOKO1 Press the return key and the extracted chromatogram is saved to the new datafile It is possible to change the scan range and the threshold manually to reduce data even further but this is not recommendable Go to Filemanager and the right directory and select the extracted data file click only 1 time Press onC opy and ENTER a menu pops up Press onL 0g to another drive and key A to activate the floppy disk drive The same menu pops up press ENTER and the data file will be save on the floppy disc be sure to put one in If you want t
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