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1. Figure 5 91 TightVNC viewer installation showing selection of Viewer Only option 6 Run TightVNC from the Start menu Simply put in the IP address of the TightVNC Server your instrument and press Connect The IP address is the same one that is used in the CHROMION software to connect to an instrument The following image shows the dialog box that opens when running the TightVNC viewer 110 OTHER OPERATIONS NIST Mew TiehtYNC Connection Ed TighVNC Sever EARE m C ight Connection profile Dpions C Low bandwidth connection Default connection options Listening mode ate C High Configuration L Ehol oaee Dennis Figure 5 92 Dialog box that opens when running TightVNC viewer An exact image of the instrument screen will appear on the computer This image can be interacted with using the mouse and keyboard on the computer There is a slight delay between action initiated on the computer screen and the action on the instrument The NIST software is the NIST mass spectral library as well as the AMDIS software package This is an optional software package Any features in the CHROMION software that use the NIST data base require that the NIST software be installed To install the NIST library open the NIST folder and run the setup program then follow the on screen instructions The NIST and AMDS are sophisticated programs Therefore the instructions for use will not be detailed in
2. 6 All of the remaining settings are used to adjust the deconvolution and baseline extraction routine The current settings are optimized to provide optimum performance for deconvolution and should not be changed Changing these setting will affect the deconvolution process They should only be changed by personnel that have been trained in their function Contact the Torion for more information Unknown Identification 1 The Match unknown compounds check box turns on and off the library search for unknown compounds that are not part of the Target List 2 The Maximum top spectral hits to show set the number of compounds that will be displayed with the compounds shown in order of quality of fit 67 OTHER OPERATIONS 3 All of the remaining settings are used to adjust the unknown search routine The current settings are optimized to provide optimum performance for identifying unknown peaks Changing these setting will affect the identification process They should only be changed by personnel that have been trained in their function Contact the Torion for more information 4 The Path 1 Path 2 Path 3 and Path4 allow the user to designate the location of unknown libraries to search The search will be conducted by looking in the first path then in each successive path until the best match is found These libraries will be stored on the SD card on the instrument and should be limited in the number of compounds to keep the data processing t
3. 114 OTHER OPERATIONS RF Modem External Power Environmental Management External Helium Vent Figure 6 4 back of instrument Caution Prior to the next step regulate the external gas pressure to a minimum of 80 psi CAUTION 4 Attach the external helium carrier line by pressing the quick connect onto the helium inlet port The quick connect is attached when it clicks into place and cannot be removed without sliding the locking cylinder back 5 To disconnect the external helium carrier slide the locking cylinder on the quick connect back until the quick connect slides off of the instrument helium connection Removing replacing the SD card 1 When removing the SD card from the TRIDION it is best to remove the card when there is little likely hood of data being written to the card 2 If the TRIDION is completely turned off the SD card may be removed or inserted at any time Otherwise the best time to remove and replace a card is when the instrument is on the Home screen 3 Do not remove or replace the SD card when running a sample or during procedures where data or method files are being worked with How to bake out the GC injection port and column Caution Baking the GC column at temperatures above 300 C may degrade the stationary phase CAUTION 115 OTHER OPERATIONS Caution Use external power for baking the column otherwise the batteries will be depleted faster than Niven d
4. Run a sample from the CALION vial by placing the SPME fiber into the vial following the procedures described in the How to sample headspace vapors from liquid or solid samples section of the Basic Operations chapter Follow the standard procedure for starting a run by running the SOP and follow the instructions to inject the CALION standard into the instrument After the analysis use the File Manager to move the RES file over to the computer Refer to the Software chapter for details about using File Manager Use CHROMION Data Review to open the file Refer to the Software chapter for details about the functionality of Data Review The TIC should look like the example chromatogram shown above 125 LIBRARIES vii Position the cursor over the methylene chloride peak This should be the second peak and should elute at around 17 seconds MS Ab undance 270 38 ol ihi a ul 0 500 Ready 2003 02 26 19 57 20 Figure 7 7 Uncalibrated mass spectral data of methylene chloride used for calibration viii In the example shown above the bin number for methylene chloride is 100 Open the Performance Validation screen in the CHROMION software and select Methylene Chloride from the table The following shows that the Methylene Chloride mass is in the mass window If the mass is not in the window adjust the minimum and or maximum values so that it is in the window DE Retention Time Calibrations i Acetone 4551 5
5. 4 The information that will be displayed on the screen is the information contained in the Hazard Level Text column How to use this information will be described in the Target List section of this manual 5 To remove an entry rick click on the line of the entry and select the remove hazard level entry option Instrument Menu Connecting to an Instrument 1 Before connecting an instrument to CHROMION it must be added to the Instrument List which is located on the Instrument Setup form 2 Toadd anew instrument to CHROMION click Instrument on the main menu and select Instrument Setup 3 Enter an Instrument Name the name is just a descriptive label and can be anything that the user enters 4 Enter the IP Address of the instrument being connected and click the Add button To find the address refer to the on instrument software section of this manual 52 OTHER OPERATIONS E Auto Connect at Startup Instrument List Dera ener Nerds A Instrument Name Tae tea 192 168 2 29 Add Figure 5 5 Instrument Setup when adding an instrument for the first time 5 Enabling Auto Connect at Startup will reconnect the default instrument each time CHROMION is launched E Auto Connect at Startup Instrument List 192 168 2 20 Instrument Name a Figure 5 6 Instrument Setup after adding instruments 6 Selecting the check box in the default column will set which instrument is connected when using Auto Connect at Startup
6. AMDISNISTEPACW J AMDISNISTEPACW J AMDISNISTEPACW AMDISNISTEPACW AMDISNISTEPACW AMDISNISTEPACW F AMDISNISTEPACW AMDISNISTEPACW AMDISNISTEPACW ave Library BER MOP AO Library BOP iO Edit Library Name R ie BOF BO t Library ane gt wBliOPf aS Import Library rn l gt sO LO Export Selected Compound to Current Target List av i gt HOF LO Add Compound OF a 0 ago OF 22 Remove Compound id H zi id d H id id A Figure 5 79 Library Editor button bar with Compound Details tab open 8 The following are the descriptions of the button bar items a Select Library This opens a drop down list of all of the libraries in the data base To open a library click on it in the list 99 OTHER OPERATIONS b New Library This option creates a blank library form that can be filled in by the user To give the library a name besides the default name type the new name into the Library Name field and then save the library c Save Library this option saves the currently open library d Delete Library This option deletes the currently open library A confirmation dialog box will open to confirm that the library should be deleted The software requires at least one active library so it is not possible to delete the last library in the list e Edit Library Name This option allows the user to enter a new library name for the currently open library f Export Lib
7. targetlist CD Figure 4 46 Viewing attached library to chosen method 12 The Data Analysis tab displays the name of the library that is part of the selected method System Settings Button 1 The following image shows the screen that is displayed after selecting the System Settings button from the Advanced screen Target4E Torion l l 44 i 1 SystemBlank al 2 Set Date Time Update Firmware Password Install Update Bluetooth Control Figure 4 47 Screen showing the system setting options 39 INSTRUMENT OPERATION 2 The following image shows the screen that is displayed after selecting the Set Date Time button from the System Settings screen te Target4E h Torion 1 SystemBlank Date Time Settings Date Time Apr 4 2012 10 58 26 AM Time Zone Pacific Standard Time Automtically Adjust for Day Light Saving Figure 4 48 screen showing the date and time settings 3 To change the date or time touch the part of the date or time you want to change The above image has the day selected Use the arrow buttons on the right of the Date Time field to change the value 4 Select a time zone by touching the down arrow on the right side of the Time Zone field and selecting the right time zone from the list 5 Set day light savings time by touching the button to the right of Day Light The value will switch between Yes and No 6 Selecting the Home button will return
8. 10 11 12 13 17 29 186 191 222 224 225 229 status screen 56 stop run button 45 Structure Image 152 157 Summed lon 142 system settings button 66 target chemical 3 4 11 Target List 85 87 94 104 105 106 107 108 109 131 133 134 136 149 154 temperatures 3 55 174 179 222 TIC 46 47 50 51 142 187 188 TIC Graph 158 TightVNC 167 168 time zone 67 TMS 0 1 6 7 8 9 tools 199 200 Tools 83 114 178 179 200 toroidal ion trap 1 2 6 7 Total lon Chromatogram 118 142 touch screen 21 45 Trap cleaning procedure 210 Trap disassembly 208 Trap reassembly 210 Tuning Wizard 146 162 163 164 165 167 TurboPump 160 161 Turn on 227 Unnecessary 106 USB port 21 vacuum 8 182 200 218 219 220 223 224 vacuum pumps 8 Validate the calibration 191 vapor headspace 12 13 18 View MSDS File 156 VNC viewer 21 VNC Viewer 82 167 Windows CE 19 20 You are not connected to an instrument 99 zoom 45 47 48 49 51 190
9. 58 Filament replacement 215 File Manager 146 147 148 158 182 187 191 195 FileZilla 187 191 flow 8 14 16 22 226 227 From Local File 95 Gas Chromatography tab 54 55 GC 0 1 4 5 8 9 10 17 55 58 142 170 174 184 199 220 221 222 224 226 228 229 GC injection port maintenance 220 GUARDION 0 i 1 3 6 7 8 9 10 13 21 27 82 167 170 171 172 173 174 176 177 178 179 183 185 186 190 191 192 194 199 206 207 218 219 220 221 222 223 GUARDION 7 223 HardSolventDelay 146 Hazard Level 87 107 Hazard Levels 87 helium cartridge 172 home screen 26 51 61 67 176 193 Home screen 174 hydrogen 6 210 Import 92 95 101 105 154 injecting 1 Injection liner and seal cleaning or replacement 222 Install the ion trap RF module 220 Instrument Setup 87 88 89 Instruments 83 90 lon Target 58 IP Address 88 Launch Deconvolution Control Window 124 130 library 8 82 169 225 229 Library Editor 149 151 152 153 155 157 Library Search Spectra 121 122 Link MSDS File 155 Main 83 106 160 manage files button 59 Manual Calibration 101 103 mass calibration 186 190 195 197 198 Mass Calibration 113 166 183 198 mass spectrometry 2 6 INDEX Mass Spectrometry tab 55 Match unknown compounds 109 Method 83 84 92 93 94 95 96 97 98 99 100 114 166 198 method list 62 methods button 61 Molecula
10. 7 There are two ways to connect an instrument to CHROMION a Click Instrument on the main menu and choose Connect Instrument Select the Instrument Name from the drop down menu and click OK 53 OTHER OPERATIONS Figure 5 7 connect an instrument to CHROMION b In the CHROMION navigation pane click Instruments and then click the expand icon for a list of instruments Right click and select Connect to Instrument Note The taskbar at the bottom of the screen will display the instrument name when the connection is made to the software Gas Chromatograph 2 Target List T Performance Yalidation Data Review E Mass Spectrometer Wr File Manager Figure 5 8 Screen showing the icon in the navigation pane has changed to show that instrument T14is now connected and the instrument name is highlighted in green 54 CAUTION OTHER OPERATIONS 8 Only one instrument can be connected to the PC at a time 9 While it is possible to use many of the software functions when not connected an instrument there are some functions that only work when the computer is connected to an instrument Details about how the software interacts with connected instruments will be described in the specific sections where this applies 10 If a connection to an instrument cannot be made an error message will display indicating that CHROMION is unable to connect to the instrument Cannot connect to lt 169 254 85 48 gt i x Unable
11. Performance M Fil System Settings Figure 7 11 Calibration succeeded 7 If the calibration succeeded then press the OK button and then press the Advanced button and select Procedure and reactivate the SOP For detailed instructions on running samples refer to the Instrument Operation chapter Confirm auto calibration Performance Validation 1 To confirm that the calibration is working follow the steps in the SOP until you can run a normal standard and run the CALION standard again Make sure that all 13 compounds in the standard are successfully identified by the TRIDION If all of the compounds are properly identified then the instrument is calibrated and ready to run analysis 2 In afew cases even after running auto calibration the instrument may fail to properly identify all of the compounds in the CALION standard If this occurs continue to the next section and follow the instruction about how to correct a failed auto calibration Correcting failed auto calibration Performance Validation 1 If the following report is displayed then the calibration failed and the calibration ict files needs to be modified to adjust the ranges around the various masses and retention times being used for calibration 130 LIBRARIES Torion Procedure stile I Diagnostics Galibration Results for x Performance i a A Method System Settings Figure 7 12 Auto calibration failed message 2 Ifthe calibration fails co
12. a false positive identification There are a couple reasons why this may happen 1 The mass spectrum of the false positive compound might match the mass spectrum of a compound that is actually present If this is the case see if there are additional unique ions that can be added to the library for more selective identification 2 The mass spectrum of the false positive might be present in the background noise This will happen especially when running compounds in a complex matrix such as gasoline or diesel TRIDION fails to reach set temperatures If at anytime the TRIDION fails to reach temperatures set in the GC settings contact Torion Technologies TRIDION is unable to run on battery power If the TRIDION has previously been successful at running on battery power ensure that the batteries have been fully recharged and are making proper connection with the TRIDION Also ensure that the batteries being used still have enough power left to run the TRIDION If the instrument is still unable to run on battery power contact Torion Technologies TRIDION suddenly powers down If the TRIDION was running on battery power the life of the battery has been exceeded Replace the batteries or switch to alternative power and perform a blank run on the TRIDION before continuing with analysis If the TRIDION was running on alternative power ensure that the power is properly connected Once the power is properly connected perform a blank run on the TRIDI
13. for example Electron Multiplier Detector Voltage that typically has a signal of 1200 to 2200 and Power Board 3 3V that will have a signal of 3 1 to 3 4 will result in scaling that makes the Power Board 3 3V reading useless 4 Tosave the data to a CSV file Disable the data logger using either the right click menu or the button on the button bar The click the Write Logging Data To File button on the button bar The save file Windows dialog box will open Navigate to the location where the file is to be saved and enter the name of the file then click on OK Tuning Wizard 1 The Tuning Wizard is used to check the performance of the GC MS 2 The following shows the Tuning Wizard screen Results Chromatography Asymmetry UARGHAT Retention time D Sensitivity ino Mass Spectra Baseline Unknown Mass calibration Unknaiin Spectral quality M Resolution Daina Background nino Identification Compound id Figure 5 87 Tuning Wizard screenfiles that are updated automatically when a new version of CHROMION is installed 106 OTHER OPERATIONS 10 11 For more advanced users it is possible to use customized INI and library files To open the file location dialog box click on the Select Location of INI File button This button is shown in the following image Figure 5 88 Tuning Wizard button bar The
14. the changes can be made in the Tuning Wizard before clicking the send button 18 The tests that return no message are for information only and are not used to tune the instrument If a test fails but no message is displayed then the users should ignore the results and continue to run the instrument as normal VNC Viewer 1 The VNC Virtual Network Computing viewer is a utility that allows the user to see and interact with the TRIDION in real time from any PC that is connected to the instrument 2 The instrument has been configured to work with TightVNC viewer 3 This software is free on the internet but is not supplied with the instrument 4 Toinstall the software Download it from the TightVNC website http www tightvnc com download php Download the Self installing package for Windows 5 Run the setup program Accept all the defaults except when asked to Choose Components Select the Viewer Only on this screen The following image shows the setup screen where the user should select the Viewer Only option EF TightVNC 2 0 4 Setup SE Choose Components Choose which Features of Tight NC 2 0 4 you want ta install Check the components you want to install and uncheck the components you don t want to install Click Next to continue Select the type of install Viewer Only m Or select the optional Bl Tight NC Server Description components you wish ko F Ti g PT Tight NC Yiewer Space required 503 0KB
15. yellow highlight With the MS graph and the Summed graph showing that the intensity of the ions in the summed graph is much higher than the intensity of the ions in the MS graph 75 OTHER OPERATIONS Scani 211 RT 32 5530 Sec Abun 3 782 Avg Range 200 211 L5e5 L 0S5 0 0 Ready T T 9 Validation G36 SD Card G36 Data CDF 000000545 caf Figure 5 43 Summed graph with TIC and MS graphs e Background This is the spectral data for a section of background selected by the user Choosing this function totals the response of all of the ions in the region that has been selected The following image shows background blue and summed yellow areas selected in the TIC graph The background graph Bknd shows the background noise of the instrument Scanr677 RT 92 2050 Sec Abun 541 Avg Range 200 211 Bkad Range 225 236 43 s 8s 97 m s00 128 149 hodis hs baadt cs a tullloctiblloratlets E AEF O ee O RE EE 256 272 286 334 366 378 1 i i L i i i 1 I Ld 1 1 p L b i 50 100 150 200 250 300 a350 Ready T T 9 Validaton 636 5D Card G36 Data ODF 00000545 caf Figure 5 44 Background Bknd graph with TIC and Summed graphs f Difference This is the spectral data showing the difference between the background spectra and the highlighted section of summed spectra The following image shows the TIC with summed yellow and background blue areas highlighted and wit
16. 143 SERVICE Alignment Pins Locations First Threaded Hole Clock Wise From Notch Notch Alignment Fixture Figure 8 18 Alignment pin installation Leave the alignment pins loose so they can move during assembly The correct installation would be to tighten them until they stop then turn them back 1 4 turn Place the Bottom End Cap Electrode and alignment pins into the Alignment Fixture Make sure the notch on the Bottom End Cap Electrode aligns with the notch in the Alignment Fixture Slide three of the ceramic spacers over the alignment pins Place the bottom polyimide spacer for the center electrode football in the center of the Bottom End Cap Electrode The polyimide spacer is symmetrical so it does not matter which side is up Place the Center Electrode football onto the polyimide spacer The next part to install is the Center Ring Electrode Look at the larger holes in the electrode One side of the holes has a bevel and the other side is flat Slide the Center Ring Electrode over the alignment pins with the beveled side down Make sure the notch aligns with the notch in the alignment fixture and the Bottom End Cap Electrode Place the top polyimide spacer on the stem of the Center Electrode football Make sure the taller part of the spacer is up Slide three more of the ceramic spacers onto the alignment pins Slide the Top End Cap Electrode onto the alignment pins with the curved surface down
17. 2 The following dialog box will open confirming that the method was saved success Method successfully saved Figure 5 14 Method successfully saved dialog box Saving a Method as a New Method 1 Select Save As to create a copy of the currently loaded method with a new name 2 The following dialog box will open allowing the user to input the method name New Method Name Figure 5 15 Save As dialog box 4 Typein the name of the new method and select OK 5 Selecting Cancel will abort the operation without saving the new method Rename a Method 1 The method name can be changed by clicking Methods and selecting Rename Method The following dialog box will open 58 OTHER OPERATIONS Rename Method Method Name Cancel Figure 5 16 Rename Method dialog box Exporting a Method to a File 1 When the Export Method function is selected the following dialog box is opened lt 9 Libraries 4 Homegroup E R Nathan Porter jii Computer E thd Network EF Control Panel Recyde Bin ub Freedom Thumb Drive Figure 5 17 Export Method file location dialog box 2 Select the location where the method file will be saved or make a new folder then click OK The following dialog will open showing that the exported file was successfully created Success O O i i Method test5 successfully exported to PF Cr Users nathan porter Desktop best5 met Figure 5 18 Method successfully exported
18. 40 L 9 1 S stemBlank d Password is required to change parameters or exit software Enter Password O Continue Cancel eiel Caps Lock HOQ Figure 4 40 Enter Password screen Caution These changes take effect immediately even in the middle of a run and should only be adjusted by experienced users The changes are not saved in the method and will be replaced as soon as a new method is loaded into the instrument If it is desired to keep the changed parameters it will be necessary to modify a method file in the CHROMION software and load the saved method as the active method CAUTION 35 INSTRUMENT OPERATION Manage Files Button 1 The following screen opens after selecting the Manage Files button The Manage Files tool is used to rename delete or copy files from the SD Memory Card on the instrument to a USB memory stick Tarqget4E Torion activated2012 04 16 13 35 40 4 4 wl i 1 SystemBlank Please Select a Folder 2011 12 10 2011 12 14 2011 12 15 2011 12 16 2011 12 19 2011 12 20 2011 12 21 Folder Emraga Card Data Figure 4 41 Screen that is displayed after selecting the manage files from the advanced screen 2 Highlight any folder by touching the folder name on the screen with the stylus and choose OK 3 The following screen will appear that lists all of the files within the folder selected in the previous step Tarqget4E Torion Technologies 1
19. ASSEMDIY c ccecccccsesecccceeseecceeeeeeceeeeeeceeseeeseseeessageeessaneeesseaes 148 Electron multiplier detector replacement ccceceeeeeeteeeeeeeeeeeeeeeees 148 Remove the electron multiplier detector ccccccceecseeeeceeeeaeeeeeeeesaeeeeeeeeas 148 Reassemble the electron multiplier detector ccccceeeeeeeeeseeeeeeeeeeeeeeeeeenes 150 Install the ton trap RF module cccceccccsseeeceeeeseeeeeseeeeeseeeeeseeeenes 150 GG injection port maintenance iucidisiivcdtaridavidesiiavadaniiosidavddosieiioradanawnt 150 Accessing the GC injection Ort cccccccceeeeeeesseeeeeeeeeeaeeseeeeeeeeeeeaaaneeeeeeess 151 SePlUM replacements a ke ee eee 151 Injection liner and seal cleaning or replacement cccccseeeeeeeeeeeeeeeeeeees 151 9 TOUDIESNOOUNG sessen rE aera eee 153 TRIDION WII MOT TURN OM s2etstateta ct tntaiterced es alecniws eon eestemersteacats 153 TRIDION wik NOt TURTON T ienien i 153 TRIDION cannot Maintain VACUUM ccceeceeeeeeeeeeeeeeeesaeeeeaeeesaeeens 153 GC baseline is noisy Or drifts UDWAIC ccceccccseeeeeseeeeeneeeeeaeeeesaaeees 154 GG peaks are ASV MIM CUS sincidesddeednsddocddaniduclduaidensdasideahdaoadeedceaideediane 154 GG peaks ale elung Ale nanssauseunorine nina 156 Acquired mass spectra are NOISY cccceececsesceceeseeseeseeceeseeseeeeenseees 156 Results are not reproduclble scriescene eeren a arai 157 There is no instrument signal sz
20. B PowerSystem AverageTimeToChargeA Average Time To Charge Battery Cell A PowerSystem AverageTimeToChargeB Average Time To Charge Battery Cell B PowerSystem BatteryCurrentA Battery Cell A Current PowerSystem BatteryCurrentB Battery Cell B Current PowerSystem BatteryVoltageA Battery Cell A Voltage PowerSystem BatteryVoltageB Battery Cell B Voltage PowerSystem CaseTemperature Internal Instrument Temperature PowerSystem Cpu33Voltage CPU Power 3 3 V PowerSystem CurrentOutMonitor Power Board Total Current out PowerSystem MainVoltage Main System Voltage PowerSystem Negative 15Voltage Power Board 15 V PowerSystem Negative5Voltage Power Board 5 V PowerSystem Positive10Voltage Power Board 10V PowerSystem Positive15Voltage Power Board 15V PowerSystem Positive24Voltage Power Board 24V PowerSystem Positive26Voltage Power Board 26V 104 OTHER OPERATIONS PowerSystem Positive33Voltage PowerSystem Positive5Voltage PowerSystem RemainCapacityA PowerSystem RemainCapacityB PowerSystem RemainPercentA PowerSystem RemainPercentB PowerSystem RemainTimeA PowerSystem RemainTimeB PowerSystem TemperatureA PowerSystem TemperatureB PowerSystem VoltagelnMonitor RoughingPump Current TransferLine Temperature TrapHeater Temperature TurboPump BearingTemperature TurboPump BottomTemperature Power Board 3 3V Power Board 5V Battery Cell A Remaining Capacity Battery Cell B Remaining Capacity Remaining Percent of Charge left in Battery Cell A Rem
21. Blank Run 3 Choosing Start Run initiates a system blank run after choosing to run a System Blank Run from the previous screen 4 The following image shows the screen that is displayed after selecting the Start Run button Tarqget4E Torion Technolo 20sample01 2012 04 1 1 SystemBlank 0 116 1 0 9 24 0 47 0 70 0 93 1 A Split Screen Stop Run Extend Run Figure 4 8 System blank screen displayed while running a blank 5 This screen shows a chromatogram of a clean system blank where there are no contaminant peaks 6 The following image shows the screen that is displayed after the system blank run is finished and the system is processing the run data looking for any contamination peaks 18 INSTRUMENT OPERATION Target4E Torion 20sample01 2012 04 1 L 4 i Ezg 1 SystemBlank od Processing Results a 40 Figure 4 9 Processing Results screen 7 The following image shows the screen that is displayed after the system blank is performed and analyzed If there were any contaminant peaks the contaminants might be identified by the on board instrument library If any positive identifications were made they would be listed in the identification table at the bottom of the screen Tarqet4E Torion Technologie 20sample01 2012 04 1 1 SystemBlank RT Identification Alert Match Area a More e Figure 4 10 Results screen shown after system blank run is performed 8 The
22. IsOn false Control SolventDelay Value 7 None Seconds Control Baseline IsOn true Control Noise IsOn true Control Noise Threshold 1 None Arbitrary Control RunningAverage IsOn true Control RunningAverage Window 2 None Indices Control BinCollapse IsOn true Control BinCollapse Window 30 None Indices Control NoiseRemove IsOn false Control NoiseRemove LowessSpan 0 1 None Arbitrary Control NoiseRemove CutoffWeight 1 5 None Arbitrary Control NoiseRemove CutoffThreshold 100 None Arbitrary GasChromatograph Helium StartCalibrationPressure 18 16 23 GasChromatograph Helium StartCalibrationTemerature 50 MassSpectrometer lonSource HardSolventDelay 0 MassSpectrometer ionSource FilamentCurrent 1 05 0 8 1 25 amps 120 LIBRARIES MassSpectrometer MassSpectrometer MassSpectrometer MassSpectrometer MassSpectrometer MassSpectrometer MassSpectrometer MassSpectrometer MassSpectrometer MassSpectrometer lonSource lonSource lonSource lonSource lonSource lonSource lonSource lonSource lonSource lonSource FilamentBiasVoltage FilamentGateLowVoltage 150 FilamentGateHighVoltage BaseLinelsOn BaseLinelsAuto BaseLineChunk BaselineValue NumberSignificantIndexes 100 lonTarget 1000 TargetStep None Arbitrary Arbitrary Indices Arbitrary Arbitrary lonizationMinimumTime 0 015 0 015 Milliseconds 9837864 MassSpectrometer lonSource MassSpectrometer lonSource lonizationMaximumTime 60 0 12 32 Milliseconds MassSpectrometer lonSou
23. Lists can reduce the accuracy of the search algorithms a Library Name This field is used to name or rename a library as well as to see the name of the currently open library b Created Date This field shows the date that the library was created This date and time comes from the computer clock and will be wrong if the clock is not set to the correct date and time c Modified Date This field shows the date and time that the library was last edited This date and time comes from the computer clock and will be wrong if the clock is not set to the correct date and time d Search Compounds This part of the software is used to search the library The following parts of the search option 97 OTHER OPERATIONS i Filter Field The user can select from search options 1 Compound Name 2 CAS 3 Formula 4 Retention Index ii Filter Term This allows the user to select from the following terms when searching 1 Begins With 2 Contains 3 Ends With 4 Exact Match iii Filter This is where the user types in the characters that are to be matched iv The first button executes the search The button with the red X on it clears the search fields 4 The following image shows the Compound Details tab Library Contents Compound Details Compound Compound Tn List Structure Thage Compe Ham ten Forme z Hetention ie RD Motootr Woot SE 3 a Spectrum Figure 5 78 Library Editor Compound Details tab 5 The following a
24. Note Importing and exporting Target Lists can result in poor compound identification since the retention times for a different method or different instrument may not be consistent with the times used in the Target List Target List Tab 1 The target list is a subset library used to target compounds of particular interest to the user It is different from the unknown library because it contains specific information that is influenced by some of the instrument settings In addition to mass information the target list also contains retention time information The same list of compounds will be used for configuring quantitative information The Masses table shows the specific ions that are associated with a compound in the target list The following image shows the masses for 1 1 Dichloroethene Target List Deconvolution Parameters i ll Se Figure 5 27 Target List Normally the tallest mass peak is designated as the Main ion and has an Intensity of 100 Each of the other masses has an Intensity that is some percentage of the parent peak For example the 98 mass has an expected intensity that is 75 of the parent peak The Confidence is an absolute value So the Confidence level for the 98 mass is 50 This allows the 98 mass to vary from 25 of the parent peak to 125 of the parent peak and still be acceptable There are three options for the Type column They are Main Necessary and Unnecessary As described ab
25. Percent of the tallest mass peak The Time Unit Display allows the user to set the x axis values to Minutes or Seconds The Mass Fragments allows the user to set the display to filter out mass fragments that have a relative percent response below the value set in the Exclude Under box The NIST option allows the user to enter in the path of the NIST software Type the location of the NIST software into the Search Path field To change the name of the temporary file that is created when exporting spectra to the NIST search type the desired name in the Spectra File Name field The Chart Synch function ties the x axis values of the TIC and RIC windows to each other To keep the times synched place a check in the box next to Sync RIC to TIC If you desire to see peaks at different retention times in the RIC and TIC windows leave the box empty Hazard Levels 1 The Hazard Levels menu is used to configure safety information that will be displayed on the TRIDION 9 when target compounds have been identified The following image shows the Hazard Levels dialog box 51 OTHER OPERATIONS Hazard Level List Hazard Level Hazard Level Text B TIC Figure 5 4 Hazard levels dialog box 2 The user can enter any numerical value in the Hazard Level column 3 The user can then enter a text or numeric value in the Hazard Level Text column This allows each user to customize the hazard level information for their specific application
26. Succeeded Figure 4 22 Calibration results screen when calibration succeeds 14 Choose OK to proceed Running Samples 1 The third step of the manufacturers SOP is running samples 2 The following screen indicates that the instrument is now ready to run samples 25 INSTRUMENT OPERATION Torion Performance Validation 0 Firms Message SOP step 3 Run Sample You may run up to 20 samples Press OK to continue Figure 4 23 SOP step 3 instrument is ready to run samples 3 Choose OK to proceed and start running samples 4 The following image shows the home screen that is displayed when the instrument is ready to perform sample analytical runs Tarqet4E Torion j Performance Yalidation 3 Sample _ Data File Location Folder 2012 04 13 File Name 20sample03 2012 04 13 09 39 22 Sample Concentration O High Medium Low Method Advanced Start Run Previous Results Figure 4 24 Home screen ready to run samples Data File Names 1 For every run the instrument automatically creates a file name as displayed in the image above Users may change this name before starting a run 2 To change the file name highlight the File Name field and an alphabet touch board will appear on the screen The user can start typing the new run name 26 INSTRUMENT OPERATION The instrument also automatically creates a data folder for each day All run data is stored in the daily folder The u
27. SystemBlank Select File s default2011 12 20 08 52 12 raw default2011 12 20 09 03 53 c I default2011 12 20 08 52 12 cdf default2011 12 20 09 03 53 n default2011 12 20 08 52 12 res default2011 12 20 10 22 50 r _Idefault2011 12 20 08 58 50 raw default2011 12 20 10 22 50 c I default2011 12 20 08 58 50 cdf default2011 12 20 10 22 50 n _Idefault2011 12 20 08 58 50 res _Idefault2011 12 20 09 03 53 raw i A Figure 4 42 Select file s to be managed 36 INSTRUMENT OPERATION 4 Individual files can be either selected or deselected by touching the check box next to the file name 5 After selecting the desired files choose to Rename Delete or Copy the files The copy function has not yet been activated 6 Selecting the Home button will return the display to the Home screen Methods Button 1 The following image shows the screen that is displayed after selecting the Methods button from the Advanced screen From the Methods screen users can select a method to activate or simply view the method parameters in a selected method Target4E 1 SystemBlank Calibration 2011 08 15 cal F30settings txt Figure 4 43 screen showing methods selection menu 2 To choose a method select it from the list by touching it to highlight it 3 The user can move through the method list by either using the arrows and sliders on the edge of the method window or by using the Up and Down buttons 4 Pressing the Act
28. TRIDION 9 make sure the gold rings on the CUSTODION Syringe touch the contact points on the GC injection port When the contact points connect with the CUSTODION Syringe the instrument automatically starts a run 2 Conversely the instrument will NOT start an analysis if the CUSTODION Syringe does not come in contact with the contact points 12 CAUTION INSTRUMENT OPERATION Contact Points Figure 3 1 Interface between the SPME syringe and the injector 3 Follow the on screen instructions as to when to depress the plunger to expose the SPME fiber 4 Depress the plunger until you hear or feel a click and then release the plunger Similar to a ball point pen 5 The following image shows a cutaway diagram of the SPME inside the GC injector port Interface between CUSTODION ale AS syringe and injector Injector hidden under face plate Inlet of GC column Figure 3 2 Cutaway diagram of CUSTODION syringe inserted into the injector port with fiber retracted 6 Follow the on screen instructions as to when to depress the plunger to retract the SPME fiber inside the protective needle Caution Ensure the SPME fiber is completely withdrawn inside the syringe needle before removing the CUSTODION from the injector port otherwise SPME fiber may be damaged 13 INSTRUMENT OPERATION 4 Instrument Operation This chapter describes the functionality of the instrument control interface This includes a description of
29. Tarqget4E 1 SystemBlank _ Data File Location Folder 20 12 04 24 v 9 AC Power s Helium value i File Name 20sample01 Inst state Ready g Sample Concentration High Medium Low Method Advanced Start Run Previous Results Figure 4 5 Instrument status shown in expanded view 7 Inthe middle section of the status bar the name of the activated method is displayed at the top as shown in the image above In this example the method name is Target 4E 8 The type of sample is displayed just below the method name in the status bar as shown in the image above In this example the sample type is 1 SystemBlank Running a blank 1 SOP step 1 is to run a system blank The first screen to appear after the system has reached operating status is shown in the figure below Target4E Torion 1 SystemBlank Firms Message System is ready for operation SOP step 1 Run System Blank Press OK to continue Figure 4 6 SOP step 1 Run System Blank 2 Selecting the OK button prepares the instrument for a system blank and the Home screen appears as shown below 17 INSTRUMENT OPERATION Tarqet4E Torion 1 SystemBlank _ Data File Location Folder 2012 04 11 File Name 20sample01 2012 04 11 08 07 33 X Sample Concentration O High O Medium O Low Method Advanced Start Run Previous Results Figure 4 7 Home screen ready to perform System
30. Thoroughly rinse the parts with deionized water and allow them to dry Einsellens assembly 1 Place the Einsel lens assembly into the Barrel with the side showing more metal down and the stem passing through the slot in the Barrel 2 Position the Barrel with the installed Einsel Lens parts over the threaded studs on the EGUN Mount The stem should point away from the center of the trap and toward the closest edge of the board 3 Install the two nuts using the 5 32 hex nut driver Tighten them so the Barrel is secure Do not over tighten the nuts as this may damage the Einsel Lens Barrel or EGUN Mount Electron multiplier detector replacement Remove the electron multiplier detector 1 The type of electronic detector used in the TRIDION is a continuous dynode electron multiplier detector It will be referred to as the detector in this section of the manual 148 SERVICE 10 11 12 Follow the instructions in the Remove ion trap RF module section of this chapter The following image shows an exploded view of the ion trap RF module from the perspective of the outside of the vacuum end cap Use this image as a reference for component identification while replacing the detector Electron Multiplier Detector Detector Board Vacuum End Cap 2 Captive Screws Detector Board Cover 4T10 Torx Screws Fo 7 Board Mounting Screws Figure 8 24 Electron multiplier replacement diagram The electron multiplier
31. ccccseececeeeeeceeseeceeeeeeeeeeesaeeess 10 Performing an Injection with the CUSTODION Syringe c0 12 4 Instrument Operation cece cceecccseeceeceeeeseeceseeeceseeeeessaueeesaeeesseeeesseeeesaees 14 PSIG FUNGUO eee E E R 14 Standard Operating ProCeCures cccccseccccseecesseeeeseeeeesaeeeesaeeesaeees 16 Status DaT ee e E ee ee a eee 16 PCMAG A AR ea E N 17 Running a Performance Validation cccccccccccseseeeeseeeeeeeeseeeeseeeeeeeaeeeeeeeaes 20 RUNNING SANDS Sessa teats ce eed coe tne aa EEEa AEEA ER ANED aan 25 Data File Narnias sosmeses ea a aeaa aa Ae aea E aa aini 26 Sample Concentration sesesesesseseseseseseseseereseseseseseseeseseseseseseseseeseseseseseseseeseseseseseseseseesesese 27 POM ANAC CO oraren cree A A E 32 POG BUTON asee E E E E E 32 Status Diagnostics BUTTON isesescs ccosescecsnssecosendencecsneuhceosiedsnscseodecausesevehervsecparsvenesssonenaassveeve 32 Manage Files BUTEO yicoscascsscicecsttessesseccivesscessencasessiescteaivncsenetcvsedaserdsceatseielssiexisustcoseescess 36 Methods Button sessesesessesesessesesessesesessesesesseseseeseseseeseseseesesessesesesseseseseesesessesesessesesessesesess 37 System Settings BUTTO arisane eranen aeran Aa erae REAR NAAA ERER 39 Previous Results vscacessteccatactads qecedere cencseenqeainaven qi ssecaceandend ceesgscaneueaaeaseceeexguensenes 42 EPOCE oa E E A yar er ere eee 45 Be SOIL E EE E E EEEE 48 SONAS OO FOG eer E 48 CH
32. components affect things like retention time generation and actions that rely on retention times like target compound identification and calibration These are primarily gas chromatographic functions 2 The functions in the tools section are either generic and not specific in nature or very specific for a single instrument Overview of Data Review 1 Below is an image of the Data Review form The following are descriptions of the different file types that can be reviewed by Data Review 71 OTHER OPERATIONS a RES is a results file This file contains all of the information that is used to create a set of data This includes the data in both the CDF format and the RAW format These are explained below The results file also contains the target library and search results A report file in the form of a text file is included The report has the same information as the report on the TRIDION 9 instrument In addition the results file also contains the setting xml file that contains the mass spectrometer and GC parameters and the ini file for the tuning wizard It is recommended that the user work with the results files since all of the information needed to repeat an experiment is contained in this file Just using the CDF and or RAW data files does not provide enough information to later recreate the method and settings used to get the data CDF is a Common Data Format file type used for chromatographic and mass spectral data It conta
33. compressed file that contains all of the information used to create a data file on the instrument The following information is stored in the RES file i Net CDF data File ii RAW data file iii Target List information iv Calibration information 1 Mass 2 Retention time v Mass spectrometer instrument settings 50 OTHER OPERATIONS Edit menu Preferences 1 The Preferences option opens the following screen This allows setting of functional preferences for different parts of the software The functions on will be described in this section of the manual and will only make sense when placed in context of the software section they are connected to For example the Data Review preferences tab is for functions that affect the Data Review form To understand these functions it may be necessary to review the Data Review section of this chapter Preferences Data Review mY Axis Display NIST Absolute Percent Search path c nist08 mssearch Spectra filename NISTSpectrum msp Time Unit Display C Mnutes Chart Sync IW Sync RIC to TIC Mass Fragments Exdude under lo Figure 5 3 Preferences form 2 The Data Review tab has settings that affect the Data Review form The Y Axis Display can be set to show the Absolute peak intensity of the masses in a given scan or display the relative intensity with the tallest peak set to 100 and the other mass peaks shown as a
34. differences between instruments or the changed GC parameters This section includes the following functions Manual Calibration Data allows the user to enter values in the calibration table This allows the user to enter a retention index value for a specified retention time GC Parameters Retention Time Calibrations i eel Pe 9 8 9 s Figure 5 25 Gas Chromatograph Retention Time Calibration 63 OTHER OPERATIONS 9 Auto Generated Calibration Data uses the auto calibration function to automatically create retention index values from the performance validation data How to enter data into and verify the correctness of the performance validation table will be discussed in the next section 10 Use manual calibration data or Use auto calibration data selects which table of data to use to create retention index values for the peaks in a sample run 11 Use calibration sets the method to either use the retention index or not 12 The Approximate curve option allows the user to select to use a single linear calibration for the retention index curve If Approximate Curve option is unchecked then the system uses a point to point piece wise fit Target List Target List Buttons 1 The following image shows the buttons that attached to the Target List screen Q RJ 3 CI woes Remove Target List Compound gt S bo gt amp R gt amp OR 33 Figure 5 26 Target List buttons with captions 2 Add New Target List
35. dilute or too concentrated when initially sampled by headspace The first 10 BASIC OPERATIONS step with any unknown compound is to sample the headspace If detection of target chemicals is too low or too high follow the flow chart on the next two pages to improve detection 2 Each box in the flow chart provides a new method for sample preparation to increase or decrease the concentration of extracted chemicals If the results are not improved by performing the method in the first box move on to the next box and perform the subsequent sample handling procedure Liquid Unknown Sample Take headspace of sample in environment If sample detection is too high If sample detection is too low Take headspace with shorter exposure time Increase exposure time Place sample into a vial and take headspace Reduce the time of exposure in injector port Heat vial warm with hand or other means such as equipment in mobile lab and take Allow sample on SPME to evaporate before injection do this by exposing the SP ME headspace fiber to the atmosphere Use a syringe to take the headspace and deliver itinto another vial Take headspace of the transferred headspace Immerse SPME directly into liquid Dilute sample in appropriate solvent Immerse SP ME directly in liquid of the dilution Do this in a mobile lab under engineering control Be careful of possible reactions with solvent Use the M 8 paper test to determine whether a
36. each screenand the functions available from the screen Basic Functions 1 The user interface is run using Windows CE as the operating system 2 Upon initialization the software will automatically launch the user interface If the user interface does not launch automatically the following screen will appear Double clicking the TRIDION icon will launch the user interface software r My Device e t E Recycle Bin tJ Internet Explorer Bo Microsoft WordPad a My Documents GC TE TRIDION Figure 4 1 screen showing the Windows CE launch window 3 Once the user interface software has been initiated the instrument pumps turn on to establish vacuum and the heated parts of the instrument begin to increase in temperature The following screen shows the status of the instrument initializing 14 INSTRUMENT OPERATION Torion Establishing Vacuum G0 Establishing Temperature S 0 R a eaer Previous Figure 4 2 Initialization of the instrument 4 The TRIDION is equipped with a touch screen interface It also has a USB port and a USB mouse can be connected directly to the instrument The functionality of the touch screen is the same as for a mouse Touching the screen will select a button and activate the commands associated with the button Using a mouse to position a pointer over a button and then clicking on the button with the mouse will also activate the command associated
37. fiber see the section Prepare the CUSTODION SPME syringe for Sampling b Replace the SPME fiber c Clean the ion trap and electron gun see the section called Trap maintenance procedures d Bake out the injector and column see the section called Bake out the GC injection port and column If the problem persists the injection port liner the septum or the column may need to be replaced To replace any of these components contact TORION e Bake out the vacuum chamber contact TORION GC peaks are asymmetric 1 Please note chromatographic peaks during a PERFORMANCE VALIDATION run will look asymmetric and will most likely have peak tailing This is not indicating a problem 2 Chromatographic peaks should be symmetric and Gaussian Asymmetric and non Gaussian peaks typically result from an overloaded column a degraded column an incompatible solute column combination or incorrect instrument parameters or operation 3 Improving peak shape is important for the best confidence in identifying target chemicals however asymmetric peaks will not necessarily prevent identification Some compounds are generally detected as asymmetric peaks in which case the chemical agent library can be calibrated to compensate 4 Asymmetric peaks may indicate problems with sampling delivery separation or ionization Fronting and tailing are useful indications of possible causes Observation Example Possible cause Fronting The sample is too co
38. following image is an example of a contaminated blank run As shown in the text at the top of the screen an actual System Blank was run but there were contaminant peaks The peaks were either identified or listed as unknown compounds by the library as shown at the bottom of the screen 19 INSTRUMENT OPERATION Tarqget4E Torion Technol les 20sample01 2012 04 1 1 Sy ystemBlank RT_ Identification Alert Match Area Unknown 2 0 0 343 9 66 5 Unknown 3 0 0 141 0 70 8 Methyl Salicylate 86 9 503 4 73 0 Unknown 1 0 0 SEES lt be a More GERT Figure 4 11 Results ofa system blank run that contained contaminant peaks lt 9 From the results screen choose Home to continue running the instrument 10 If the System Blank run was contaminated the following screen appears Target4E Torion 1 SystemBlank Instrument appears contaminated Repeat Blank Y N w Figure 4 12 Contaminated System Blank run notice 11 The above screen is only shown if there were contaminant peaks found The user may choose to continue to run the instrument as normal or choose to perform another blank run If the user chooses Yes then the same screens as above are displayed on the instrument 12 If the user chooses No not to perform another System Blank run or if the System Blank run was clean in the first place the following screen will appear The system is now ready to perform SOP step 2 Running a Perf
39. following image shows three masses from bromoform The masses are 171 173 and 175 When calibrating the bin number at the apex of the bin distribution is used to correlate the bin to the specified mass So mass 171 correlates to bin 1 157 and mass 173 correlates to bin 1 175 1 175 1 157 1190 1150 1200 Figure 7 5 Uncalibrated bin data for bromoform masses 171 173 and 175 iii The following image shows the same sample with the collapsed bins and properly assigned masses 124 LIBRARIES vi vii viii 1743 171 175 172 174 l l l I 170 175 Figure 7 6 Calibrated mass data for bromoform masses 171 173 and 175 The following procedure changes the instrument settings to produce uncalibrated data from the TRIDION In CHROMION Mass Spectrometer screen select the MS Calibrations and uncheck the Use auto calibration data and if checked uncheck the Manual check box In CHROMION Mass Spectrometer screen MS Settings tab change the following values Control RunningAverage lsOn false Control Hanning IsOn false Control BinCollapse IsOn false Control GaussCentroid IsOn false Select the Send Mass Spec Settings to Instrument button The instrument will return a message saying that the method was successfully sent c Set mass calibration vi Refer to the Software chapter section on the Performance Validation screen for details about setting up the mass and retention time calibration information
40. in order to get it to lay flat Be very careful to not over stretch the o ring The following image shows the effect of o ring groove tolerances on o ring installation lt 4 Inside edge of o ring Figure 8 11 Effect of o ring groove tolerances on o ring installation 139 SERVICE Once the o ring is in place inspect the o ring o ring grove and mating surface for dust and dirt Use the dust off to remove any particles The following figure shows the use of dust off to remove dust particles from the installed o ring and the mating surface Figure 8 12 Use of dust off to remove dust particles from the installed o ring and the mating surface 11 Assemble the mating surface to the o ring and the groove and uniformly tighten screws Remove the ion trap RF module 1 Use the 7 64 hex driver to remove the front cover of the TRIDION There are 5 screws along the bottom edge of the cover After the screws have been removed pull the bottom of the cover As the cover pulls forward the top edge must drop down to remove the cover Set the cover aside The following image shows an expanded view with the front cover removed lon Trap RF Module Front Cover Front Cover Screws __ Figure 8 13 TRIDION front cover removal 2 Using the same 7 64 hex driver loosen the two captive screws that are holding in the ion trap RF module Use the handles to pull the ion trap RF module out of the TRIDION The following image shows
41. is located under the white Detector Board Cover and under the Detector Board Use the T10 Torx driver to remove the four flat head screws that hold on the white Detector Board Cover The cover should come off with the screws Set the cover aside Remove the captive screws that were loosened during the ion trap RF module removal from the TRIDION Use the 5 64 hex driver to remove the screws that hold the Detector Board to the ion trap RF module Use the 3 32 hex driver to remove the remaining screws that hold the Detector Board to the ion trap RF module Carefully pull the Detector Board off the ion trap RF module Some of the connectors are tight and can be difficult to pull out If the board is twisted or slid sideways the glass of the detector can come in contact with the metal part of the vacuum end cap and can break If this happens the detector cannot be used Be careful to not damage the O ring The O ring and the area inside of the O ring are in the vacuum chamber Any user that will be handling any parts internal to the vacuum chamber needs to be wearing lint free laboratory gloves Use the 3 32 hex driver to remove the screws that hold the Detector to the Detector Board 149 SERVICE Reassemble the electron multiplier detector 1 Position the new detector and using the screws in the detector mounting holes secure the new detector to the detector board 2 The following image shows a detector side view of the d
42. is thin Use of brushes or other abrasive cleaning materials will remove the artiste plating and cause permanent damage to the performance of the trap 2 Carefully remove the electrodes from the peroxide solution and place them in a clean beaker of deionized water This will ensure that the peroxide solution and any contaminants that were removed from the trap parts do not redeposit before being rinsed off by the deionized water 3 Further rinse the parts thoroughly with more deionized water and allow them to fully dry before reassembly Trap reassembly 1 The following image shows the electrodes Ring Electrode Center Electrode football Bottom End Cap Electrode Top End Cap Electrode Figure 8 17 Trap electrodes 2 Use the alignment fixture to reassemble the trap 3 Install the alignment pins in the Bottom End Cap electrode The Bottom End Cap Electrode is differentiated from the Top End Cap Electrode by the number of larger holes The Bottom End Cap Electrode has fewer larger holes than the Top End Cap Electrode refer to the last image for help in properly identifying the electrodes 4 Place the Bottom End Cap Electrode on a clean flat surface with the curved side up Refer to the previous image for help in identifying which electrode is the Bottom End Cap Electrode The first pin is installed in the first threaded hole clockwise from the notch The image below shows the Bottom End Cap Electrode with the alignment pins in place
43. method with a new name f Rename Method This opens a dialog box that allows the user to change the name of the loaded method 55 OTHER OPERATIONS g Export Method This allows the user to save the method to a file h Send Method to Instrument This allows the user to load the method on to the attached instrument When loading the method there are two choices 2 All of the menu items are available by clicking on Method on the menu bar The following image shows the Method menu T CHROMION Target4P Figure 5 10 Method menu open Creating a New Method 1 Anew method can be created by clicking on Methods in the menu bar and selecting New Method 2 When clicking New Methodthe following dialog box will open asking for the user to enter a new method name By clicking the OK button a new method is created in the database New Method Name _ k Figure 5 11 New Method Name dialog box 3 After creating a new method the method settings forms Gas Chromatograph Target List and Performance Validation will become enabled under the large Method button in the navigation pane 4 Methods contain a lot of information In most cases it is easier to open an existing method and under the Method menu select Save Method As and give the open method a new name Then edit the method to contain the desired changes Load and Delete Methods 1 Selecting the Load Delete option opens the method list The following image shows
44. of a chemical is related to its retention time tr The retention time is the time a chemical takes to travel through the column The typical representation of a GC analysis is a plot of detector response as a function of time called a chromatogram see figure 2 2 The time at the center of the near Gaussian peak of a resolved chemical is its retention time and the area under the peak is related to the amount of chemical extracted and may be corresponded to the amount of chemical in the sample TUTORIAL 140000 130000 3 l T tR 1 Dimethyl methyl phosphonate DMMP 4 2 2 Chloroethyl ethyl sulfide 1 2 HD 110000 3 Diethylmalonate DEM 100000 4 Methyl salicylate MES 90000 2 5 2 Chloroacetophenone CN 80000 70000 1 60000 50000 5 40000 30000 20000 10000 02 04 06 O08 10 12 14 16 18 20 Time min Figure 2 2 Typical chromatogram obtained using the TRIDION GC TMS showing the retention time of diethylmalonate 3 A chemical that is volatile within the temperature range of the GC method parameters will eventually exit the column assuming the compound is not irreversibly adsorbed to the capillary coating If the Same method parameters are always used a specific chemical will have the same retention time Tentative identification of a chemical can be made by comparing its retention time with retention times of known standards Changing the temperature of the capillary column will change the retention times of compo
45. peak will be shown in the Deconvolution Control Center The area is the sum of the intensities of the ions that have been included in the deconvolved peak multiplied by the scan to scan difference in time The height is the height of the deconvolved peak ions and the intensity is the height of the selected scan 2 The following image shows a highlighted peak that is not in the Target List Grane RT 37 1 10 Sec AbuneS 303 Figure 5 62 Deconvolved data with an unknown peak highlighted 3 When a peak that is not in the Target List is selected the Deconvolution Control Center will display Unknown and then a number The number part of the label is random In the Deconvolution Parameter tab in Target List the user can specify the number of unknown peaks to show This is to maintain the speed of analyzing the sample when on the instrument If a complex sample is analyzed and it has a larger number of unknown compounds the processing can be very long By limiting the number of unknown peaks that are allowed to the 10 largest then the on instrument processing can still be kept reasonable 86 OTHER OPERATIONS If a large number of unknowns is expected and the intention is to obtain good search results for as many of the unknown compounds as possible then this setting can be increased to allow the software to deconvolved all of the unknown peaks 4 The following image shows the Deconvolution Control Center with the unknown peak highlighted
46. plotted side by side since the retention time of the data points is not a fixed time Therefore each set of data will have different times on the x axis This is a result of the dynamic ionization used in the toroidal ion trap Mass Spectrometer 1 The Mass Spectrometer screen is where the settings that control the instrument are configured and sent to the instrument It is also where the data for mass calibration are stored 2 These settings are not included in the method because they are specific to the instrument Methods can be transferred between instruments while the Mass Spectrometer settings cannot 92 OTHER OPERATIONS 3 Itis not recommended that most of these setting be changed Recommended default values are given in the Advanced Operations section of this manual Read the entire chapter before making any changes to the mass spectrometer settings Caution Changing setting on the mass spectrometer without proper training may cause damage to the instrument and may result in costly repairs Only adjust these setting if you have a complete understanding of what the setting is used for and what it does CAUTION 4 The button bar in the Mass Spectrometer screen allows the user to backup the settings for an instrument before making changes For the reasons stated in the above caution the settings from one instrument should not be loaded onto a different instrument 5 The following image shows the button bar for the Mass Sp
47. poe emer ae ad ene Methylene Chloride 4 1 7 1 4 net i Masses for lt Methylene Chioride gt m es tsk ts SC CU Figure 7 8 Methylene Chloride mass calibration in Performance Validation screen ix When using manual calibration the mass and bin number are entered into the manual calibration data section of the MS Calibrations in the Mass Spectrometer window x The next mass is from the MTBE peak Return to the Data Review screen The following image shows the TIC with the cursor on the MTBE peak 126 LIBRARIES MS Abundance Ready 2005 02 26 19 57 20 Figure 7 9 Uncalibrated mass data for MTBE xi The actual bin number for the 73 065 mass is 303 Return to the Performance Validation screen and select MTBE from the table to verify that the mass is in the window If the mass is not in the window adjust the minimum and or maximum values so that it is in the window to adjust the settings that will be used for auto calibration For manual calibration return to the MS Calibration tab in the Mass Spectrometer screen and enter in the mass and the bin number in the manual calibration data table xii Continue this process for each of the compounds that are used for calibration xiii The following table shows the chemicals that are typically used for calibration and the masses associated with the compound The bromopentafluorobenzene BPFB has two masses
48. red and black wires onto the top of the filament if they did not come pre installed on the new filament Ensure that the red wire aligns with the Egun pin on the RF board and on the brown plastic part of the filament assembly Make sure the black wire aligns with the Egun pin on the RF board and on the brown plastic part of the filament assembly 6 Use the 1 8 hex nut driver to make sure the nuts on top of the filament are tight 7 Slide the wires of the new filament onto the pins on the RF board Einsel lens maintenance Einsel lens cleaning procedure 1 Follow the instructions in the Remove ion trap RF module section of this chapter 2 The following image shows an exploded view of the einsel lens assembly 147 SERVICE Nut and Washers ail Barrel Einsel Lens EGUN Mount Figure 8 23 Einsel lens exploded view 3 Follow the instructions in the Filament Replacement section and remove the filament assembly 4 Slide the Einsel Lens wire off the Einsel Lens and off the pin on the RF board Set the wire aside on a clean lint free surface 5 Use the provided 5 32 hex nut driver to remove the Einsel Lens nuts 6 Lift the barrel off 7 The Einsel Lens is comprised of a brazed together ceramic spacer and a stainless steel lollipop shaped electrode Remove the Einsel Lens from the Barrel 8 Clean the Barrel and the Einsel Lens using soap Alconox works well water and a soft bristle brush or cotton tipped swab 9
49. system to shut down without going through the normal process This should not be used except in emergency situations since not following the normal shut down process risks pulling contaminants from the turbo pump back into the vacuum chamber 4 The following image shows the location of the Reset and Emergency Shutdown buttons They are located under the utility cover on top of the instrument Reset Button l Battery Connection Emergency Shut Down Button Figure 7 3 Reset and emergency shutdown buttons 5 To activate either button press it down for approximately one second and then release the button Delete all sample data from the SD card 1 Refer to the Instrument Operation chapter in the Manage Files Section of this manual for directions on deleting files directly from the instrument 2 Refer to the File Manager section of the Software chapter of this manual for instructions on deleting and moving files from the SD card using a computer 3 Itis also possible to remove the SD card from the instrument and install it into a card reader slot on a computer The use standard Windows functionality to view move or delete files from the card TRIDION Manual Mass Calibration 1 Preparations a Chemicals used in calibrating a TRIDION instrument i Provided standard CALION Performance Validation calibration vial CV mix ii The image below shows a chromatogram of the Performance Validation mix 122 LIBRARIES 45 C 30 s D
50. that are used xiv In some cases it may be necessary to zoom in the view of the uncalibrated mass data to accurately determine the correct bin number for a given mass 127 LIBRARIES XV The following image shows the zoomed in uncalibrated spectral data for bromoform The masses are 171 173 and 175 1 175 1 157 1 190 l l 1150 1200 il LLI Figure 7 10 Uncalibrated bin data for bromoform masses 171 173 and 175 XVI xvii xviii X X XX After all of the data for the masses and corresponding bin numbers have been entered it is necessary to return the TRIDION to the proper settings so that the new mass calibration will be used To use manual calibration leave the Use auto calibration data box unchecked Place a check box in the Manual check box In CHROMION Mass Spectrometer screen change the following values Control RunningAverage IsOn true Control Hanning IsOn true Control BinCollapse IsOn true Control GaussCentroid IsOn true Send the new settings to the TRIDION by selecting the Send Mass Spec Settings to Instrument button on the menu bar d Validate the calibration using the CALION mix Run a sample from the CALION vial by placing the SPME fiber into the vial following the procedures described in the How to sample headspace vapors from liquid or solid samples section of the Basic Operations chapter Follow the standard procedure for starting a run by starting the SOP and following t
51. the display to the Home screen and will save the Date Time Settings 40 INSTRUMENT OPERATION 7 The following image shows the screen that is displayed after selecting the Password button on the System Settings screen Target4E Torion 1 SystemBlank Change Password Old Password New Password Confirm New Password Change Password Cancel eet slot eee Figure 4 49 Screen showing the password setting screen 8 This screen is used to change the system password 9 The following image shows the screen that is displayed after selecting the Update Firmware button on the System Settings screen Target4E Torion 1 SystemBlank 2 Calibration D Data ma irmware 1 5 Libraries D Library LoadedMethods a Methods Figure 4 50 Firmware updating screen 10 When updating any Firmware on the instrument a Torion Service Technician will give the user step by step instructions at the time of the update 11 The following image shows the screen that is displayed after selecting the Install Update button on the System Settings screen 41 INSTRUMENT OPERATION Target4E Torion 1 SystemBlank Set Date Time Unable ToFindUpdate um Bluetooth Control Figure 4 51 Install update error screen 12 When updating any Firmware on the instrument a Torion Service Technician will give the user step by step instructions at the time of the update 13 The following image s
52. the ion trap RF module removed from the TRIDION 140 SERVICE Handles lon Trap RF Module Figure 8 14 lon trap RF module removal Trap maintenance procedures Trap disassembly 1 The following image shows an expanded view from the trap side of the ion trap RF module The following instructions will tell how to disassemble the trap portion of the module Use this image as a reference during the disassembly of the module Filament EGUN Mount Polyimide Spacer RTD Trap Assembly Ceramic Spacers RF Wire and RF to Center Electrode Tab Heater RF Board and Trap Mounting Hardware Figure 8 15 Exploded view of main trap components 2 The following image shows the location of the wires on the trap assembly 141 SERVICE RF Wire Center Electrode football Tab Red Filament Wire Black Filament Wire Einsel Lens Wire Top End Cap Electrode Wire RTD Wires RF RF Wire EGUN Filament Red Wire EGUN Filament Black Wire DET CAP No Connection FILGATE Einsel Lens Wire FILCAP Top End Cap Electrode Wire RTD Black RTD Wire RTD White RTD Wire HTR Either Heater Wire HTR Either Heater Wire Figure 8 16 Trap wire locations 3 Gently pull the wires for the Heater RF Red and Black Filament wires Einsel Lens Top End Cap Electrode and RTD loose from the pins on the board 4 The 5 64 hex driver is used for all of the screws on the trap assembly 5 Remove the screw that is holdin
53. the location of the files that are to be added to the table Click on the name of the first file to be added to the table Then while holding the shift key click on the name of the last file to be added to the table Alternatively while holding the control key down click on the names of files you want added to the table After the files names have been highlighted click the open button to add them to the table To remove a file from the table right click the mouse on the name of the file that is to be removed and select remove file from the popup menu The Date column shows the data that the file was created The Clear All Entries button removes all of the file names from the table except the original file that was open when the overlay menu was opened The X Offset allows the user to move a files starting time location to adjust the alignment with other TICs that are being overlaid 83 OTHER OPERATIONS 12 The Y Offset allows the user to move a files intensity to adjust the alignment with other TICs that are being overlaid 13 The Cancel button returns the user to the default graph window view of AP 14 The OK button opens the overlay window view shown below Torin AP Sothern Sonalar inatedata ind ioe CO Mest TE be 1 HE Figure 5 58 CHROMION overlay view window 15 The user exits out of this window by pressing the overlay files On Off button on the button bar which looks like two overlaying pieces of paper 16 Th
54. the method list 56 OTHER OPERATIONS Target4P 4 2 2012 11 15 09 AM lt aa lt lt 3 19 2012 5 35 71 PM Indicates the method you are currently editing _ Delte ok Canca_ Figure 5 12 Load Delete Dialog Box 2 Highlight a method by clicking on the name 3 Select OK to load the method 4 Select Delete to delete the method Importing a Method 1 The Import Method option opens the following dialog box Import Method O O OOOO Source f Currently Loaded Method On Instrument From Local File From Remote File On Insrument default_1 7 met PY iris ret Figure 5 13 Import Method dialog box 57 OTHER OPERATIONS 2 This dialog box allows the user to import a method into the CHROMION data base from three different locations a Currently Loaded Method On Instrument loads the current method from an attached instrument If there is no instrument attached this option is not available b From Local File allows the user to navigate to a file location on the PC where an exported method file has been saved c From Remote File On Instrument activates the list of files shown in the Remote Files window located at the bottom of the dialog box The user can open one of the files by selecting it from the list then clicking the OK button If an instrument is not connected then no files will be visible in the Remote Files window Saving a Method 1 Select Save to save the currently loaded method
55. this manual Refer to the NIST and AMDIS documentation and help files that are included with the software for instructions on how to use the software 111 OTHER OPERATIONS 6 Other Operations This chapter describes how todo other operations suchas changing the battery connecting to power changing GC camergas and other similar operations Power supply and battery 1 The TRIDION can operate from a power supply connected to line power or a battery Under typical operating conditions the battery will allow field operation for about 2 hours The actual run time may vary by up to 15 minutes depending on the frequency of injections The battery used in the GUARION is a 15 V 13 8 MAH rechargeable Li ion battery The battery can be charged either with an external charger or by plugging the instrument into line power while the battery is installed When charging the battery with the instrument the instrument does not have to be on just simply plugged into line power The following image shows the battery indicator lights on the TRIDION Toarion Technolo ih Figure 6 1 TRIDION battery indicator lights If the top indicator light is lit the TRIDION is connected to line power and there is not battery installed If the second indicator light is lit then the TRIDION is operating from battery power only If the bottom indicator light is lit the TRIDION is connected to line power and the battery is installed and charging The
56. to a file dialog Send a Method to an Instrument 1 Before sending a method to an instrument it is necessary to save any changes that have been made to the method Caution Because of the structure of data entry tables in Microsoft Windows it is necessary to save a method to ensure that all changes have been accepted Changing a value in a table and exiting the part of oN the software where the change was made without first saving the change can result in the value reverting back to the original value 59 OTHER OPERATIONS 2 Selecting Send Method to Instrument send the loaded method to the currently connected instrument 3 The following dialog opens Send Method Figure 5 19 Send Method dialog box 4 Theuser has two options a Send and activate sends the current method to the connected instrument and makes the method the active method b Send sends the current method to the connected instruments SD card for later use 5 The following dialog box opens to confirm that the method was successfully sent Success x Method successfully sent and activated Figure 5 20 Method successfully sent and activated dialog box 6 Ifthe Send option was selected the dialog box will indicate that the method was sent but will not say that it was activated 7 Ifthe send fails a dialog box will open that indicates that the method did not reach the instrument If this happens try resending the method If the failed
57. to connect to instrument Verify the IP address Figure 5 9 Message showing that the software failed to connect to an instrument 11 In the case where an instrument cannot be connected check the network cables and the IP address settings to ensure they are correct for the type DHCP server or Direct of connection you are attempting to make Methods Menu Caution The instruments operational parameters for the Gas Chromatograph and Mass Spectrometer can be altered by creating a method in CHROMION and sending it to the instrument Many of the parameters interact directly with important instrument functions Be sure to use caution when changing these operational parameters as making inappropriate adjustments will result in poor instrument performance and could cause damage to the instrument Method Menu 1 The options available under the Method menu are a New Method This opens a dialog box where the user can enter a method name and then creates the method in the database b Load Delete This opens a dialog box that allows the user to load a method into the software or to delete methods from the data base c Import This allows the user to import an exported method This is a convenient way to move information like target compound lists and GC parameters from one TRIDION 9 to another TRIDION 9 d Save Method This saves the method to the data base e Save Method As This opens a dialog box that allows the user to save the
58. to the currently open library j Create New Compound This option creates a blank line in the compound list and opens the Compound Details tab for data entry k Copy Compound This option creates a copy of an existing compound in the Library Compounds table To create a copy highlight the desired compound then click the Copy Compound button A compound with identical information is added just below the selected compound It has the name modified to say copy X The X is an incremented number that increases by one for each copy made For example if a copy of benzene is made the new compound would be named benzene copy 1 If a copy of toluene is then made it would be named toluene copy 2 The compound can then be renamed and edited The columns can be sorted by clicking on the top row of the Library Compounds table The Search Compound field can also be used to find the new compound Remove Compound This option is used to delete a compound from the compound list Select the compound by clicking on it Then click the Delete Compound button A dialog box opens allow the user to confirm that they would like to delete the compound 9 The following image shows the Library Editor button bar with the Compound Details tab open 100 OTHER OPERATIONS Figure 5 80 Library Editor button bar with the Compound Details tab open 10 The following are descriptions of the Library Editor buttons that are active when the Compound Details tab
59. to the next step in the SOP 23 Once the instrument has finished the entire SOP the following screen will appear Torion The current procedure has ended R Start the current procedure over again Restart Procedure Analyze samples using the last method Activate from the procedure that ended Last Method Advanced Start Run Previous Results Figure 4 33 Current procedure has ended screen 24 Selecting Restart Procedure will start the SOP from the beginning with first running a System Blank 31 INSTRUMENT OPERATION 25 Selecting Activate Last Method will allow the user to run samples on the instrument using the last GC method This bypasses having to re run a System Blank or Performance Validation prior to running samples 26 Selecting Advanced or Previous Results will move to these functions within the user interface which are discussed in detail in the following sections Advanced 1 Pressing the Advanced button from any screen within the user interface displays the following Target4E m D orion ey 4 Sample W y 4 Status Procedure f Diagnostics screen Figure 4 34 Advanced screen Procedure Button 1 The Procedure button will be used to select and load various SOPs Status Diagnostics Button 1 Selecting the Status Diagnostics button opens the following screen 32 INSTRUMENT OPERATION Taraet4E P Torion Technologies activated2012 04 16 13 35 40 1 S
60. way to transfer files to and from the instrument SD card 2 From the file manager the user can create a directory on the connected computer and can move data files to the computer from the SD card The types of files have been described earlier They are a RES These contain all of the results of an analysis including the data and the libraries settings and reports that were generated or used during an analysis It is highly recommended that these be the files moved to the computer b Zip These are the results files for Performance Validation runs and are used in the Tuning Wizard Like the RES files they contain all of the information used and generated during a Performance Validation run cC CDF This is the data that has been converted to usable searchable data These files are contained in the RES file d RAW This is the unconverted data that is gernerated by the instrument These files are contained in the RES file e TXT These are a text report file generated during an analysis The same data as that shown on the instrument front panel is contained in this file These files are contained in the RES file 3 The following image shows the File Manager E E P En 3w H T Xilinx El Storage Card FA aaBdb2c7cc27e7112d9eb0 Calibration H T Beagle Data H S Bugga 4 Datal H S Calibration H E Libraries E E Library El El LoadedMethods H Documents and Settings m autocal H From15Data gt metho
61. 2 03 29 03 41 SystemBlank giannis 2017 02 20 N 46 CuctamRiank Figure 4 55 Choosing a data file to view previous results 4 To choose a datafile select it from the list by touching it to highlight it 5 The user can move through the Results list by either using the arrows and sliders on the edge of the results window or by using the Up and Down buttons 6 Choose the View button to view on the instrument the results of the data file The following screen is displayed while the instrument loads the data file Target4E Torion 1 S ystemBlank Identification Figure 4 56 Wait screen while instrument processes previous data 7 The following screen is displayed once the data file has been loaded onto the instrument 44 INSTRUMENT OPERATION Target4E Torion 1 SystemBlank 3 8 ee 9 10 7 Acetone 11 7 Unknown 3 12 6 Methylene Chloride More Figure 4 57 Previous data displayed with library identification table 8 The same data is displayed as when the analytical run was processed the first time Export Files 1 There are two ways to export files from the instrument SD card to a USB storage device 2 From the Home screen choose the Previous Results button and then choose the Export button The following screen will be displayed Target4E Torion 1 SystemBlank Source Folder 2012 03 29 Check box to select file s E 20sample0i 2012 03 29 00 11 23 cdf l Select All 120sample01
62. 2012 03 29 00 11 23 raw I20sample01 2012 03 29 00 11 23 res 120sample0i 2012 03 29 00 15 14 cdf E 120sample01 2012 03 29 00 15 14 raw 20sample01 2012 03 29 00 15 14 res Ana lAN Ana A An AND AIA ae mal Export Files Figure 4 58 Export Files screen 3 To choose a data file select it from the list by touching the box on the left to place a check in the box 4 The user can move through the list by using the arrows and sliders on the edge of the window 45 INSTRUMENT OPERATION 5 The user can select or deselect all of the data files by using the corresponding buttons on the right of the screen 6 Once one or more files have been selected choose the Export Files button and the following screen will be displayed Target4E Torion 1 SystemBlank Please Select a Folder El D Application Data Documents and Settings 1 5 Hard Disk D Data Files B Lost Clusters D My Documents Program Files D Recycled Folder Hard Disk Figure 4 59 Selecting where to export files to 7 A Windows directory is displayed on the left The user should navigate to and highlight the location where the data files will to be exported to The Hard Disk is the storage device plugged into the USB port Choose OK to export the data files 8 When the data files have successfully been exported the following screen will be displayed Tarqet4E Torion 1 SystemBlank Source Folder 2012 04 02 Figur
63. 7 16 Performance Validation correction showing methyl salicylate peak with binned centroided but B acats 7s ete Es seer nee Peer E TRE cP SPREE E SET RPP ROR EEEE E E EE err rarer een oe 133 Figure 8 1 Dust off A Kimwipes B Lint free antistatic gloves C Tool for removing o rings that will not scratch the surface of the o ring groove D Methanol E Magnifying lens F sssesseesssesssesssessseesseesseesseessseosseosseesseesseesse 135 Figure 8 2 Properremoval OF ORT INO sssaaa neioii REEERE EE EEEE EEA Rai 135 Figure 8 3 Wet lint free tissue with cleaning solvent A Clean o ring groove with wet tissue B sssssssesssessserss 136 Figure 8 4 Cleaning ea ER ES A A A A E 136 Figure 8 5 Dust off o ring groove s sssesssessseesseesseessressscesseesseesseeosseosseosseesseesseeosseosseosseoeseeuseeoseroserossroseosseesseeeseeoserossroseeosseesseresersss 137 Figure 8 6 Inspecting o ring for defects esessssesssesssesssessserssseosseosreosseessersssrosseosreosseosserssersserosreosseosseesseessersssrosseosseosseesssesssrssersss 137 Figure 8 7 solvent Cleaning the o ring with solvent wetted lint free tiSSUe sss ssseesseesssesssessseesseesseessseosseosseesseesseesss 138 Figure 8 8 Using dust off to remove dust particles from an O ring s sseesseesssesesesseesseesssessseosscosseesseesseeoserosseosreosseesseessersss 138 Figure 8 9 Storing a clean o ring in a dust free environMent sesesserssersseesssessseesse
64. 9 Ready T T 9 Validation G36 80 Cad G36 Pate DFP S caf Figure 5 47 Library Search Spectra LibSrch graph with the TIC and MS graphs 6 The next three buttons are used to set the cursor mode The following image shows these buttons highlighted with their labels Er LA T Ua ae och 362 all Al BB A Set Mode to Zoom r LA Abe CRN ab al REE lh gt OF a Bey Uy de A oR are ee ae Oe ee CIE Figure 5 48 Data Review button bar with cursor mode buttons highlighted and labeled 7 The following describes the different cursor modes a ZOOM When the cursor is set to the zoom mode the user can enlarge parts of any of the graphs that are open To zoom in the user uses the mouse to drag a box around the area they want to zoom in on To activate Unzoom move the mouse so the pointer is over the graph that is being worked on For example to unzoom the TIC use the mouse to place the pointer over the TIC graph then click the right mouse button and select unzoom from the menu The following image shows the right click popup menu UnzZoon Unzoom All Cursor Mode Glear Region Figure 5 49 Right click mouse menu for unzoom function There are two modes of unzoom The Unzoom function steps the zoom back one step The Unzoom All function returns the graph to a completely unzoomed state 78 OTHER OPERATIONS b Summed Select When the cursor is set to this mode it is only functional in the TIC In all of
65. B peak retention time should be 48 1 and it has a window from a low of 46 to a high of 53 The actual retention time of the BPFB peak is 45 8 This is not within the retention window set in the calibration table As a result the calibration will fail To fix this change the calibration window to a low of 42 and a high of 50 with an ideal time of 45 8 The same process must be completed for all peaks used in the auto calibration file to determine that the actual retention times are falling within the set retention times The same process must be completed for mass calibration The following shows the methyl salicylate peak highlighted The mass that is being used for calibration is mass 152 047 This corresponds to a bin number of 1005 Scan 498 RT 74 2870 Sec Abun 69 632 Figure 7 146 Performance Validation correction showing methyl salicylate peak with binned centroided but uncalibrated data The Mass Calibration table above has a window of 980 to 1000 As a result the methyl salicylate peak will fail calibration since the actual index is 1 005 as shown in the figure above To fix the mass calibration change the window so it is more centered on the actual bin number of 1005 by setting the low index to 995 and the high index to 1015 Repeat this process for each of the peaks and the associated masses Once all of the data has been corrected save the method and then send the new method to the instrument by selecting the Send Me
66. C has been selected 5 The masses used in a RIC trace can also be selected from the main window by using the right click menu to open a pop up dialog box in the RIC display chart The following shows the menu used to turn RIC selection on and off Figure 5 54 RIC edit masses right click popup menu 6 In addition to the popup menu having the RIC display window open also enables RIC selection from the MS chart 81 OTHER OPERATIONS 7 With RIC graph open the user can add ions to the RIC table by simply clicking on the mass in the MS chart 8 Using the menu the user can open the RIC table to see and edit the list of the selected ions 9 CHROMION AP shows the selected ions as colored numerical references along the top edge of the RIC graph window This is shown below with a mass of 272 being shown in the RIC window and in the box in the top right corner of the RIC graph It is color coded to assist in identifying the trace in the RIC chart and the selected ion in the MS chart Ts CHROMDON dla Fle Ede Method Teos Instument View Toggle Dapostks x dg 454 iii amp uniDlee lt EA if ka RT 44 7050 Sec Abun 49 535 Aimane 108 Gira Rendy ClDocuerts acct Sects che lene octal ik Da des CDF AS ot Figure 5 55 RIC ion selection from MS graph 10 To remove ions from the screen right click on RIC graph to open the popup menu From the menu the select clear all masses to delete them from the RIC masses table or the RIC Mas
67. CHROMION main window with Navigation pane Collapsed ou ssssssssssssececscsssscsecscscsssssesecscssssssesesscsencasees 49 Figure 5 3 Preferences fOrM emer eenen eee rena er ees ern ne one ned en anes ee 51 Figure 5 4 Hazard levels dialog ION g2ecsecseccazezeaseecarvcdzcacsecseaeseesezeseesezescascarscdeadesessasesce cccesce cescsceccgeaeaccgeacscescacsccscacsecseacnecseassccseueszesezede 52 Figure 5 5 Instrument Setup when adding an instrument for the first time ssesssesseessesseessesssesseessesseesseoseesseoseesseoseessees 53 Figure 5 6 Instrument Setup after adding instruments sssesssessseesseesssessseesseesseessersssessseosseosseesseesseroseeosseosseosseesseesseesseessseossees 53 Figure 5 7 connect an instrument to CHROMION seessessessesscsecsscsseoscoseoseossoseeseesecsscsscoscoscossossossoseoseesseseessesscsscoecossossossossoseeseess 54 Figure 5 8 Screen showing the icon in the navigation pane has changed to show that instrument T14 is now connected and the instrument name is highlighted IN green es ssessessessessesseoseeseeseessessessessesseoseoseoseoseoseoseeseese 54 Figure 5 9 Message showing that the software failed to connect to an instrument es sssessseesssesssessseesseesseesseesssesssess 55 POUES IONE Gd MENU ODE rera EE EE E 56 Figure 5 11 New Method Name dialog DOK sireisas NS NNN NSA EN 56 Figure 5 12Load Delete Dilog DOR eee ee 57 Figure 5 13 Import Method dialog DOX ssessessessessesseeseessesees
68. Compound Clicking this button inserts a line at the end of the compounds list Details about how to enter a new compound are described below This button is only available in the Target List tab 3 Remove Target List Compound Clicking this button will remove a selected compound from the target list Details about how to remove a compound from the target list is described below This button is only available in the Target List tab 4 Send Unknown Libraries To Instrument If a library has been referenced on the Deconvolution Parameters tab then the user can send the referenced library to the instrument Depending on the size of the file sending files to the instrument can take from a few seconds to a few minutes Because of the potential size of the library files the libraries are not sent every time a method is sent This button is only available in the Deconvolution Parameters tab 5 Reset Deconvolution Parameters to Default Values Clicking this button resets the Deconvolution Parameters to factory defaults All changes to the parameters will be lost This button is only available in the Deconvolution Parameters tab 6 Export Target List to File This opens the normal Windows file save dialog box and allows the user to save the Target List as a file for use in other methods OTHER OPERATIONS 7 Import Target List from File This opens the normal Windows open file dialog box and allows the user to open a previously exported Target List
69. Create a data folder on the computer by right clicking on the computer drive C or a sub folder of C The following image shows the create folder menu that open after right clicking on a folder on the left side of the File Manger window 95 CAUTION OTHER OPERATIONS c 9b7e30c2d4383ef0adcbecf4 backup Gey F GO dell Create Directory Rename Directory gt ProEssentials6 ProgramData Ii Swsetup System Recovery gt temp TSWG OSHA Data Figure 5 76 File Manager Create Directory and Rename Directory dialog box Click on the name of the folder where the files are to be stored The frame at the bottom left side of the window will display the files that are already in the folder If it is a new folder the bottom left frame will be empty Click the plus symbol next to the top folder on the right top side of the screen This will expand the tree view Next select the plus symbol next to the folder labeled Storage Card and the tree view will be expanded Next select the plus symbol next to the data folder Finally expand the folder that is labeled with the date when the data were collected The data will be displayed in the bottom right frame Click on the RES file name that you want to move and while holding down the mouse button drag it to the bottom left frame To select multiple files click on the top file that is to be selected then press and hold down the shift key then click t
70. DION is used to separate and identify volatile and semi volatile organic compounds present in gas liquid and solid samples The CUSTODION SPME syringe is used to extract various classes of compounds depending on the sorbent coating of the fiber and to concentrate the sample for improved sensitivity at low concentrations The CUSTODION is used to introduce the sample into the TRIDION After injecting a sample into the TRIDION it is separated into its chemical components Resolved components are characterized by retention time from the gas chromatograph GC and mass spectral fingerprint from the toroidal ion trap mass spectrometer TMS The mass spectral fingerprints of the chemicals are compared to a database of known mass spectral fragmentation patterns and are identified by the on board library TUTORIAL 2 Tutorial This chapter provides a tutorialabout solid phase microextraction SPME low thermal mass LTM gas chromatography GQ and toroidalion trap mass spectrometry TMS What is solid phase microextraction SPME olid phase microextraction SPME is a sampling method for extracting target chemicals from a gas liquid or dissolved solid sample and concentrating them for subsequent analysis Compared to liquid liquid extraction and cartridge based solid phase extraction SPME is faster and less prone to user error Following extraction SPME allows immediate introduction of sample into the analytical instrument SPME consist
71. Deconvolution Control Center j ioj x Run All Resuts E Retention time 35 354 Seconds Name Area Height Intensity Ready Unknown 5 Known 12 Figure 5 63 Deconvolution Control Center with Unknown peak 2 selected in the TIC 5 The area is the sum of the intensities of the ions that have been included in the deconvolved peak multiplied by the scan to scan difference in time The height is the height of the deconvolved peak ions and the intensity is the height of the selected scan 6 Selecting the All Results tab opens the following table 87 OTHER OPERATIONS Deconvolution Control Center i E m x Fin All Results 27121 31 Figure 5 64 Deconvolution Control Center All Results tab showing unknown 2 identified as tetrachloroethylene 7 The unknown peaks are compared to the unknown library that is selected in the Deconvolution Parameters tab in the Target List The number of possible peaks that will be is set in the Deconvolution Parameters tab The possible matches are sorted on Match Factor The following image shows the Unknown 3 peak showing three possible matches The correct match is acetone Deconvolution Control Center Trimethylamine waar 106207 maw hs l ee o om 2 aoe a 0 wms O S S Ready Unknown 5 Known 12 Figure 5 65 Deconvolution Control Center showing the All Results tab with multiple possible unknown matches for the peak labeled Unknown 3 88 OTHER OPERATI
72. F 3 coeoogno coF E coeongPo CDF E cosogoo cDF E coson9R0 cOF S coeo0o50 CDF E coeoogTo cor E co6o0QU0 CcDF E cosooqva cor ed CoeoooWwo CDF E coscogxa coF 23 COBO0RO0 CDF COG00R10 CDF COS00R20 CDF 23 CO600R40 CDF 3 CO601410 C0F 3 COEO1A20 CDF CO601430 CDF a COBOLA40 CDF 23 CO6O1A50 CDF 23 COe01460 CDF CO601A70 CDF a COE01A80 CDF E Coe01AA0 CDF CO601 4E0 CDF fl COBO1AFO CDF C0601460 COF E COOL A10 CDF 0601410 CDF E COBOLAKO CDF eS CO6014L0 CDF E CO601 4M0 CDF CO6014N0 CDF E CO601A00 CDF T C0601 ASO CDF E co601 ATO CDF z CO6014 0 CDF Ger 3 COBOLAVO CDF CO601 420 CDF CO601B20 CDF a CO6O1B30 CDF 3 CO601B50 CDF A COe01B70 CDF CO601B80 CDF a COBOL BAC CDF E CO60LBFO CDF COB01BHO CDF CO601B10 CDF CO601BL0 CDF E coe01850 CDF a is Ei z 1 Et Ee EL E coeo1 460 CDF 3 COBO LADO CDF E COBOLETO COF CO6018 0 CDF CO601AWO CDF J cogair coeniAxo CDF gt E cosnooz0 cOF Mu Computer w File name E F My Network Files of type EDF Files cdf v E Open iF Cancel Figure 5 57 File window used to select multiple data files for display in the overlay graph From this window the user can select and insert multiple files into the overlay file table To select multiple files click the Multi Select button at the bottom of the window Navigate to
73. F TORION A Solid Science Creative Ideas Innovative Products User s Manual TRIDION 9 Gas Chromatograph Toroidal lon Trap Mass Spectrometer GC TMS TORION TECHNOLOGIES INC TRIDION Torion Technologies Incorporated 796 East Utah Valley Drive Suite 200 American Fork UT 84003 Phone 801 705 6600 Fax 801 705 6649 Email information torion com Version 2 0 1 May 2012 Table of Contents DMT OCC ON aac tease TEE EEEE edi cee cade cede ceeds 1 2 NOON oerna EE EEE EIEEE E EEEE E E EEEE E EE EEES 2 What is solid phase microextraction SPME ccccceeeceeeeeeeeeeeeeees 2 What is the CUSTODION SPME syringe cccccccececeeeeeseeeeeeeeeeeaes 3 What is low thermal mass LTM gas chromatography GC 3 What is toroidal ion trap mass spectrometry TMS cccccseeeeeeeeees 4 What IS the TRIDION cot taiesesc cece date ercer ETE 6 3 Basic CUSTODION Operations cc cceccccseeeeceeeeeeeeeeesaeeeesaeeeeseeeeeseeeeeeas 8 Prepare the CUSTODION SPME syringe for Sampling c ceeee 8 Using the GUST ODIO csc cctrnuices dines cede cedex EEE EEEN ERAEN 8 Sample headspace vapors from liquid or solid Samples 00008 8 ANI ISO a SSS terse ce eres E E E E E 9 Seo 294 e 10 0 eee ene ee E 9 Sample SOLIGS cecccesececsesececcsecescsesecceecesesececeseeesceneeccaneeceeeencseresceeess 10 Sample unknown liquids and SOS
74. Figure 2 7 Top view TRIDION GC TMS BASIC OPERATIONS 3 Basic CUSTODION Operations This chapter gives basic instructions on how to use the CUSTODION Prepare the CUSTODION SPME syringe for sampling ach CUSTODION SPME syringe is shipped with the syringe needle protected by a screw tight cap Prior to use remove the protective cap Prior to initial use the SPME fiber should be conditioned by placing it in a heated GC injection port for at least 15 minutes For multiple use application the SPME fiber in the CUSTODION syringe should be cleaned before re use as outlined in the following steps 1 Insert the syringe needle with the fiber retracted of the CUSTODION syringe into the injection port of the TRIDION or other GC heated to at least 250 C 2 Depress the plunger to extend the SPME fiber and allow the fiber to desorb contaminants for 30 60 seconds or longer if necessary 3 Depress the plunger to retract the SPME fiber 4 Remove the CUSTODION syringe needle from the injection port 5 Start the TRIDION and conduct a System Blank Run to remove any compounds that may have desorbed from the SPME fiber into the GC for instructions on performing a System Blank Run see the TRIDION Operation chapter 6 If large amounts of sample are visible in the blank analysis repeat the SPME cleaning process until no large peaks are visible in the System Blank Run Using the CUSTODION 1 Detection of target chemicals by the TRIDION depend
75. Figure 5 45 Difference Diff graph with TIC graph uu esesssscssssssesscscsssssssessccscsssssesecscsesssssesescseassssesecsesesssssesecseseacsesesecseacaes 77 TROUBLESHOOTING Figure 5 46 Deconvolution Decon graph With TIC Graph essssssssececscssssssscsececscsssssesecscesesesesesecscscsesesececcnsacsesesecneneacees 77 Figure 5 47 Library Search Spectra LibSrch graph with the TIC and MS graphs sssssssscscectssesesececsstssssesesseseneeeees 78 Figure 5 48 Data Review button bar with cursor mode buttons highlighted and labeled s sssssesssesseessesseessesseessees 78 Figure 5 49 Right click MOUSE MENU for UNZOOM FUNCTION ccscsssecscssscscassssscassesscarsesecasassecasassecssassecscasseescosseeseasseescasseeseans 78 Figure 5 50 Data Review right click dialog with Clear Region menu expanded 1 esessssssssececscsctesssesecscseeseseeeeseteneseees 79 Figure 5 51 Copy lons from RIC to TIC Select Overlay File List Change Overlay Files On OFF Launch Deconvolution Control Window and Launch NIST Search buttons sects reer eres 80 Figure 5 52 Copy lons from RIC to TIC showing Masses 98 99 ANC 100 ssssssessssececsssectsssseccseseccsesececsessccssssscesscescees 80 FOU Sas INS SOS CMOS gastos S 81 Figure 5 54 RIC edit masses right click POPUP MenU s ssessessessessessesseoseeseeseessessessesseoseoseoseoseoseosseseesresseoresseoseoseoseossoseoseoseeseeseess 81 Figure 5 55 RIC ion selection from MS graph cescassicicciccescccacesce
76. ION software is also used to view and work with chromatographic and mass spectral data from the TRIDION instrument VNC Viewer This software is used to monitor and control the TRIDION from a PC NIST This is the NIST mass spectral library and software used to interact with the library CHROMION Installation and Operation 1 Locate the folder in which the CHROMION setup exe is located 2 Double click setup exe to install the program following the instructions on the screen 3 ACHROMION icon will automatically be installed on the desktop 4 Double click on the icon to run CHROMION CHROMION Main Screen 1 This image shows the initial screen that appears when opening the CHROMION software 48 OTHER OPERATIONS es ad m Figure 5 1CHROMION main window 2 There are many ways to navigate within CHROMION The main functions are accessible from the navigation pane on the left side of the screen 3 In addition to the main functions other functions are available thru the top bar menus the button bars and by using right click popup menus 4 The navigation pane on the left side of the screen provides centralized navigation to easily access the CHROMION forms which are bundled in different categories such as Method Tools and Instruments 5 When using a lap top it can be useful to hide the navigation pane in order to increase the viewable area of the screen The Navigation pane can be easily hidden and unhidden by clicking on t
77. ME fiber is completely retracted before pulling the CUSTODION syringe needle out through the sample septum CAUTION Sample gases 1 Vapors in air or other gas samples can be sampled directly or from a gas sampling container using the CUSTODION syringe The steps for vapor headspace analysis as discussed above should be followed when applicable Sample liquids Caution Samples that are too concentrated will overload the GC column and TMS possibly requiring cleaning of the system CUSTODION SPME fiber ion trap etc before the next sample can be analyzed Of particular concern is the viscosity of the liquid sample Viscous samples should never be sampled and analyzed directly CAUTION 1 Place the liquid or dissolved solid sample into a sample vial Add sufficient volume of liquid to completely immerse the SPME fiber when it is fully extended from the CUSTODION syringe needle BASIC OPERATIONS 2 Cap the vial with a septum cap 3 Insert the CUSTODION syringe needle through the sample vial septum Caution Be certain that the SPME fiber is retracted inside the CUSTODION syringe needle before piercing CAUTION it through the sample vial seotum Caution Be careful not to bend the flexible SPME needle when piercina the septum CAUTION 4 Check for adequate space inside the vial to extend the CUSTODION fiber without touching the sides or bottom of the vial 5 Depress the CUSTODION plunger to ext
78. Make sure the notch aligns with the notches in the Alignment Fixture Bottom End Cap Electrode and Center Ring Electrode Remove one of the three alignment pins Install one of the three screws with the polyimide spacer in the hole where the alignment pin was removed and tighten it so it just begins to clamp the assembly together In a later step the rings still need to be able to move so do not over tighten the screw at this point One at a time remove each of the other alignment pins and replace them with the screws and polyimide spacers Tighten them so they just begin to clamp the assembly Grasp the outside of the Alignment Fixture and gently squeeze so that the inside comes in contact with the trap assembly on three sides This will align the ring stack 144 SERVICE 18 While holding the Alignment Fixture in contact with the rings tighten each screw until they are snug Avoid tightening one of the screws all of the way down before tightening the other two screws Over tightening one screw will cause the stack to go out of alignment 19 Continue tightening the screws sequentially until they are tight It is not necessary to exert excessive force on the screws but they need to be tight enough to keep the stack from moving If a torque screwdriver is available a final tightening to 12 in oz is recommended Mount the trap assembly onto the RF board 1 Use the following image to orient the trap on the RF board No
79. ON before continuing with analysis TRIDION is dropping data points Under typical parameter settings the TRIDION should produce 7 10 scans per second If the TRIDION is dropping data points contact Torion Technologies 159 TROUBLESHOOTING Table of Figures Figure 2 1Diagram of the CUSTODION sampling Syringe csssesesesscssssssssecscsssssssssessescscsssesescsesssssesecscscsesssesecscscacasseseescseseassees 3 Figure 2 2 Typical chromatogram obtained using the TRIDION GC TMS showing the retention time of HES GUY MTV CAN Se asc cs ccccccccccecsccccaucuascsascsaseacsasattscscssstanstearqscseseasecasscccacecscccaceccacedsaiesasasesasecesaceaasadenteasestsasasasasessatacceacececeeseseasesesees 4 Figure 2 3 Mass spectrum obtained by the TRIDION showing the mass to charge m z of ionized fragments of FPS OI lea AU see cee aceseesesscwevesutsecea wencvacneseesescuuceeiutes etiuusetcnccrsedestusssese evieness eaten sucaucuestenycscnesstseaecsueueceiearaiweraseeveurveestnuesesreseees 5 Figure 2 4 Cut away drawing of the toroidal ion trap showing trapping of ions red dots in a toroidal geometry around tne conter CCU OCS ssa EE R seaecsasentezassatcnceeneenaeareeadia 5 Figure 2 5 Diagram of the TMS assembly with ion source filament and electron multiplier detector ou eee 6 Poue FO TRDION CC TN sE E 7 Foe 27 TOP AEON TRIDION CEN meee Te 7 Figure 3 1 Interface between the SPME syringe and the injector sesesssessseesseesseesssesss
80. ONS 9 The following image shows a TIC with three peaks two of the peaks co elute at 53 54 seconds Deconvolution has been performed and three peaks have been detected Sone 382 RT 53 3220 Sex Abun 1 026 aj 4 Ready Cz bers inathan oor te Desktop andine Some 2002404 13 sd od Figure 5 66 Deconvolution of three peaks with two co eluting peaks 10 The following image shows the results of the unknown search of the deconvolved peaks Deconvolution Control Center B l oOj x Ready Unknown 3 Known 0 Figure 5 67 Deconvolution Control Center showing the All Results tab for three peaks identified in the unknown library Unknown 2 and Unknown 3 are co eluting peaks 11 The compounds are shown with the top hits for each NIST Search 1 Launch NIST Search Clicking this button launches the NIST library search software 89 OTHER OPERATIONS 2 In each of the following graphs there is an option to send spectra to a file that can be opened in the NIST MS Search software a MS b Summed c Background d Difference e Deconvolution Spectra 3 The following image shows the dialog box that opens when right clicking in the MS graph Unzoom Unzoom All Add Peak to Library Wit Spectra to NIST Fie Figure 5 68 Right click menu on the MS graph Showing Write Spectra to NIST File 4 The following image shows the dialog box that opens when the Write Spectra to NIST File option is selected FE E
81. ROMION TH seseina ai ni EaR RSi E e DEAE eE EE E e EEEE 48 NIS Tonan savant angina wai ate eaten eae 48 CHROMION Installation and Operation cccsecceeseeeeeeeeeeseeeeeseeeees 48 CHROMION Mali Screen wcnaniusasuadimra nee 48 CERROMION Menu Bal se AA 50 FS VSIA iae a a 50 Et MENU otea R R E E E A RA 51 Preeren OS ideon onana e EANA A Aa 51 Hazard Levelei EE E S 51 MSrumeEnt Me M e a ebasen 52 Connecting to an INStFUMENT cccceeeeeccecceeeeeceeeceeeeceeccseeseceeeeseaeeeesessaaeeeess 52 Methods Men sins seairictd recta dicate a seta hdacmebundtatebuhateneneisnd 55 Memnod VI CRU ssr a N a a Aa A a 55 Creating a New Method cccccccccessseceecceeeeecececeeesececeeeaaeceeseseaseeeessaaeeeess 56 Load and Delete MelNodS eni nnen E eee 56 Mponng a Metod cesia aae aa 57 Saving a MEMO orbs a a S 58 Saving a Method as a New Method cccccccccceesseeeeeeeeeeceeeeaeaeeeeeessaeeeess 58 Rename ai IVIGTNOG sesona A moaubuascaeadotanvcssans dines a Naa 58 Exporting a Method to a File cccccccccssseeeeccceseeeeeeceeeseeeeeseeeeeeeessaaeeeeesseaass 59 Send a Method to an INStruUmMmeNt soraira 59 Gas Chromalogiap Nzsnsiase aie ee ee 61 Gas Chromatograph Buttons sche ie esscde rence Paraceccdesexacthatesecadsinensstandssdedtaweccebedeencs 61 GC Parameter Va areno ca acsavauca san tddede a E 62 Retention mme Calibrations Tab sissccvcsscessicceseciane tudrseeaisesvaiateorhevesseeaestosedenadeea
82. Results SC eei casssccics55cesecccs 5scs c022scescsescecasssceeassscoecsescacaseseseect cescactccsceetscsieecessteedsdaceetsvstoenscscacasvsracaststscasaseaiest 43 Figure 4 54 Choosing a folder from the Previous Results SCreen sss sssessseesseesseesseessseosseosseeseessersseeoseeosseoseosssesseesserssseossees 43 Figure 4 55 Choosing a data file to view previous results ssessseesseesssessseesseesseesseesssessseosseosseeoseesseroseeosseosseosseesseesseessersssrossees 44 Figure 4 56 Wait screen while instrument processes previous data ssesseessesssesseessesseesseoseesseeseesseessesseesseoseesseoseesseoseessees 44 Figure 4 57 Previous data displayed with library identification table ss sssesssesseessesseesseoseesseossesseessesseesseoseesseoseesseossessees 45 e E e a E 9 EEEE EEEE OE EEEE EEEE 45 Figure 4 59 Selecting where to export files toO s ssseesssesesesesessseesseesseesseeosseosscoseesseesseeosseosseosseosseesssesseroserosseosseosseesseessersserssseossees 46 Figure 4 60 File export Was SUC SSO sacs E 46 Figure 4 61 Screen displaying end of run data s sssesrerssesrerssesesrereossesreosueorersaesrersseorersrervursreevresrersreorersaeoveeorervarsrevuroreosresrersre sser 47 Figure 4 62 Choosing More OptiOnS ses sesesssessseesseesseesssessseosseesseessersseeoseeosscosseesseeoseesserosseosseosseesseeeseesseroserossrosseosseesseesseroseroserossees 47 Foure s TCHROMION ese I EO ss EnS a E eee eee ee 49 Figure 5 2
83. TR and the other to HTR 9 Install the RF wire screw polyimide spacer and RF tab The tab must be positioned so it is in contact with the top pin of the Center Electrode football 10 Slide the RF wire onto the pin on the RF board 11 Slide the Einsel Lens wire onto the pin on the Einsel Lens and onto the connector on the RF board Filament replacement 1 Follow the instructions in the Remove ion trap RF module section of this chapter to remove the ion trap from the vacuum chamber 2 Slide the Red and Black Filament wires off the pins on the RF board The following image shows the position of the electrical connections on the RF board RF RF Wire EGUN Filament Red Wire EGUN Filament Black Wire DET CAP No Connection FILGATE Einsel Lens Wire FILCAP Top End Cap Electrode Wire RTD Black RTD Wire RTD White RTD Wire HTR Either Heater Wire HTR Either Heater Wire Figure 8 21 Trap wire connections 3 Squeeze the tabs on the filament clip with needle nose pliers and slide the filament straight up and out of the EGUN barrel 146 SERVICE F lt Filament lt EGUN Barrel Figure 8 22 Filament removal 4 Slide the new filament assembly into the EGUN barrel Squeeze the filament clip with needle nose pliers and gently press the filament down until it snaps into place A correctly installed filament will sit level and with slight sideways pressure it will be able to rotate 5 Use the 1 8 hex nut driver to install the
84. TRIDION battery will charge when line power is connected and the instrument is not running When the instrument is running the battery will only charge during times when the overall power draw is sufficiently low to allow extra power to be diverted to the charging operation Power will not be drawn from the battery as long as the external line power is connected 112 OTHER OPERATIONS Changing the battery 1 Turn off the TRIDION or connect it to an external power supply see the next section called How to operate with external power Lift the battery straight out of the battery compartment After removing the battery insert the new battery into the battery compartment so the connector in the compartment aligns with the hole in the battery see figure 4 2 Note Push the battery into the compartment until it is stopped by the bottom of the compartment The battery should extend out of the compartment approximately one half inch Battery Connection Figure 6 2 Empty battery compartment Operating with external power 1 External power may be connected to the TRIDION at any time The sophisticated monitoring circuitry will automatically adjust the power without interrupting the instrument performance As described in the previous section the indicator light will change to indicate that the external power has been connected If a battery is present then both the line power and battery power lights will be lit The battery powe
85. Tuning Wizard Files dialog box will open The following image shows this dialog box Perfomance Validation File C Program Data Torion Technologies Peromance Validation ini Figure 5 89 Tuning Wizard Files dialog box The files are custom and can be save in any location The only requirement is that they be in the correct file and that the Performance Validation File be saved with an INI file extension and the library file be saved with a tlib file extension If a file location has been specified that location will still be specified when a new copy of CHROMION is installed To Change back to the default files select the Default button Contact Torion for more details on making and using custom INI or library files To check the performance of an instrument it is necessary to run a performance validation analysis on the instrument Instructions on running a performance validation are described in Chapter 4 After running the performance validation use the File Manger to move the Calibration Results file to the computer The calibration results are saved in the following folder on the instrument storage card Storage Card Calibration Results The performance validation results files have a zip file extension They are archived on the storage card by date It is important to make sure that the most recent file is the one moved to the computer Load the file into the Tuning Wizard by clicking the Find button in the Calibration Fil
86. VB PDMS Extraction Abundance 6 9 80000 7 13 70000 11 a2 60000 50000 10 40000 4 30000 5 20000 2 10000 il 0 20 0 40 0 60 0 80 1 00 1 20 1 40 Figure 7 4 Chromatogram of the CALION Performance Validation mix iii The CALION mix contains the following 13 compounds The order of the list matches the elution order shown in the above chromatogram K o C 5 Methylcyclohexane 6 Toluene d8 m Trea aTe SO 123 LIBRARIES iz Steps a Set GC Settings i Set column temperature settings in CHROMION Settings GC as follows Column Begin Temperature C 50 Column Final Temperature C 270 Column Ramp Rate C sec 2 0 Column Begin Temp Hold Time sec 10 Column Final Temp Hold Time sec 20 b The instrument must be in uncalibrated mode i Uncalibrated data shows the bins of data used to create mass spectra The TRIDION electronics stores the data from an analysis in 4096 discrete locations or bins The mass range of the instrument is 500 amu The number of bins per mass is obtained by dividing the number of bins by the mass range of the instrument So there are about 8 bins per 1 amu In order for the instrument to display correct mass information it is necessary to calibrate which bin corresponds to which mass The difference from instrument to instrument is usually only a few bins but this can be enough to shift the mass assignment and result in poor peak identification ii The
87. age shows how to do this Figure 8 3 Wet lint free tissue with cleaning solvent A Clean o ring groove with wet tissue B 4 Clean mating surface to the o ring with lint free tissue and cleaning solvent The best way to do this is to wet the tissue with the solvent and wipe the o ring mating surface The following image shows how to do this Caution When handling all components e g ion trap module do not touch areas of the components in locations that reside directly in the high vacuum chamber when assembled Figure 8 4 Cleaning o ring mating surface 136 SERVICE 5 Use dust off to remove any particles from the groove and surface The following image shows how to do this Figure 8 5 Dust off o ring groove 6 Inspect groove and surface for attached particle and dirt If there are any particles or dirt attached to the o ring groove or mating surface clean again steps 1 3 7 Inspect o ring carefully to make sure that there are no cracks dimples cuts abrasions embedded particles or excessive flash The following image shows how to do this It is recommended to start with a new o ring as opposed to re cleaning a previously used o ring Figure 8 6 Inspecting o ring for defects For round cross section o rings make sure there are not any flat or obround sections For square or quad cross sectioned o rings make sure they have a consistent thickness in both directions 8 Clean o ring with lint free tissue and cle
88. aining Percent of Charge left in Battery Cell B Remaining Time Left For Battery Cell A Remaining Time Left For Battery Cell B Battery Cell A Temperature Battery Cell B Temperature Voltage Coming In From Wall Power Current Being Drawn By Roughing Pump Transfer Line Temperature lon Trap Assembly Temperature Turbo Pump Bearings Temperature Turbo Pump Temperature at Bottom of Housing loj x Detector High Voltage Voltage Hement0 Path Hement1 Path Injector Temperature lon Source Filament Bias Voltage lon Source FilamentCurent lon Source FilamentGate HighVoltage lon Source FilamentGate Low Voltage lon Source Filament Voltage MassAnalyzer Amplitude Voltage MassAnalzer DriveCurment MassAnalyzer Drive Temperature Mass Analyzer Drive Voltage Figure 5 86 Real Time Plots Data Logger Items dialog box 105 OTHER OPERATIONS h Select the item to be plotted from the Available side of the dialog box and click the top blue arrow to move the selected item to the Current side of the dialog box i Items can be removed from the Current side of the dialog box by selecting them with the mouse and using the second arrow button to move the selected item back to the Available side of the dialog box j All of the items in the Current side of the dialog box can be moved back to the Available side of the dialog box by clicking on the bottom blue arrow Note Selecting items to plot that have large differences in value
89. am 1 Copy lons from RIC to TIC If RIC ions have been added to the RIC table then clicking this button will toggle to show the RIC ions in the TIC graph or not show the RIC ions in the TIC graph The following image shows the Copy lons from RIC to TIC turned on It also shows the color coding of the selected ions in the MS graph Scan 207 RT 32 2090 Sec Abun 44 229 Ready T T 9 Vasbdation 1G36 8D Card G35 Pats OOF 900000595 ccif Figure 5 52 Copy lons from RIC to TIC showing masses 98 99 and 100 2 Selecting the RIC lons button from the Edit menu opens the following window 80 OTHER OPERATIONS FR RIC Masses Figure 5 53 RIC Masses table 3 In this window the user can select the masses that will be shown in the RIC chart of the software The masses are entered in by typing the mass into the blank field They can be entered in three ways a They can be entered as an individual mass for example mass 105 would display a single trace of the intensity of mass 105 in the RIC graph chart b They can be entered in as a range of masses for example 91 93 would display a single RIC trace of the sum of the intensities of ions 91 92 and 93 c They can be entered in as a group of masses for example 91 93 105 would display a single RIC trace of the sum of the intensities of ions 91 92 93 and 105 4 To view the RIC chart first open the View menu from the top menu bar and select Charts Ensure that the box next to RI
90. ame time as that set in the lonSource HardSolventDelay Next find the Subgroup Detector HardSolventDelay is the second item in this Subgroup set this time to the same value as the other two times b Detector Voltage The detector is an electron multiplier These detectors degrade over time To maintain the performance of the instrument it is necessary to change the voltage on the detector For inexperienced users it is suggested that the changes be made using the Tuning Wizard in the software The setting can be changed by entering the desired value in the MassSpectrometer Group Detector Subgroup and the HighVoltageVoltage field Normal operating range is 1200 to 2200 Inappropriate values will result in poor performance of the instrument c Filament Current The filament is used to create electrons The electrons are used to ionize the analytes The filament degrades over time To maintain the performance of the instrument it is necessary to change the current on the filament For inexperienced users it is suggested that the changes be made using the Tuning Wizard in the software The setting can be changed by entering the desired value in the MassSpectrometer Group lonSource 94 OTHER OPERATIONS Subgroup and the FilamentCurrent field Normal operating range is 0 85 to 1 2 Inappropriate values will result in poor performance of the instrument File Manager 1 The File Manager is similar to Windows file management It is intended as a safe
91. and Retention Maximum set the window for the compound identification The Hazard Level is a self configured value The information displayed in the Hazard Level column can be configured by selecting the Edit menu at the top of the screen and selecting the Hazard Level option Information about entering information into a Hazard Level table is given in the menu section under Edit Hazard Level To select a Hazard Level Click the drop down arrow and select the desired Hazard Level from the list Since this data is created by the user it can be setup to display any information desired For example it can be used simply as present or not present option for applications where the chemicals being analyzed are not considered hazardous Deconvolution Parameters Tab Target List Search l There only a few items in the Deconvolution Parameters that should be adjusted The following image shows the Deconvolution Parameters screen 66 OTHER OPERATIONS Target List Search Unknown Identification IV Search for known compounds IV Match unknown compounds V Search for unknown compounds Maximum top spectral hits to show 3B Maximum unknown compounds jo Shared percent coefficient 2 e V Noise remove on Dot product coefficient 0 75 Steps jo Minimum unknown compound correlation 65 Auto delta x i Path 1 CALibrary Files AMDISNISTEF Find Cutoff weight 3 OO Cutoff threshold ho Shot window i Path 2 Find Shot thresho
92. aning solvent The best way to do this is to wet the tissue with the solvent and wipe the o ring The following image shows how to do this 137 CAUTION SERVICE Figure 8 7 solvent Cleaning the o ring with solvent wetted lint free tissue 9 After solvent cleaning the o ring use dust off to remove any remaining particles and inspect o ring to ensure that it is clean refer to the figure in step 6 The following figure shows how to use the dust off to clean the o ring Figure 8 8 Using dust off to remove dust particles from an o ring If the o ring is not clean repeat the cleaning process steps 7 and 8 Caution Do not lay the o ring down on a surface that is not clean and dust free If you need to put the o ring down it is recommended that you lay it on a clean lint free tissue See the following figure 138 SERVICE Figure 8 9 Storing a clean o ring in a dust free environment 10 Carefully lay the o ring into the o ring groove The following image shows how to do this a gt _ D l 4 4 Se a oe i i T N AEN Figure 8 10 Placing o ring into vacuum chamber groove Be careful to not roll the o ring into the groove It is important the tool parting lines on the o ring are facing the groove sides O rings tolerances are designed so that they may possibly have a slight interference with the inside edge of the o ring groove so you may need to gently stretch the o ring a very small amount
93. aph open with the TIC The spectrum that is shown is for the scan where the cursor is positioned in the TIC graph 74 OTHER OPERATIONS Scan 246 RT 37 0320 Sec Abun 76 945 Figure 5 41TIC and MS graphs c RIC Reconstructed lon Chromatogram This is the chromatographic trace for selected masses and can be used to look for a specific peak with a given mass or group of masses The following Image shows a RIC graph with a TIC and MS graph open Scan 356 RT 44 7650 Sec Abun 49 535 AjInten 0 00 S Int 50000 40000 30000 Q 20000 10000 0 aml Powel e a A r iaren e eat n aae foment Geng aa reece eas a R Seger A Won Soma aa arail a a fuer EN oor A al a Rawal A A E a a A moa eaat aa el lowed fone foment aa Immo a eaa aN aaan raa anA E Eaa e heal e aaor as Saal aas pany 10 20 30 40 50 60 70 80 90 100 110 120 173 20000 W 10000 1 66 136 160 189 331 373 433 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 50 100 150 200 250 300 350 400 450 Ready C Documents and Settings shirlene schofield Desktop Files CDF O0000535S cdf Figure 5 42 RIC graph with TIC graph and MS graphs d Summed This is the spectra of a group of chromatographic scans that have been selected using the Summed function Choosing this function totals the response of all of the ions in the region that has been selected The following image shows a selected area in the TIC for summing
94. ary Contents Compound Details Library Mame Modfied Dare AMDISHISTEPACW araram OAM O O SOO O Search Crmpoumis LCE N Filler Tim Ha E Library Googe A Baruri bjehu CANES 75 15 H __ Benzofqhilperyiene 191 242 Beruro j Marcie bere 7 207 08 9 271 896 496 162 CFO 5 25 0 COHLOOR PL I Ol a como ICER CBHBOZ 118 90 1 emmo sas conio Tons 04 5 camooz soes __catteciz03 191 009 Figure 5 77 Library Editor Library Contents tab 3 The software comes with a library loaded This library is an edited version the NIST Amdis EPA library This library consists of data that are generated on quadrupole mass spectrometers The unknown search algorithms in most cases work well to match the data from the ion trap to NIST libraries Caution The difference between Target Lists and libraries is primarily where the data came from While it is possible to add compounds from any library to the Target List it is important to note that some library data were generated on instruments that may give slightly different spectra than the TRIDION instrument This is because different types of mass spectrometers work in different ways It is usually best to generate Target Lists on the instrument using standards Second best is to use compounds from libraries that have been generated using a TRIDION GC MS instrument Using other libraries to create Target
95. atile chemicals are more likely to leave the solution as vapor at higher temperatures What is the CUSTODION SPME syringe 1 The SPME syringe designed for the TRIDION is called the CUSTODION The CUSTODION triggers the injection and analysis to start on the TRIDION without having to push a start analysis button 2 The SPME syringe consists primarily of a barrel plunger spring protective needle and fiber lt _ Plunger Protective needle Retractable fiber gt Figure 2 1Diagram of the CUSTODION sampling syringe What is low thermal mass LTM gas chromatography GC 1 In microcolumn gas chromatography GC volatile chemicals separate as they travel through a capillary column Separation is dependent upon the equilibrium distribution of each chemical between a liquid coating on the capillary wall and the carrier gas flowing through the capillary An equilibrium constant called the partition coefficient K governs the separation of chemicals and is a ratio of the concentration of the target chemical in the stationary phase coating versus the mobile phase carrier gas The affinity of a chemical for the stationary phase is a function of temperature and determines the chemical s partitioning between the two phases K concentrat ion in stationary phase mass in stationary phase volume in mobile phase concentrat ion in mobile phase mass in mobile phase volume in stationary phase 2 The partition coefficient
96. aximum temperature is 270 C 3 The Split Injection section is used for controlling the GC inlet s split injection controls Normal operation is to run with the split values open To introduce more sample into the GC column the valves should both be closed for 1 to 2 seconds To do this the user would set the Split On time to 2 seconds telling the instrument to turn the split on at 2 seconds this will keep the valve closed after the sample is injected for 2 seconds then it will open to sweep the injector Turning the split on for longer times will have a detrimental effect on the peak shape of early eluting peaks Later eluting peaks will refocus at the head of the column so they will not be as adversely affected a The 10 1 Split On opens the lower flow split valve at the time the user defines Normal setting is to turn on the split at time 0 b The 10 1 Split Off closes the lower flow split valve at the time the user defines Normal setting is to turn off the split at 10 seconds c The 50 1 Split On opens the higher flow split valve at the time the user defines Normal setting is to turn off the split at 10 seconds d The 50 1 Split Off closes the higher flow split valve at the time the user defines Normal is to turnoff the split at 30 seconds 62 OTHER OPERATIONS Retention Time Calibrations tab 1 The Retention Time Calibration tab is used to set up the instrument to determine retention index values Using retention in
97. cecescecacescecascscscacescacace scucacescucsceccscacesescseesescaeesezcaeesezcecasesceeacescocasescotast 82 Figure 5 56 Data File Overlay Setup table cscs scscocecescoscccicenscesttecstscovesisceitccuconssextencessesssetsesnbencdtucntitbibes assent evcoseseeconesencoteesncorcaencoltc 82 Figure 5 57 File window used to select multiple data files for display in the Overlay Graph sesss ssesssesseessesseessesseessess 83 Figure 5 58 CHROMION overlay view WINCGOW cscscsssssssscscscsssssssesscscsssssssesscscsssssesesececsesesesesecscscsssescsececucsesesesececscnsaeseseseencacacars 84 Figure 5 59 Deconvolution Control Center RUN Tab uu csssssssssssecscsssessssesscssessssssssscscsssssssesessensasacsecesscssassssesesscnsasacsesesscasasees 85 Figure 5 60 TIC with color coded peaks and spectra after a deconvolution ssesssesseessesseessesseesseessesseessesseesseoseesseossessees 85 Figure 5 61 Deconvolution Control Center with bromoform Selected essssscecsssscecsssssscscsssecessssscsesssesscsssssesssseesessseeeeees 86 Figure 5 62 Deconvolved data with an UNKNOWN Peak highlighted se ssesssessessessessesseoseoseeseeneeseessessessesseoseoseoseoseoseeseeseess 86 Figure 5 63 Deconvolution Control Center with Unknown peak 2 selected in the TIC s ssssssesssessessesseessesssesseossessees 87 Figure 5 64 Deconvolution Control Center All Results tab showing unknown 2 identified as tetrachloroethylene88 Figure 5 65 Deconvolution Control Cent
98. compound is entered here In the above example the 174 mass found in bromoform has been entered b Index Expected Minimum In the above example this is the lowest index bin number that the user would expect the 174 mass to elute c Index Expected Maximum In the above example this value is the highest index bin number that the user would expect the 174 mass to elute d Peak Number To improve the accuracy of the calibration the user can specify a peak number For example bromoform has a group of masses at 170 172 and 174 Since the last peak in a group is less susceptible to trap overloading effects we would choose to use mass 174 for calibration In this case mass 174 is peak number 3 of the group so we would enter a value of 3 for the peak number e Total Peak Count Total peak count specifies the number of mass peaks expected in a group of peaks In the case of bromoform there are three peaks to the Total Peak Count would be 3 f Mass Calibration Placing a check box in this column sets the auto calibration routine to use the specified mass Leaving the box unchecked allows the user to leave the information in the table but not use it for the calibration 11 Above the Mass for lt compound name gt table are two buttons 12 The first button is used to add masses to the table To add calibration masses highlight a position in the table and click the Add calibration Mass button A new line will appear at the bottom of the table T
99. ctor at the end of the continuous dynode that produces a measurable voltage that is proportional to the number of ions of each type i e m z value isolated by the mass analyzer TUTORIAL 6 A variety of mass analyzers are available for laboratories however few are available as portable instruments due to overall size and power requirements The latest advancement in miniaturization of mass spectrometers is the miniaturized TMS see figure 2 4 and 2 5 The miniaturized TMS requires less power and operates under higher pressures than quadrupole mass spectrometers Furthermore the miniaturized TMS combines many advantages of larger non toroidal ion traps such as simplicity pressure tolerance and comparable ion storage volume The miniature TMS operates at less than 2 5 kV compared to 15 kV for the larger alternative portable ion trap Electron Multiplier Outer Ring Detector Electrode lon Storage Region ee u bel a i Trap Heater Filament Gate Filament NS Inner Ring Electrode iaia End Caps Figure 2 5 Diagram of the TMS assembly with ion source filament and electron multiplier detector What is the TRIDION The TRIDION Figure 2 6 is an easy to use hand portable GC TMS system The primary purpose of the TRIDION is to allow rapid chemical analysis and detection on site so that informed decisions based on chemical analysis can be made as quickly as possible The combination of
100. d ccccccceceeceeeeeeseeeeeeeeeees 122 TRIDION Manual Mass Calibration ccccccecccsseeeeeeteeeteneeaeeneeetans 122 TRIDION Auto Calibration Performance Validation c 00c0 129 Confirm auto calibration Performance Validation cccccsseeeeeeeeseeeeeees 130 Correcting failed auto calibration Performance Validation cc ece 130 DIC ennon in orian i TETE EAE ATO 134 Trap service tools and materials ccccccsecceseeeeeeeeeeeeeeeeeeeeeeesaeeeeas 134 O ring Handling Cleaning Installation and Removal 08 134 REMOVING OTINI S eaa 135 ASANG OTN aaea r e 136 Remove the ion trap RF module ccccccccseeeceeeeceseeceeeeeeeeeeseeenees 140 Trap maintenance procedures cccccseccceeeceeeeeeeeeeeeeeseeeesaeeeeaeeeeas 141 TFA CISASSEMDIY wiassiauscteriaieiahoearasdctrelev a a asa naataieeetecatoains 141 Trap cleaning PKOCCC UN Crea ceca ace nae arabia cance ca A 142 TAP TEASSEMDIY A 143 Mount the trap assembly onto the RF DOaId ccccceeceeeeeeeeeeeeeeeeeeeeneeees 145 Trap TINA FOASSCIMDIN aes iecashciieonst anlecaan wns A tune tleuintaterasethins 145 FIAMENEFEDIACEMON sieveisvesssesziesewwereereverieavies einen eee 146 INSEL ICMS MAMI ACS ito sctot tacit tate atnl ate tnl el aietat ataretat ot aretnt st aseeat ats 147 Einsel lens cleaning procedure xicnctce ccdes eeaecotsh csetielencdda ceeenebhvartatchceeeelees 147 Einsel lens
101. d fH GTK H P mix 4 1386 4 gt tmpea2 txt H IntelPRO Methods gt Library notUsed Results H LoadedMethods Scripts fH Maggie Settings f maggiescripts Temp H Methods Tools fH MSOCache UnknownLibraries FS msvsait FileName Sze Type Date Modified Tin Date Modifi 000000005 cdf 218 031 KB CD 9 22 2011 53 P mix8 met 211 829 KB MET file 13 33 02 06 12 000000025 cdF 211 938 KB CD 9 22 2011 5 default met 209 395 KB MET File 09 22 02 15 12 000000035 cdf 185 141 KB CD 9 22 2011 5 default_1 met 34 948 KB MET file 10 50 02 08 12 000000045 cdf 186 820 KB CD 9 22 2011 5 default_17 met 207 583 KB MET file 15 40 02 09 12 000000055 cdf 192 137 KB CD 9 22 2011 5 PY mix met 211 824 KB MET File 11 34 02 17 12 AUTOEXEC BAT 0 Bytes BA 12 14 2010 Br autoimp msd 15 Bytes MS 10 3 2011 1 boot ini 211 Bytes INI 9 7 2011 gi COMFIG SYS 0 Bytes SY 12 14 2010 Bie filespec Fil 13 Bytes FIL 10 3 2011 1s 10 S S 0 Bytes SY 12 14 2010 Bie library 15005 mat 5 370 MB MA 8 8 2011 Fie library 1S005MW mat 7 087 MB MA 9 7 2011 4 libsrchparms txt 1 049 KB TX 9 14 2011 10 MPUsbSIn log 2 885 KB LO 10 4 2011 11 MSDOS SYS 0 Bytes SY 12 14 2010 Bie NTDETECT COM 46 449 KB CO 8 4 2004 4 0 ntldr 244 188 KB file 12 14 2010 11 pagefile sys 2046 000 MB SY 2 16 2012 Bie preferences xml 1 185 KB xM 12 20 2011 11 sibe 1e NE opao Siu Figure 5 75 File Manager 4
102. dex times makes it easier to transfer methods between instruments In addition using retention indexes allows the user to modify the GC method without losing peak identification information The target list uses retention times to narrow the library search If the gas chromatographic method is changed then the retention times will also change The change in retention times will invalidate the target list since the compounds will have retention times that are different than that setup in the target list Retention indexes were developed to make it possible to compare data from a variety of instruments using similar columns but different oven programs One of the most common indexes is the Kovats index All straight chain hydrocarbon molecules are assigned an index value of 100 per carbon So a molecule like heptane with 7 carbons would have a Kovats value of 700 And a molecule like tetradecane with 14 carbons would have an index value of 1400 The retention time calibration uses the following compounds that are included in the CALION standard vial Compound Methylene Chloride Toluene d8 759 853 1400 If retention indexes are used in the target list then simply calibrating the retention time allows the same target list to work on another instrument or with different gas chromatography ramp rates or hold times The user does need to adjust the retention time windows used in the performance validation to reflect the new times that result from
103. e PS Si as Xt O Peak successfully written to MIST Figure 5 70 Peak successfully written to NIST file dialog box 11 Clicking the Launch NIST Search button will open the NIST MS Search software and allow the user to compare the saved spectra to the NIST data base Exporting Charts 1 Export Charts This opens the following dialog box gt A r u 5 x Pi blk boo Export filetype Windows Metafile WMF C JPG Bitmap BMP Comma Delimited CSV Figure 5 71 Export Charts dialog box active charts are not grayed out Inactive charts are grayed out and not available to create images 91 OTHER OPERATIONS 12 To create an image place a check mark in the boxes by the type of chart you want The following is a list of the different types of charts More detail on how to get these charts and what they are used for will be given latter in this section of the manual a TIC Total lon Chromatogram This is the GC trace of the entire signal that is generated by the detector in the mass spectrometer b MS Mass Spectra This is the spectra for a single scan in the TIC c RIC Reconstructed lon Chromatogram This is the chromatographic trace for selected masses and can be used to look for a specific peak with a given mass d Summed lon This is the spectra of a group of chromatographic scans that have been selected using the average function e Back
104. e 4 60 File export was successful 9 The Export Files function can also be accessed from the screen displaying end of run data shown in the following figure 46 INSTRUMENT OPERATION Target4E Torion 20sample04 2012 04 1 4 Sample iL 5 13 5 Methylene Chloride 15 5 Diethylamine 1 7 Allyl Alcohol Figure 4 61 Screen displaying end of run data 10 From this final identification screen choose More Options and the following screen will be displayed Target4E Torion 20sample04 2012 04 2 4 Sample 13 8 Methylene Chloride 14 3 Unknown 10 1a 8 Unknown 3 More Figure 4 62 Choosing More Options 11 Currently the Details option has not been activated 12 Choosing the Export to USB button will display the Export files screen as shown above This functions exactly the same as discussed in the steps above 47 OTHER OPERATIONS 5 Software This chapter describes how to installand use the various software programs thatare induded with the instrument Software programs The TRIDION is supplied with several software programs The following is a list of the various programs and a brief description of what they are used for CHROMION The CHROMION software is used for instrument control library management library known compound identification interface multiple instrument control deconvolution unknown identification and creation of methods for use on the instrument The CHROM
105. e PC and then use CHROMION Data Review to open the file The file will look different because it is collected with unusual system settings and contains uncalibrated data The system needs to run this way in order to create a calibration file correctly 10 In the following image the cursor has been placed on the methyl salicylate peak 11 12 13 14 Scan 498 RT 74 2870 Sec Abun 69 632 Figure 7 124 Performance Validation correction showing methyl salicylate peak with binned centroided but uncalibrated data Just below the button row in the upper left corner of the screen there is a numerical listing of the cursor position This includes the scan number retention time and abundance for the selected scan The retention time RT 74 287 rounds to 74 3 seconds The table shows the retention time window as low 65 high 80 and ideal 74 So the actual peak falls within the specified retention time window and would not cause the calibration to fail Place the cursor on each peak and verify that the retention time is within the defined retention time window for the peak The following image shows the cursor placed on the bromopentafluorobenzene peak 132 LIBRARIES 19 Scan 275 RT 45 8710 Sec Abun 99 861 Figure 7 135 Performance Validation correction showing bromopentafluorobenzene BPFB peak with binned centroided but uncalibrated data According to the Performance Validation table the BPF
106. e frame located at the top left of the Tuning Wizard screen The Windows open file dialog box will open Navigate to the location of the calibration file and click on it to select it then click open to load the file into the Tuning Wizard Click the Run Test button to check the performance of the instrument 107 OTHER OPERATIONS 12 The results are displayed in an easy to read format The detailed report shows more information about the tests and the results Some of the tests shown in the detailed report are grouped into the results on the main screen 13 If a test fails then the field to the right of the test name will say failed and the suggestions field will give information about how to solve the problem 14 The following screen shot shows a test where all of the tests have succeeded Calibration File C Library Files Performance Validation autocal2012 04 11 13 39 Rnd 44 zip Perform Test 4 19 2012 1 43 42 Perform Test 4 19 2012 1 48 11 Figure 5 90 Tuning Wizard showing a system that has passed all tests 108 OTHER OPERATIONS 15 The following is a list of the tests and what they are testing Screen Results Detailed Results Message Asymmetry Asymmetry Check Sample Amount Retention Time Retention Time Check Septum and or GC Settings or Check GC Method and or Splits Sensitivity Toluene d8 SNR TEST No Message Sensitivity TIC ABSOLUTE INTENSITY TESTS Reduce Fila
107. e solution remain constant The amount of a chemical extracted by the fiber is proportional to the concentration of the sample before and after equilibrium 3 Sensitivity to a target chemical extracted by SPME can be improved significantly in three ways increasing the sorbent thickness on the sampling fiber employing a more selective sorbent or changing the extraction temperature A thicker sorbent layer absorbs more target chemical increasing the sensitivity to all absorbed chemicals however thicker sorbent also increases the equilibration time between the absorbed chemical and the chemical in solution Rather than thicker sorbent longer fibers may be used to increase sensitivity however longer fibers may not be used on the TRIDION the instrument is not designed to accept them and they may break inside the injection port Sorbents with greater selectivity to the target chemicals will improve sensitivity however they may also increase the extraction of unwanted chemicals Finally changing the extraction temperature will affect the sensitivity of a target chemical The sensitivity for high mass and high boiling chemicals will generally improve with increased temperature particularly for headspace gas extractions Increasing the temperature will also decrease the equilibration time High temperature TUTORIAL extractions of volatile chemicals in solution may decrease the sensitivity to those chemicals when sampling by immersion because vol
108. e user can also return to the Overlay Files selection window to turn on and off the overlaying function Deconvolution 1 Launch Deconvolution Control Window Clicking this button launches the Deconvolution Control Center This window is used to display and interact with data that have been deconvolved 2 The following image shows the Deconvolution Control Center 84 OTHER OPERATIONS Deconvolution Control Center Ioj x Run All Resuts E ee Figure 5 59 Deconvolution Control Center Run Tab 3 The Deconvolution Control Center uses the settings from the Target List and Target List Deconvolution Parameters to extract the spectra for a specified peak 4 To extract the spectra press the run button at the bottom of the control window 5 The following shows the TIC window after the spectra have been extracted Scan 310 RT 44 7310 Sec Abun 154 498 Ready T T 9 Validation 636 SD Card G36 Data CDF 000000545 cdf Figure 5 60 TIC with color coded peaks and spectra after a deconvolution 6 The image above shows the cursor positioned on bromoform The peak outline is highlighted and the colored spectra are visible in the deconvolution Decon graph 85 OTHER OPERATIONS Deconvolution Control Center Figure 5 61 Deconvolution Control Center with bromoform selected 1 Ifa peak is in the Target List it will be identified and the when the cursor is place on the peak in the TIC graph the name of the
109. eal lt Injection Port Figure 8 26 Exploded view GC injection port assembly Accessing the GC injection port 1 The following steps are required before doing any maintenance on the GC injection port 2 Unscrew the plastic cover from the Universal Interface 3 Using the Ring Removal tool remove the stainless steel Interfacing Mounting Ring Nut 4 Pull the Universal Interface out of the top of the TRIDION 5 After removal of the Universal Interface the GC injection port is accessible Septum replacement 1 Make sure the instrument is cool 2 Remove the Septum Nut from the top of the GC injection port by unscrewing the nut 3 Remove the old Septum 4 Install the new Septum 5 Replace the Septum Nut Make sure the nut is tight Injection liner and seal cleaning or replacement 1 2 The injection port must be warm to replace the Injection Liner and or Seal Before heating the injection port remove the Septum Nut 151 SERVICE It is preferable to load a custom method that heats only the Injection Port The method should have all of the other temperatures set to off and the Injection Port set to 50 C Allow the temperature to reach 50 C After the Injection Port has reached 50 C grasp the Injection Liner and pull it out of the Injection Port Remove the Liner Seal from the bottom of the Liner Replace the Liner and Seal with the new Liner and or Seal Remove the Septum from the old Liner and insert it into t
110. ectrometer screen F Open Mass Spec Settings 2 Save Current Mass Spec Settings E d l Save Current Mass Spec Settings As F ols Delete Current Mass Spec Settings n A Send Mass Spec Settings to Instrument Figure 5 72 Mass Spectrometer screen button bar a Open Mass Spec Settings This allows the user to load previously saved settings into the Mass Spectrometer table It is also used to update the displayed data The following image shows the dialog box that opens when opening mass spec settings Open Mass Spec Settings 0 x Source From instrument C From database Test 1 Figure 5 73 Open Mass Spec Settings dialog box When the From instrument option is selected the table will be updated from the currently connected instrument The From database option allows the user to select saved settings to load into the table b Save Current Mass Spec Settings This option allows the user to save the currently displayed settings to the current settings database entry This option is only available when 93 OTHER OPERATIONS a settings table has previously been saved The name of the saved table is displayed in the blue bar at the top of the Mass Spectrometer screen just below the button bar C Save Current Mass Spec Settings As This button is used to save the settings and provide the database entry with a name If the settings table has been saved previously this but
111. een 6 This screen shows actual values from the mass spectrometer These values are used by service personnel to diagnose potential problems with the instrument 7 Selecting the Status tab displays the following screen Target4E Torion Technologies activated2012 04 16 13 35 40 1 SystemBlank Jet Battery B Calibration Values Battery Voltage Internal Temp Wireless Total Runs Trap Runs Figure 4 38 Status tab of the Status Diagnostics screen 8 This screen shows the percent of Battery life remaining Internal Temperature of the system Wireless status Total Runs and the number of Trap Runs on the instrument since the trap was last cleaned 9 The following image shows the Edit tab screen 34 INSTRUMENT OPERATION Target4E Torion Te activated2012 04 16 13 35 40 1 SystemBlank Filament Current Detector Voltage Ion Target Baseline Value Exit Software Baseline Chunk Figure 4 39 Edit tab of the Status Diagnostics screen 10 On this screen the user can manually set the Filament Current Detector Voltage and the lon Target by touching the desired field with the stylus In future releases other parameters that deal with the GC will also be editable from this screen 11 To edit any of the parameters touch the box containing the setting and the following screen will appear where the users will have to enter a password Tarqet4E Torion Technologii activated2012 04 16 13 35
112. een at the location where the cursor should be placed 29 INSTRUMENT OPERATION 16 The following image shows the screen that is displayed while using the zoom function in the spectra plot va Torion 42723 2 341785 6 25633 9 Plot View Figure 4 30 Screen showing the zoom function in the spectra window 17 The following image shows the screen that is displayed after using the zoom function in the spectra plot Ve Torion 42723 2 341765 6 25633 9 170689 3 8544 6 fo 0 0 30 3 34 6 14142 9 11514 3 8885 7 6257 1 a 3626 6 E 1000 0 Plot View Figure 4 31 Screen showing the zoomed in section of the spectra window 18 The following image shows the screen that is displayed when zooming out in TIC plot 30 INSTRUMENT OPERATION fox I Torion Te z 2 37714 3 30171 4 226268 6 150585 7 7542 9 38 5 42 0 45 5 49 0 52 4 Zoom Normal 2Rom Out Figure 4 32 Screen showing the zoom out function 19 To zoom out in either the TIC plot or the spectra plot select the bottom axis area of the plot with the stylus The box will open with the option to Zoom Normal or Zoom Out 20 Zoom Normal restores the full view of the TIC plot or the spectra plot depending on which plot axis was selected 21 Zoom Out returns to the view to the last zoom selection If the user has zoomed in twice the view returns to the first Zoomed in view 22 Selecting the Home button returns the screen
113. eesscossesseosseoseeseoseeeseoseesseossesseosseoseesseoseesseossesseess 145 Figure 8 20 EGUN mount orientation s ssessessessessesssessessessessessesseoseoseoseoseossessessessessesseesesseoseoseoseoseeseeseessessessteseoseeseoseoseoseoseosseseess 145 CUS A Ea e AAAA E 146 Figure 8 22 Filament KENMOV al ssicssascsseessdtacaseseseatasasavosessaratasavesonsarasaravesonsouasaravesonsaiaiaiavesensotaranavesousotanasavesnasotanasareenueotananaveenueataid lidiadase 147 Figure 8 23 Einsel lens exploded view s ssssssesssessessesseessesssesseossesseossesscesseoseesseossesssossesseosseoscesseoseestoseesseoseesseosseoseesstoseesseoseesseess 148 Figure 8 24 Electron multiplier replacement diagram cssssssssssscssssssssssssesssesssesesesesesssesscscsescscscsecscscscscscscscecasasesssasasscesseees 149 Figure 8 25 Electron multiplier detector mount to detector board s sssesssesesessseessersssessseosseosseesseessersserosseosreosseesseessersss 150 Figure 8 26 Exploded view GC injection port assembly csssssesesecscsssssssesecscscsssssssecscscsssesesecseseassssesecsesesssssesecseseassesesessescers 151 163 INDEX Index RES 85 115 116 146 147 148 187 191 Advanced 143 176 177 179 192 223 227 231 advanced buiton 52 176 Advanced screen 61 Attach 172 173 auto calibration 193 195 Auto Calibration 192 Auto Generated Calibration Data 103 Background 142 bake out 174 226 229 batteries 1 223 bat
114. em List Clear Chart Figure 5 85 Enable Data Logger dialog box f Following list shows the various values that can be plotted To select the items to plot right click on the Data Logger screen and select the Edit Data Logger Item List option from the popup menu or click the Edit Data Logger Items button on the button bar 103 OTHER OPERATIONS Column Temperature Column Temperature Detector HighVoltageCurrent Electron Multiplier Detector Current Detector HighVoltageVoltage Electron Multiplier Detector Voltage Helium HighPressure Internal Helium Cylinder Pressure Helium VSOPressure Pressure at the Head of the Column Injector Temperature Injector Temperature lonSource FilamentBiasVoltage Filament Barrel Bias Voltage lonSource FilamentCurrent Filament Current lonSource FilamentGateHighVoltage Einsel Lens High Voltage lonSource FilamentGateLowVoltage Einsel Lens Low Voltage lonSource FilamentVoltage Filament Voltage MassAnalyzer AmplitudeVoltage RF Amplitude Voltage MassAnalyzer DriveCurrent RF Drive Current MassAnalyzer DriveTemperature RF Drive Temperature MassAnalyzer DriveVoltage RF Drive Voltage MassAnalyzer StepAVoltage RF Step A Voltage MassAnalyzer StepBVoltage RF Step B Voltage PowerSystem AverageCurrentA Average Current Battery Cell A PowerSystem AverageCurrentB Average Current Battery Cell B PowerSystem AverageRemainTimeA Average Remaining Time Battery Cell A PowerSystem AverageRemainTimeB Average Remaining Time Battery Cell
115. end the fiber into the sample and start the timer Carefully swirl agitate the liquid sample in the vial around the SPME fiber to increase contact of the fiber coating with as much of the total sample volume as possible making certain that the fiber coating is always covered with the liquid sample Caution Make certain that there is enough liquid in the sample vial to completely cover the SPME fiber coating when it is extended into the sample and the sample is agitated CAUTION 6 After the desired extraction time depress the CUSTODION plunger to retract the fiber into the syringe needle 7 Remove the CUSTODION syringe needle from the sample vial Caution Be certain that the SPME fiber is completely retracted before pulling the CUSTODION syringe CAUTION needle out through the sample septum 8 Prior to injection on the TRIDION extend the SPME fiber out of the CUSTODION syringe needle and shake off residual sample droplets that may have been taken up in the syringe needle during sampling Sample solids 1 Always perform vapor headspace analysis of a solid sample as described above before attempting other sampling methods 2 Dissolve or suspend a small amount of the solid sample in the appropriate solvent and follow steps 2 8 as described above for sampling liquids Sample unknown liquids and solids 1 The following two pages provide sequential procedures for trouble shooting liquid and solid unknowns that are too
116. eosseesseessersseeoseeosseosseesssessersserosseossees 13 Figure 3 2 Cutaway diagram of CUSTODION syringe inserted into the injector port with fiber retracted 13 Figure 4 1 screen showing the Windows CE launch winNndOW ssessssssesssesseessesseessesssesseoseesseossesseosseoseeseoseesseoseesseossesseossessees 14 Figure 4 2 Initialization of the iNsStruMeNte ccscssecssessecscessecscessecscossssscassesscassesscassesscassssecasossecasasseessassecscasseeseasseescasseeseasscescans 15 Figure 4 3 instrument Par ee en rrr ee 15 Figure 4 4 Status bar displayed at the top of the SCre n csssssssecssscsssssssssscscscsssssecsccsesssssssecscssassesesecsesesesssesecseseasseseseeseneees 16 Figure 4 5 Instrument status SHOWN in expanded VICW csssssecscecscsssssesesecscsssssescsscsctssssesesecscsesesescsecscsseassesecessensasseseseeeasacens 17 FIGUKE 4 6 SOP step f1 RUM Systeri Blanik sscsssuccievsivsoicoseseseossbecosorcsescacseueoreseseacssusonsvsaeaeceusonsveneaeseusosonensaeseusoaoneneseseqsosonenensaesenetens 17 Figure 4 7 Home screen ready to perform System Blank RUN cccsssssssssesscscssssssesscscsssssssesscsesssssssssecsescssssseseceseassssesesseseees 18 Figure 4 8 System blank screen displayed while running a blanK ss ssssssesssessesssesseessesssesseossesseossesscessesseesseoseesseoseesseossessees 18 Figure 4 9 Processing RESUS SOCCN eee eee ee SAAR SANE ANSASSA 19 Figure 4 10 Results screen shown after s
117. er showing the All Results tab with multiple possible unknown matches for the PEAK Labeled UNKNOWN 3 wessssscsssssssscosusssscscccsssnsasosesnadsscscsssasasoansesusacacacsnsassasseanaaescansasnsonsansseaascacasansasesessensacocacsnsasonesecasg 88 Figure 5 66 Deconvolution of three peaks with two co eluting peakS ssesssesseessesseesseoseesseossesseessesseesseoseesseoseesseoseessees 89 Figure 5 67 Deconvolution Control Center showing the All Results tab for three peaks identified in the unknown library Unknown 2 and Unknown 3 are co eluting PEAKS ssssecsssssecscssscscsssecscsssececsssecscssssscessccecessssecssaseecsseees 89 Figure 5 68 Right click menu on the MS graph Showing Write Spectra to NIST File sssssessssssesssesseessesseessesseesseossessees 90 Figure 5 69 Write Spectra to NIST File dialog bOX sssessesssessessesseesseossesseossesscossesseosscoseesscossesscosreoseosseoscesseoseesseoseesscossesseossessees 90 Figure 5 70 Peak successfully written to NIST file dialog bOX ssesssesssessseesseessersssessseosseosseesseesseeoseeoseeosseosseesseesseesseessseossees 91 Figure 5 71 Export Charts dialog box active charts are not grayed out Inactive charts are grayed out and not available to create IMAGES scsssssessssssssssssecscscssscsssecscscsesssssesscseseassesesseseseasseseseseseassesescseseacsesesecseseasaesesecseseassesesesseseaeaesees 91 Figure 5 72 Mass Spectrometer screen button baf ssessesssesseesses
118. es res CDF Files cdf CSV Files csv RAW Files raw Figure 5 35 Data Review open file dialog box showing file types 3 The following image shows the dialog box that opens when the user opens a RES type of file 72 OTHER OPERATIONS File Type q What type of file do you want to view netCDF File RAW Data File Figure 5 36 File Type option box that is displayed when opening a file with the RES extension 4 Selecting the netCDF File option will open the CDF file that is in the results file Choosing the RAW Data File will open the raw data that is in the results file 5 The following image shows a CDF data file open in the data review window CHROMION Target4P Fle Edt Method Instrument Wen Togge Daywstks Took Help x EE E 2G or gt 22 8 47 Glee lt BY 6G Scan 353 RT 42 4350 Sec Abun 28 221 Figure 5 37 Data Review window with a CDF file open 6 Print Chart From the popup menu in any graph the user can print the chart The print option uses the windows default printer to print the chart To change to a different printer go to control panel in the Windows operating system and open devices and printers and change the default printer to the printer you want used Data Review Button Bar 1 The button bar specific to the Data Review part of the software is located directly above the data window 2 The following image shows the button used for opening a data file The open file dia
119. es 171 173 and 175 sss sssesssessssesssesssessseesseesseesserosseosreosseesseesseesss 125 Figure 7 7 Uncalibrated mass spectral data of methylene chloride Used for calibration ss ssesssesssessesssesseessesseessesss 126 Figure 7 8 Methylene Chloride mass calibration in Performance Validation screen s sesesesesssessseesseesssessseosseesseesseesss 126 162 TROUBLESHOOTING Figure 7 9 Uncalibrated mass data for MTBE cecssscsssssssssscsssssssssesscscsssssssssscsescsssssesessesesssssesessesesesesesecseseaesesesecseseaeassesecseacass 127 Figure 7 10 Uncalibrated bin data for bromoforM masses 171 173 and 175 ses sssessssesssesssesssessseesseesseesseeosseosseesseesseesss 128 Figure 7 11 Calibration SUCCeede ssscscsssssecsssssecsssssecssossecscassecscassesscassesscasassscasasseessassecss Error Bookmark not defined Figure 7 12 Auto calibration failed message rece ee ere eee 131 Figure 7 13 CHROMION Performance Validation screen ssssssessseseseesseesseesseesssessseesseesseessseosseosseoseesseesseeoseeosseosseosssesseesseesss 131 Figure 7 14 Performance Validation correction showing methyl salicylate peak with binned centroided but alatele E e Ea E i E A E A E E T A AE A 132 Figure 7 15 Performance Validation correction showing bromopentafluorobenzene BPFB peak with binned CORTON A TOU UC Or a e cusses scususs susan eussussacususdiesstss tists suvcudsesexsauvscsssveutustucmsassiisaususcnvestecseys 133 Figure
120. esserssseosseosseosseesseesseeoserossrosseosseesseesseesss 139 Figure 8 10 Placing o ring into vacuum chamber groOVe sssesssessesssesseesseossesseossesscosseoseesseoseeseoseesseoseesseosseoseesseoseesseoseesseess 139 Figure 8 11 Effect of o ring groove tolerances on o ring installation s esssesesesssessseesseesseessseosseesseesseesserssseosseosseesseesseesss 139 Figure 8 12 Use of dust off to remove dust particles from the installed o ring and the mating surface 140 Figure n i min DIO Bice queen sa removal En eon ea a 140 Figure 8 14lon trap RF module FINO AM ccsccsesesescccccecescccesccsescceasesesceseccsasousszesccceascuesceaceceasesescesceceasesescesceasascsesccsceasasesesccsecaeascateseaees 141 Figure 8 15 Exploded view of main trap cCoMponentsS sesssesseessesseesseessesseessesseesseossesseoseeoseeseoseesseoseesseoseesseossesseesseoseesseoseesseoss 141 VU 1G TE EN Oa OIG sreccxsesesetnccwencees anys wenreuvesvasswencsussrse essousssssssrsesseusssonesiessesensuursseaseuessurstsssedesusussesaedesueusstesvedenmennstenseneriens 142 ee Ulg cis cg FA E Eee a E A reverts reverts ceereryreererrerrerererrreererceeereyveveres revert cerertrrererirct reer etrereretrererttrerertrrecerttrerert trent re 143 Figure 8 18 Alignment pin installation diesavevernnrnvenrannwenrannwenrannwenrannnnnninnnanrinnnenrinnnanrinunnndnniie 144 Figure 8 19 Trap orientation on RF board sessssesssesseessesssesseossesseossesseesseoseesseos
121. etector board Detector Board Detector Mounting Holes Electron Multiplier Detector Figure 8 25 Electron multiplier detector mount to detector board 3 Insert the detector into the vacuum chamber and simultaneously plug the electrical connections of the detector board into the ion trap RF module 4 Using 3 32 driver replace the smaller screws 5 Reinstall the captive screws that hold the ion trap RF module in the TRIDION 6 Reinstall the 7 64 driver replace the larger screws 7 Position the white Detector Board Cover and using the T10 Torx driver reinstall the flat head screws Install the ion trap RF module 1 Insert the trap assembly into the vacuum chamber ensuring that the alignment pins slide into the holes on the vacuum chamber and that the vacuum chamber O ring stays in place 2 Using a 7 64 hex driver screw the captive screws into the vacuum chamber end cap 3 Place the front cover of the TRIDION in place by positioning the bottom edge and pushing the top edge into place Use the 7 64 hex driver to install the five screws along the bottom edge of the cover GC injection port maintenance 1 The following sections provide instructions on maintenance of the GC injection port 2 The following image shows an exploded view of the GC injection port Refer to this image while doing maintenance on the GC injection port 150 SERVICE lt Septum lt Injection Liner lt Interface Liner S
122. f b Lint free tissue Kimwipes 134 SERVICE n Clean lint free antistatic gloves or very clean hands d Tool for removing o rings that will not scratch the surface of the o ring groove wooden or plastic tooth pick or plastic tweezers e Cleaning solvent technical grade or better methanol or ethanol f Loop or magnifying lens Figure 8 1 Dust off A Kimwipes B Lint free antistatic gloves C Tool for removing o rings that will not scratch the surface of the o ring groove D Methanol E Magnifying lens F Removing o rings 1 Sharp hard or metal tools should never be used to remove o rings Use plastic or wooden tools as shown in Figure 1D Proper removal of o ring is illustrated in the following figure Figure 8 2 Proper removal of o ring 135 CAUTION SERVICE Installing o rings 2 Before handling any parts or o rings wash clean antistatic gloved hands or bare hands with soap and deionized water Do not use plastic or elastomeric gloves that are not antistatic they attract dust Make sure you rinse several times and ensure all soap is removed from gloves or hands If you use lint free cotton gloves make sure they are really lint free not over used and clean 3 Clean o ring groove with lint free tissue and cleaning solvent The best way to do this is to wet the tissue with the solvent and wipe the o ring groove ensuring that the wipe directly contacts the sealing surfaces of the groove The following im
123. g the RF wire and RF tab to the center electrode football Remove the wire tab and spacer and set them aside on a clean dust free surface 6 Remove the screws that are holding the EGUN mount onto the top of the trap assembly Lift the EGUN mount off of the trap assembly and set it aside on a clean dust free surface 7 Remove the screws that are holding the trap assembly onto the RF board assembly and lift the trap off of the board assembly Set the board assembly aside on a clean dust free surface 8 The trap assembly has many ceramic spacers that are used for electrical isolation and alignment of the parts Make sure that you are working over a flat surface that is clean and dust free Place the trap on the clean dust free surface and carefully remove the screws that are holding the trap assembly together The ceramic spacers may fall out as the screws are being removed this is normal just make sure they all stay together and stay clean Trap cleaning procedure 1 The cleaning is done by placing the two end cap electrodes the ring electrode and the center electrode football in 35 hydrogen peroxide and heating it enough to where the solution boils Allow the parts to soak in the boiling solution for 30 minutes Be careful to avoid scratching or in 142 SERVICE other ways damaging the curved surfaces of the electrodes and end caps Damaged parts must be replaced for proper performance of the instrument Caution The gold plating
124. ground This is the spectral data for a section of background selected by the user f Diff This is the spectral data showing the difference between the background spectra and the highlighted section of chosen spectra g Overlay This is a chromatographic trace of several TICs that have been selected and are displayed together in the same chart h Decon Spectra This is the spectral graph of the deconvolution peaks i Search Spectra This shows the head to tail spectra of an unknown compound search The spectra from the library are on the bottom and the spectra from the analytical run are on top 13 The charts can be exported as WMF JPG BMP or CSV files One of these options needs to be selected in the Export File Type box 14 The Find button allows the user to enter a file name and to select the location where the image files will be stored after they are created 15 The Append Chart Type Suffix option when checked adds the wmf jpg bmp or CSV extension to the file name 16 The CSV data are saved in two columns with the time first and the response second In the case of overlaid TICs the data are in two columns with the time starting at zero then progressing to the end of the first file The time then returns to zero and starts the with the data from the next file This is repeated until all of the files in the overlay graph have been stored in the CSV file The data can be plotted as one single plot The data cannot be easily
125. h the difference graph shown Diff The difference graph shows the background subtracted from the summed values 76 OTHER OPERATIONS Scan 677 RT 92 2050 Sec Abun 2 541 Avg Range 200 231 Bknd Range 225 236 t i i i i i i i i i t r t aiis f 50 100 150 200 250 300 350 Ready 7 7 4 Validation 636 SD Card G36 Data COF O00000 5 cof Figure 5 45 Difference Diff graph with TIC graph g Deconvolution Spectra This shows a graph of the spectra for a single scan in a deconvolved TIC More detail about how to use this feature will be provided in the discussion about the deconvolution control window later in this manual The following image shows the deconvolution graph with the TIC graph The deconvolved peaks are shown in different colors and can be shown in the deconvolution graph by clicking on the peak in the TIC The toluene d8 peak has been highlighted and the purple is bolded The purple spectra are seen in the deconvolution graph S n 205 RT 32 0530 Sec Abun 88 312 i bi ie PE eaaa A Ready 7 T 9 Vakdation G35 SD Card G35 Data CDF W00000545 0dF Figure 5 46 Deconvolution Decon graph with TIC graph h Library Search Spectra This shows head to tail spectra comparing the library spectra to the sample spectra The following image shows the library spectra compared to the instrument spectra 77 OTHER OPERATIONS Scar 204 RT 31 9750 Sec Abun 72 60
126. he horizontal expand collapse arrows located in the orange bar at the top of the pane Figure 5 2 CHROMION main window with Navigation pane collapsed 6 Many of the items in the Navigation pane open forms that contain specific information used to complete the tasks required to operate the GC TMS When a new form is opened additional menu 49 OTHER OPERATIONS items and buttons are added to meet the requirements of the open form The functions of the various menus and buttons will be described later in the chapter CHROMION Menu Bar The following are the menus that are always present on the menu bar Some of the contents of these menus change as needed for a specific open form a File b Edit c Method d Instrument e Help File menu 1 The Exit option closes the CHROMION software 2 When Data Review is active an option to open a data file is included in the File menu 3 Data file types currently supported are a Net CDF This is standard mass spectra file type The header information for this type of file may contain or be missing information that will affect some operations in the Data Review part of the software b RAW This is a Torion file that contains the unfiltered data from the instrument It can be useful for troubleshooting instrument problems It is not easy to interpret the data from this type of file Therefore it is only useful to individuals that have been properly trained c RES This is a
127. he compound listed in the table to elute 68 OTHER OPERATIONS e Retention Calibration If the compound is to be used by the auto calibration routine to calculate the retention indexes of unknown compounds The compounds where the box is left unchecked are used for mass calibration not retention time calibration 3 Above the Retention Time Calibrations table are two buttons 4 The first button is used to add compounds to the table To add compounds highlight a position in the table and click the Add Compound button A new line will appear at the bottom of the table Type in the name of the compound and fill in the numeric values for the other columns 5 Ifavalue is entered that is not acceptable a red exclamation point will be shown in the column on the far left The following image shows an error in the last column of the table next to Ethyl Acetate In this case a letter has been entered into a numeric value only field Retention Index If this happens the software will not allow the user to change to another field until the error situation has been corrected Time Calibrations ioe i eS ec 41 7 Bromoform 853 45 1 43 Dibromotetrafl 1100 65 6 63 Methyl Salicylate 1281 717 68 Tetradecane 1400 85 83 J Ethyl Acetate A O Masses for lt Ethyl Acetate gt fa Figure 5 30 Performance Validation screen showing an error in data entry 6 To remove a compound use the m
128. he bottom file that is to be selected The using the mouse click on the highlighted files and while holding down the mouse button drag them to the left side of the screen Files can be deleted only from the bottom frames To empty the SD card it is possible to delete files by right clicking and selecting the delete option from the popup menu To do more advanced file manipulation remove the SD card from the instrument and insert it into a computer Then use the software on the computer to move and delete files Caution When using the File Manager in the CHROMION software some files and directories are protected This prevents deletion of items that are important to the operation of the instrument When viewing and editing the SD card directly on a computer none of these safeguards are in effect To prevent loss of data it is best to create a copy of the SD card on the computer before deleting any files If files or folder have been deleted the firmware on the instrument will reconstruct the SD card directories but all data and libraries will not be loaded until they are sent from a computer running CHROMION 96 CAUTION OTHER OPERATIONS Library Editor 1 The Library Editor is used to look at and change libraries After they have been refined they can then be exported as an unknown library for use on the instrument or compounds can exported to the Target List 2 The following screen shows the Library Editor Libr
129. he new Liner There are two separate Liners that can be used in the TRIDION There is a liner for SPME type injections and a larger volume liner for small liquid injections Reinstall the Septum Nut Make sure the Septum Nut is tight The Liner has a deactivated surface It can be cleaned with normal solvents like methanol or hexane Use of aggressive acid or base will damage the liner coating and result in poor performance for active chemical compounds If the Liner appears to be scratched or damaged in any way it is recommended that the Liner be replaced Re install the Universal Interface by positioning it with the flat side of the port lining up with the flat side of the opening Make sure the assembly is plugged into the board Reinstall the stainless steel Interface Mounting Ring Nut and the protective cover 152 TROUBLESHOOTING 9 Troubleshooting This chapter describes basic troubleshooting of the TRIDION TRIDION will not turn on 1 Press the power button firmly for ten seconds see figure 5 1 2 Check the batteries for proper installation Remove and re install the batteries or replace them with new charged batteries 3 Check the external power source for proper function and verify that the voltage regulator meets the correct specifications see the section called Power Supply and Battery Remove the power source connector from the TRIDION and re insert it snuggly TRIDION will not turn off 1 Press t
130. he on screen instructions to inject the CALION standard into the instrument After the analysis use File Manager to move the RES file over to the computer Refer to the Software chapter for details about using File Manager Use CHROMION Data Review to open the file Refer to the Software chapter for details about the functionality of CHROMION Data Review Evaluate the masses look at each scan in the peaks rather than the average At least 80 of the scans for each peak should have the correct masses The 128 LIBRARIES following list contains all the peaks in the CALION mix along with a few of the masses in each compound The data file should have all of the listed masses correctly identified to validate the calibration 6 Toluene d8 98 100 SS 11 Methylsalicylate 92 120 121 152 vi If each mass does not match the list above then the instrument needs to be recalibrated vii To recalibrate repeat above procedure TRIDION Auto Calibration Performance Validation 1 Open the Advanced screen on the TRIDION 2 Select the Procedure button and end the procedure 3 Usethe Home button then select the Advanced button to return to the Advanced screen 4 Select the Performance Validation button and follow the on screen instructions 5 Runthe 13 mix CALION standard 129 LIBRARIES 6 The instrument should give the following report l Efx Torion Hogi 4 Diagnostics sen Calibration Results xia
131. he power button firmly for ten seconds see figure 5 1 2 Re set the on board computer see the section called Re set the on board computer in the Advanced Operations chapter of this manual TRIDION cannot maintain vacuum 1 If recent maintenance was performed on the instrument where the vacuum chamber was opened ensure that the O ring seal to the vacuum chamber is properly seated to maintain a proper seal 2 Refer to the Instrument Operation chapter under the Advanced Status Diagnostics Mass Spectrometer section for images of the screens 3 The turbo pump information is shown on the Mass Spectrometer tab 4 Verify that the frequency of the Turbo Pump is not increasing see Hz column to the right of Turbo Pump it should progress until 1500 10 Hz If the frequency is increasing wait to see if the vacuum can be established If the frequency is not increasing or the vacuum is not established continue with the next step 5 Restart the instrument Another attempt may be successful If the vacuum is not achieved after the second try contact TORION Technologies 153 TROUBLESHOOTING GC baseline is noisy or drifts upward 1 A noisy chromatogram suggests chemical contamination Contamination can arise from dirty components such as from the SPME fiber injector port chromatographic column vacuum chamber or ion trap 2 The following list provides possible solutions for correcting a noisy GC baseline a Clean the SPME
132. hows the screen that is displayed after selecting the Bluetooth Control button on the System Settings screen Target4E Torion 1 SystemBlank Smiths Detection version 1 00 Connection Attempts 2405 Figure 4 52 Bluetooth control screen 14 Use this screen to input any settings when using a Bluetooth device with the instrument Previous Results 1 Pressing the Previous Results button from the Home screen will display the following screen 42 INSTRUMENT OPERATION Target4E Torion 1 SystemBlank Folder 012 04 23 v Figure 4 53 Previous Results screen 2 From the Previous Results screen touch the drop down arrow on the Folder list to display a list of folders on the SD card as shown below Tarqget4E Torion 1 SystemBlank 2012 04 19 2012 04 19 1 2012 04 16 2012 04 13 2012 04 12 2012 04 11 2012 04 02 2012 03 30 2012 03 29 Figure 4 54 Choosing a folder from the Previous Results screen 3 Highlight and double touch the desired folder A list of all the data files within the chosen folder will be displayed as shown in the following figure 43 INSTRUMENT OPERATION Target4E 1 SystemBlank Folder 2012 03 29 20sample01 2012 03 29 00 11 20sample01 2012 03 29 00 15 SystemBlank 20sample01 2012 03 29 03 10 SystemBlank 20sample03 2012 03 29 00 23 SystemBlank 20sample03 2012 03 29 03 15 SystemBlank 20sample04 2012 03 29 02 05 SystemBlank 20sample04 201
133. iessneewidsnnwad an adliaannnanenwhitn 157 Acquired mass spectra are NOt COIe Ct cccceeceeseeeceeeeeeeeeeneeeeeeeeees 158 SPME fiber came off inside the GC inlet ccccccssseeeseeeeeseeeeeneees 158 TRIDION fails Performance Validation ccccsescccseeeeeeeeeeeeeeeseaeees 158 TRIDION fails to identify a compound cece eceeeeeeeeeeeeeeeeeeeeeaeeeees 158 TRIDION falsely identified a compound cceeceeeeeeeeeeeeeeeeeeaeeeees 159 TRIDION fails to reach Set temperatures ccccccseeeeceeeeeeeeeeeeeeees 159 TRIDION is unable to run on battery power ccseceecseeeeeeeeeeeeeeees 159 TRIDION Suddenly powers GOWN cccsescecseeeeeeeeeecaeeeesaeeeesaueeesaaeees 159 TRIDION is dropping data points ccceccccsseeeeseeeecaeeeeseeeeeeseeeessaeees 159 Table OF ROUIGO teteacceaistntctatesacegies a A A 160 MO OX n daet ane idewenes scandens cemrtectcaeneestee tear 164 INTRODUCTION 1 Introduction This chapter contains a brief introduction to the TRIDION and CUSTODION products TRIDION GC TMS and the CUSTODION line of solid phase microextraction SPME syringes Both basic operations such as running a sample and changing the batteries and advanced operations such as re analyzing data and changing the instrument operating parameters are included T his user s manual provides step by step instructions for operating and trouble shooting the The TRI
134. ime reasonable 5 The Window refers to retention index window to be used Part of the search algorithm uses retention index The window is normally set to 75 Performance Validation 1 The Performance Validation is used to setup the information used for calibration of both retention time and mass The following image shows the performance validation screen DEJ Retention Time Calibrations Acetone 455 Methylene Chl 531 MTBE 510 Toluene d8 759 875 41 7 853 45 1 Masses for lt Acetone gt Figure 5 29 Performance Validation window 2 The following is a description of each of the columns in the Retention Time Calibrations table a Name This column is used for the names of the standards that will be used for the calibration and validation of the instrument performance b Retention Index These are retention index values from the NIST data base A description of retention indexes and how they are used is provided in the Retention Time Calibration section of this manual c Retention Time Expected This is the time that the compound is expected to elute from the instrument If the Gas Chromatography method is changed then it is necessary to run the standard mix and adjust the retention times in the Performance Validation table d Retention Time Expected Minimum and Retention Time Expected Maximum are used to set a window of time where the automatic calibration routines would expect t
135. in on Tarqet4E y Torion Technologies 20sample04 2012 04 1 4 Sample 19776 9 15821 5 11866 1 7910 7 3955 4 0 0 Options Figure 4 27 Screen showing Zoom feature in the TIC window post run 28 INSTRUMENT OPERATION 12 The following image shows the library results screen displayed a the end of a run Target4E Torion 20sample04 2012 04 1 4 Sample 0 6 26 6 52 6 78 6 104 6 RT Identification Allert Match __ 11 5 Acetone 99 5 5099 7 13 5 Methylene Chloride 97 0 7586 6 15 5 Diethylamine 84 3 79 5 15 7 Allyl Alcohol 90 2 AE x gt feet ie 7 More Figure 4 28 Library results screen shown at the end ofa run 13 In the figure above the table on the bottom of the screen shows the post run results table or the library hits See the Run a Sample section of this manual for a detailed description of the table The zoom features works the same during a run as it does post run 14 The following image shows the screen that is displayed after choosing the Split View option and using the zoom function on the TIC plot 42723 2 34178 6 25633 9 17089 3 8544 6 0 0 15000 0 12000 0 9000 0 6000 0 3000 0 0 0 Figure 4 29 Screen showing the zoomed in results with Split View showing spectra at cursor position 15 The spectra of a specific scan can be previewed by placing the cursor at the desired scan in the TIC plot at the top of the screen To place the cursor simply touch the scr
136. ins all of the information needed to display the chromatogram and mass spectra in the correct format for peak identification RAW is a format of data that is produced directly by the instrument The mass spectral data has not been calibrated and does not display masses rather is displays indices It is not sorted and labeled so that it can be used to compare to traditional data In addition it has not been processed using the auto ionization algorithms It is used for diagnostic purposes to determine the performance of an instrument CSV is a standard file type that can be opened in most spreadsheet programs like Windows Excel These files are created by the user through export functions 2 Data can be directly opened from a RES CDF or RAW file In the case of the RES file the users can choose between opening the CDF file or the RAW file The following image shows the open file dialog with the file type drop down menu visible RS iy x Q K T 9 Validation G46 2012_03_21 KE search 2012_03_21 o Organize New folder z 0 a Name Ww Favorites BE Desktop m 00000057S res 3 21 201 JB Downloads i 00000058C res 3 21 201 teen t 00000059S res 3 21 201 Ey Lbraries ra 00000065C res 3 21 201 Pe ra 00000066S res 3 21 201 a Music t Pictures F Videos a Homegroup J amp E Computer amp os C G2 Mechanical on SBS1 M yi gt File name Result Files res Result Fil
137. ion sssesssesessesssesssessserssersserseeosrcosscosserssersssrosreosreosreosseosserosersssrossrosreosseesssesssrsserssreosseessees 25 Figure 4 22 Calibration results screen when calibration succeeds sesssesesessesssesseessesssesseossesseosseoseessesseesseoseesseossesseossessees 25 Figure 4 23 SOP step 3 instrument is ready to FUN SAMPIES cesscsssssssecscscsssssssesscscscsssssesscsessssssseseesescacsssesecscseassesesecscseass 26 Figure 4 24 Home screen ready to gUiquct lga 0 ocean ner er re are ere eee nr 26 Figure 4 25 Screen SHOWN during a sample FUN csssssssssececscsssssssececscesscsssecscscasscsesesesscacassesecessensassesesesscssassesesessessasacsesessensarens 27 Figure 4 26 Screen shown during a run USING the Split Screen ssessessesseeseeseessessessessesseoseoseoseeseesressesressesseoseoseoseoseoseoseeseeseess 28 Figure 4 27 Screen showing Zoom feature in the TIC window post rUN ssessseesssesssessseosseesseesseesseeoseeosseosseosseesseessersseeossees 28 Figure 4 28 Library results screen shown at the end Of a FUN sssssssssecscssscecsesssecscsesecscsesecscsesecscscsecscsesscecsessescsessencasseencees 29 Figure 4 29 Screen showing the zoomed in results with Split View showing spectra at Cursor poOSition 00 29 Figure 4 30 Screen showing the zoom FUNCTION in the spectra WINKOW ssscscsssscscsssssecsssssecsssesecssssseessseseceesssseteasseeeeees 30 Figure 4 31 Screen showing the zoomed in
138. ionized chemical fragments are separated by a mass analyzer before they are registered by the detector Typical mass analyzers include quadrupole time of flight and ion traps The TRIDION uses a miniaturized toroidal ion trap TMS mass analyzer that possesses advantages of simplicity low power consumption and high sensitivity Mass analysis is accomplished by first trapping ions in the trap with an RF and then applying a constant frequency tickle voltage as the RF voltage is increased causing ions to be ejected from the ion trap to the detector based on m z and their resonant frequency for ejection Discrete ranges windows of the ejection RF voltage are assigned to discrete m z values of the detected ions Figure 2 4 Cut away drawing of the toroidal ion trap showing trapping of ions red dots in a toroidal geometry around the center electrode lon detection provides the abundances of the fragment ions in the mass spectrum The detector in the TRIDION is a continuous dynode electron multiplier Positive ions exiting the trap are directed by a negative bias to strike a surface at the entrance of the detector The surface emits electrons when struck by ions with sufficient energy The electrons are directed by a positive bias striking further along the continuous dynode emitting increasingly more electrons as they sequentially strike the dynode in areas of decreasing negative voltage The positive bias ultimately directs the electrons to a colle
139. is open a Link MSDS File This option opens the following dialog box which allows the user to link a file to the Compound Details MSDS field x K J OS C Library Files MSDS Sheets v ka Search MSDS Sheets a Organize v New folder r i E FY Favorites ME Desktop meun L Downloads remrem E Recent Places Z Libraries See a Music gt E E Pictures fh Hines 7 Computer Benzo_a_pyrene MSDS pdf amp os c xj File name All files v Figure 5 81 Link MSDS file location dialog b View MSDS File This opens the MSDS file that was linked previously c Add Compound Image This opens the following dialog box that allows the user to select an image file that shows the compounds structure 101 OTHER OPERATIONS SS SS E a ENS A Alpha methylstyren Benzo a pyrene pn g png Figure 5 82 Library Editor Add Compound Image dialog box d Zoom Into Image This option opens a larger copy of the Structure Image 11 Almost all of the functions found on the menu bar are duplicated using the right click popup menus Real Time Plots 1 Real time plots are used to display information from the instrument on a computer To display a plot the software must connected to an instrument Information from only one instrument at a time can be displayed 2 The following shows an image of the Real Time Plots screen TIC Graph Spectra Gra
140. ivate button will make the selected method the active method that the instrument will use for future runs 5 Selecting the View button will open a window as shown below which displays the settings in the method 37 INSTRUMENT OPERATION Target4E Torion Tec 1 SystemBlank Injection Parameters Column Parameters Data Analysis Injector Settings Split Splitless Settings Injector Temp 270 10 1 Split On Transfer Line Temp 270 10 1 Split Off Inlet Pressure o 50 1 Split On 50 1 Split Off Figure 4 44 Viewing method injection parameters 6 The first tab inside the Methods View screen is the Injection Parameters tab as shown above This screen displays the method settings for the Injector and the Split Flow 7 Choosing the Back button will take the screen back to the Method screen 8 Choosing the Activate button will activate the method that is being displayed 9 Choosing the Column Parameters tab will display the Column Parameters tab as shown in the figure below Tarqget4E 1 S ystemBlank Initial Temperature Initial Hold Time Temperature Rate Final Temperature Final Hold Time Figure 4 45 Viewing method column parameters 10 The Column Parameters tab displays the set column parameters in the chosen method 11 Choosing the Data Analysis tab will display the Data Analysis tab as shown in the figure below 38 INSTRUMENT OPERATION qet4E Torion SystemBlank 4499
141. ld wo Window 0 Kok aah i5 Pah3 oo Find Smoothing parameter m o Window 0 ee Window 0 Minimum known compound area jo Figure 5 28 Deconvolution Parameters screen 2 The Search for known compounds check box enables the deconvolution algorithm to extract the spectra of target compounds and compare the extracted spectra to the Target List The default is for this to be checked Unchecking this option will result in the search algorithms not returning matches for compounds it the Target List 3 The Search for unknown compounds check box enables the deconvolution algorithm to extract and save the spectra of compounds that are not found in the Target List It does not search the unknown library it only allows for the extraction of the spectra 4 The Maximum top spectral hits to show allow the user to specify the number of unknown compounds to display in either the CHROMION software or on the instrument If a chromatogram has a large number of small peaks allowing deconvolution and display of all of them will result in slowing down the on instrument post run data processing The default of 10 is a good compromise that allows for significant peaks to be identified while limiting the burden on the instrument processor 5 The Noise Remove check box turns on and off the noise removal portion of the deconvolution algorithm Unchecking this box will result in poor spectral extraction and potential miss identification of compounds
142. lidation Removing Compound Mass dialog bOX ssesssesseessesseessesssesseessesseessesseesseoseesseossessees 71 Figure 5 35 Data Review open file dialog box showing file types esesssscsssssssecscscsssssssessccsssssssesecsesesssssesecscseassssesecseaeaes 72 Figure 5 36 File Type option box that is displayed when opening a file with the RES extension ssessesseessesseessess 73 Figure 5 37 Data Review window with a CDF file open uuu sssscsssssesessssscscsssscecsssscecsssssecsssssecssscsecessesecscsesscucsesecucseseescasssescess 73 Figure 5 38 Data Review Button bar showing the location of the open file button sssesssessseesssesssesssessseesseesseesssesssess 73 Figure 5 39 Data Review button bar with labels for the buttons that are used to show Graphs s sssesssesssessseesssesssess 74 Figure 5 40 TIC graph showing TIC of 13 compound calibration standard sssssssesssesssessseesseesseessseosseosseosseesseessersssesssees 74 Figure 5 41TIC and MS graphs ee 75 Figure 5 42 RIC graph with TIC graph and MS graphs ccsssssssssesscscssssssesscscsssssssesscscsesssssesseseseassesesecsescaesesesecscseassesesecseaeass 75 Figure 5 43 Summed graph with TIC and MS grap S ssesssessesssesssesscossesscossesseossesseosscoseesscossesscosseoscosseoseesseoseesscosersscossesseossessees 76 Figure 5 44 Background Bknd graph with TIC and Summed graphs ssssssesssssesssesssessesssesseossesseossesscessesseesseoseesseossesseossessees 76
143. log box can also be opened using the files menu O LA dd LB a th 98 oll A OT ab BB a Open Data File Figure 5 38 Data Review Button bar showing the location of the open file button 3 The following image shows the Data Review button bar with labels for the buttons that are used to show graphs 73 OTHER OPERATIONS EAFF E a A POR co BH A Dy 1 he ar n Show Hide TIC Window HOIA D oo a a A POT od a B AT HOIA wia a a A POS o gt ee bs LOJA w CRE k ah eT a 8 Td ESP Ac ahd Da GY 385 all A POT ay 2 Show Hide Background Window HOJA oth GH oc oe ES ol A OS a a BI At EO lA wh D ot amp GA Oe 4 1 a ED lA de D a eh 8 all FAY TOS cd a b A Figure 5 39 Data Review button bar with labels for the buttons that are used to show graphs 4 All of these functions are also available through the menus in the software 5 The following are descriptions of the graphs that are opened by the buttons a TIC Total lon Chromatogram This is the GC trace of the entire signal that is generated by the mass spectrometer The following Image shows the TIC graph window open with no other graphs being displayed Figure 5 40 TIC graph showing TIC of 13 compound calibration standard b MS Mass Spectra This is the spectra for a single scan in the TIC The spectra displayed are selected by the placement of the cursor The following image shows the MS gr
144. low thermal mass GC and TMS allows rapid separation of chemicals in the sample and generation of a mass spectral fingerprint for each chemical The on board central processing unit CPU compares the retention time and mass spectrum of each chemical to a library of retention times and mass spectra of known chemicals and indicates whether or not any of the target chemicals in the library are present in the sample The front panel of the TRIDION contains the battery compartment display screen power and operating buttons SPME sample injection port memory card slot Ethernet port carrier gas cartridge connection status lights and manual shut off access The internal components are precision mechanical and electronic parts including heaters vacuum pumps pressure controller gas flow lines circuit boards CPU SPME injector low thermal mass GC and TMS TUTORIAL Stylus i M _ Utility Cover Touch Screen Display a Status Lights l GC Injection Port Operating Buttons fi Cooling Air Flow Cover Service Cover Figure 2 6 TRIDION GC TMS External Vent Helium External Power Battery Cavity LAN Port IPN USB Port SD Memory Card Processor Reset Q System Reset in a Touch Screen Display ___ Helium Cylinder Helium Cylinder Tool GClnjection Port Torion Technologies esc Status Lights i Battery Power Power Button lt lt Control Buttons
145. ly deactivated one see the section entitled GC injection port maintenance Replace the column contact TORION Increase the split flow rate 7 A peak may be non Gaussian if too few data points are obtained Too few points result from low sample concentration low ionization yield incorrect detector voltage detector malfunction steep temperature gradient in the temperature program or rapid carrier gas flow rate 8 The following list provides additional solutions for correcting peak shape due to low concentration Analyze a more concentrated sample Increase the filament current increase number of electrons and therefore number of ions however the filament may burn out faster Increase the detector voltage This may help slightly but the noise increases as well Too high of a detector voltage can permanently damage the instrument and will age the detector faster Replace the detector with a new one Reduce the temperature programming rate to broaden the bands in the column and thereby broaden the peaks Reduce the carrier gas flow rate to broaden the bands in the column and thereby broaden the peaks 155 TROUBLESHOOTING GC peaks are eluting late 1 When users notice that the GC peaks are eluting late or early this indicates a change in air flow or pressure A change in air flow or pressure can be due to several things If the peaks are eluting late the following is a list of things for users to verify a Verif
146. lysis 4 Turn onthe TRIDION if it is off otherwise begin with step 5 5 Select the Advanced button from the Home screen The following image shows the Advanced screen Val Seca Status Diagnostics Performance a Manage Files Validation J Method System Settings Procedure Figure 7 1 Advanced screen 6 Foracomplete description of all the operations available from the Advanced screen see the Advanced Screens section in the Instrument Operation chapter of this manual 7 Exit the Advanced screen any time by selecting the Home button 117 CAUTION LIBRARIES Viewing current calibration points and operating parameters 1 Current calibration points and operating parameters may be viewed in three ways from the TRIDION instrument screen opening the saved settings file using CHROMION software or by retrieving the settings file from the instrument using CHROMION software Viewing calibration points and operating parameters on the screen of the TRIDION 1 Calibration information is found in the Status Diagnostics section of the advanced screen 2 Follow the instructions in the instrument control user interface chapter to access the calibration information on the instrument Viewing calibration points and operating parameters by retrieving the method file from the instrument 1 Open the CHROMION software on a computer that is connected to a TRIDION Follow the procedures in the software chapter to assign the c
147. ment 0 02 or Increase Detector Voltage 25V Baseline BASELINE TEST No Message Mass Calibration BIN SHIFT TEST Reduce Filament 0 02A and or Increase Detector Voltage 25V Mass Calibration CALIBRATION CHECK No Message Spectral Quality Bromoform 171 m z SPACE CHARGE Reduce Filament 0 02 Increase TEST Detector Voltage 25V Spectral Quality Toluene d8 MS SPECTRAL QUALITY No Message OVER SCANS TEST Spectral Quality Bromopentafluorobenzene MS Increase Detector Voltage 25V SPECTRAL QUALITY TEST Spectral Quality 1 2 Dibromotetrafluorobenzene 308 Increase Detector Voltage 25V m z AT APEX TEST Spectral Quality Bromoform ION STATISTICS TEST Reduce Detector Voltage 25V Spectral Quality Heptane MS SPECTRAL QUALITY No Message TEST Resolution Bromoform 173 m z FWHM TEST No Message Resolution 1 2 Dibromotetrafluorobenzene 308 No Message m z FWHM TEST Background BACKGROUND LEVEL TEST No Message Compound ID Compound ID Test Recalibrate 16 Some of the suggestions will recommend adjusting settings on the TRIDION 9 instrument These will be shown in the Adjustments field on the left side of the Tuning Wizard screen The Set value field shows the current settings The New value field shows the suggested changes 109 OTHER OPERATIONS 17 The user can send the suggested changes to the instrument by clicking on the Send button If the user is experienced and would like to adjust the new values before sending them to the instrument
148. n aqueous or an organic solvent should be used Table 3 1 Liquid unknown sample flow chart 11 BASIC OPERATIONS S olid Unknown S ample Take headspace of sample in environment If sample detection is too high If sample detection is too low Take headspace with shorter exposure time Increase exposure time Place sample into a vial and take headspace Reduce the time of exposure in injector port Heat vial warm with hand or other means Allow sample on SPME to evaporate before such as equipment in mobile lab and take injection do this by exposing the SPME fiber headspace to the atmosphere Dissolve sample in appropriate solvent Use a syringe to take the headspace and Immerse SPME directly in liquid of the deliver itinto another vial Take headspace dilution Do this in a mobile lab under of the transferred headspace engineering control Be careful of possible reactions with solvent Use the M 8 paper test to determine whether an aqueous or an organic solvent should be used Dilute sample in appropriate solvent Immerse SPME directly in liquid of the dilution Do this in a mobile lab under engineering control Be careful of possible reactions with solvent Use the M 8 paper test to determine whether an aqueous or an organic solvent should be used Table 3 2 Solid unknown sample flow chart Performing an Injection with the CUSTODION Syringe 1 When performing an injection with the CUSTODION Syringe on the
149. ncentrated and is saturating the column allowing some of the sample to elute faster than expected 5 The following list provides possible solutions to correct for fronting a Usea faster injection time by leaving the SPME fiber extended for a much shorter time during the introduction of the sample To do this extend the SPME fiber when prompted by the screen and then immediately retract the fiber and remove the syringe without waiting for the additional prompts 154 TROUBLESHOOTING Observation Tailing Collect the sample using the headspace method described in the section called Using the CUSTODION for obtaining a sample for analysis Dilute the sample Use a sample solvent with less affinity for the SPME fiber For example replace acetone with water if possible Example Possible cause 1 A surface to which the sample is exposed is adsorptive This can arise because the injector column or transfer lines are not deactivated well enough or these surfaces become contaminated with nonvolatile components in the sample 2 Dead volume or cold spot in the injection a port 6 The following list provides possible solutions to correct for tailing d e Try baking out the injector and column see the section entitled Bake out the GC injection port and column Clean the injection port liner with appropriate solvents see the section entitled GC injection port maintenance Replace the injection port liner with a new
150. nd A blue box will be visible on the TIC Each mass associated with the scans in the highlighted area will be added together and can be displayed by opening the Background graph To clear the selected region place the cursor in the blue highlighted area by clicking on the area with the mouse Then click the right mouse button to open the right click menu Then select Clear Region and choose Under Cursor Summed or All option to clear the selected area The Under Cursor option only clears the region where the cursor line is located If the cursor is not in a highlighted region than choosing the Under Cursor option will not have any effect The Summed option will clear all of the yellow Summed regions but will leave the blue Background regions The All option clears all selections regardless of type The following image shows the right mouse click dialog box with the Clear Region menu expanded 13 The following image shows the last buttons on the Data Review button bar 79 OTHER OPERATIONS LOJA dh D a a ol A ED gt so BY 5 2 EOLA thd ae ait 982 all FOS gt a B Ay U da BN a halle I a E EOL A de D aa BER hg so BU iO lA td D ath ts 85h EO a BS AT I Launch NIST Search Figure 5 51 Copy lons from RIC to TIC Select Overlay File List Change Overlay Files On OFF Launch Deconvolution Control Window and Launch NIST Search buttons Detail on Use of Data Review Functions RIC Reconstructed lon Chromatogr
151. ndard Mix Analyze the 3 runs to determine if the acquired masses although incorrect are the same for each run 1 amu If from run to run the masses are shifting dramatically contact Torion Technologies If the masses although incorrect are staying the same 1 amu from run to run continue to perform the steps below until the problem is corrected When the acquired mass spectra are not correct the TRIDION should be recalibrated see section Performance Validation Button in the Instrument Operation chapter After performing the Performance Validation run the CALION mix again as a sample to verify that the acquired masses are now correct If needed repeat the Performance Validation a couple times Another problem that can contribute to incorrect mass assignments is a dirty trap For trap removal and cleaning instructions see the Service chapter After cleaning the trap perform a Performance Validation then analyze the CALION Mix using the TRIDION and ensure that the acquired mass spectra are correct If none of these steps corrected the acquired mass spectra contact Torion Technologies SPME fiber came off inside the GC inlet Occasionally a SPME fiber can come off inside the GC inlet This can happen when the fiber is getting old if the fiber is used in an incompatible solvent it swells or breaks if the SPME syringe is pulled out of the inlet while the fiber is exposed etc It is very important that the SPME fiber is removed from the i
152. nge and remove the syringe from the GC injection port 22 INSTRUMENT OPERATION Torion Performance Validation L 4 r 0 nd 2 Depress plunger then remove syringe Figure 4 17 Depress plunger then remove syringe screen 8 The following image shows the screen that is displayed while the system is running a performance validation Torion Performance Validation Figure 4 18 Screen shown while running a Performance Validation 9 The following image shows the screen that is displayed when the calibration succeeds 23 INSTRUMENT OPERATION Torion Performance Validation Galibration Results Calibration Succeeded Figure 4 19 Calibration Succeeded 10 The following image shows the screen that is displayed if the calibration fails Torion Performance Validation Galibration Results Calibration failed Figure 4 20 Calibration results screen when calibration fails 11 After choosing OK the following screen appears to retry the performance validation 24 INSTRUMENT OPERATION Torion Performance Yalidation 0 Firms Message Your instrument failed Performance Validation Press OK to retry Figure 4 21 Retry Performance Validation 12 After choosing OK the instrument screens prompt the user to perform an injection as shown previously 13 The following image is shown when the calibration succeeds Torion Performance Validation 0 Galibration Results Calibration
153. nlet immediately If the fiber is left inside the inlet subsequent fibers that are inserted in the inlet might break off because there is not enough room for the fiber Fibers left inside the inlet can also allow fiber debris to block the GC or even damage the GC column To remove a SPME fiber from the GC inlet follow the steps in the GC injection port maintenance section of the Service chapter Ensure that the entire fiber is removed from the inlet Merlin Septum and GC liner TRIDION fails Performance Validation See the section Correcting failed auto calibration Performance Validation in the Advanced Operations chapter TRIDION fails to identify a compound It is possible that the TRIDION can fail to identify a compound that is actually present a false negative identification There are several reasons why the TRIDION would fail to identify the compound Address each of the possibilities listed below 1 The target compound did not elute within the correct retention time window This may happen if a The retention time window set in the library may be too small b The TRIDION may be running out of helium 2 The target compound does not have the correct mass spectrum If this is the case see the troubleshooting section Acquired mass spectra are not correct to solve this problem 158 TROUBLESHOOTING TRIDION falsely identified a compound It is possible that the G 7 can identify a compound that is actually not present
154. nnect the instrument to a computer 3 Open the CHROMION software 4 Follow the instructions in the CHROMION software section of this manual for instructions on how to connect the computer to the TRIDION 5 Open the Performance Validation section of the CHROMION software 6 The following image shows the window that will open after selecting the Performance Validation option Retention Time Calibrations Toluene d8 amp ta 328 Bromofom 853 asa t Dibromotetraf _ 1100 5 6 igi ae fethyl Salcyate 1281 E aad esd 1400 ee 88 al E Masses for lt Methyl Salicylate gt Figure 7 113 CHROMION Performance Validation screen 7 The windows for retention time and mass calibration are shown in the Performance Validation tables The retention times are in the top table and the masses are in the bottom table To select a compound click on the compound name in the top table and the mass data displayed in the bottom table will change to the data associated with the selected compound 131 LIBRARIES 8 Most of the time an auto calibration fails because one of the retention times or mass calibration bins has changed and is no longer in the window set in the method To check the information it is necessary to open the last auto calibration data file Use the File Manager to browse to the storage card calibration data folder on the storage card Move the file to a location on th
155. ormance Validation 1 The second step of the manufacturers SOP is running a Performance Validation 20 INSTRUMENT OPERATION 2 After running a System Blank run the following image shows the screen that is displayed Target4E Torion 1 SystemBlank Firms Message SOP step 2 Run Performance Validation Press OK to continue Figure 4 13 SOP step 2 Run Performance Validation screen 3 Choose OK to run a Performance Validation 4 Sometimes the following screen will appear in between instrument runs This screen indicates that the instrument is still cooling down the GC column back to the initial set point before the next run can be performed Torion Performance Yalidation 0 Please Wait Figure 4 14 Please Wait screen indicating that the GC column is still cooling to initial set point 5 Once the instrument is ready to perform the next run the following screen will appear prompting the user to insert the syringe and depress the plunger 21 INSTRUMENT OPERATION Torion Figure 4 15 Instructions on how to perform an injection 6 The following image shows the screen indicating for the user to wait while the analytes thermally desorb from the SPME fiber into the GC injection port Torion Performance Validation L 4 Part at e 2 Please Wait W Figure 4 16 Please wait injection screen 7 The following image indicates when the user should depress the plunger of the CUSTODION syri
156. orrect IP address for an instrument and attach to the desired instrument 2 From the CHROMION main screen choose the Mass Spectrometer section under the Tools tab located on the left side of the screen 3 If an instrument is already attached to the computer the settings and calibration information will already be loaded onto the computer If no instrument is attached then the calibration information will not be visible 4 The settings are visible in the MS Settings tab 5 Select the MS Calibrations tab to see the mass calibration information Loading operational settings onto the TRIDION 1 Methods store information about items that are affected by the chromatographic conditions The operating settings are separate and are used to control instrument specific functions 2 Both the method and the settings file are stored on the SD memory card Settings become active immediately while method settings must be activated before taking affect 3 New settings may be sent to the instrument at anytime while methods can only be sent when the instrument is not performing an analysis If inappropriate setting changes are sent while a sample is running the analytical results will not be correct and there is a risk of locking the instrument resulting in a need to do a hard reset Caution Only voltages and temperatures can be safely changed while an instrument is performing an analysis Other settings are used for filtering of data and may cau
157. ouse to highlight the compound in the table then click the Remove Compound button which is the second button from the left with the trash can on it The following image shows the dialog box that opens after clicking on the Remove Compound button Remove Compound a i Remove the selected compound Figure 5 31 Performance Validation Remove Compound dialog box 7 Selecting yes will remove the compound from the table 8 The Masses for lt compound name gt table displays the selected masses for a specific compound 69 OTHER OPERATIONS DEJ Retention Time Calibrations Toluene d8 BPFB Bromoform Dibromotetrafi Metin Saicyiate 1281 Tetradecane 1 lt 1 1 1 XI xI Figure 5 32 Performance Validation showing Masses for Bromoform 9 The TRIDION 9 instrument has approximately 4000 bins for mass data Each mass has a width of about 8 bins To convert the index numbers to actual mass values it is necessary to assign a specified mass to a specific index number The auto calibration routine built into the instrument will apply the calibration automatically The mass information is stored in the Mass for lt compound name gt table The data that are entered into the table are described below 10 The following are the columns for the Masses for lt compound name gt table a Mass Expected This column is where the mass to be used for calibration that is in a specific
158. ove there is only one Main mass peak and it is usually the largest peak in the spectrum It is always assigned the value of 100 65 OTHER OPERATIONS All other masses can be defined as being Necessary or Unnecessary Necessary masses must be present in a spectrum or the search algorithm will not identify the peak Unnecessary masses are in the spectrum but are not used by the search algorithm to identify a compound Unnecessary masses are usually masses that are less than 20 of the main mass The values in the masses table can be edited by highlighting the entry with the mouse and typing in the new value Clicking the right mouse button on a mass opens the delete mass option If a mass is deleted by accident exit the program without saving the method when prompted to save the method select no Then reopen the software and the method will be the same as before the mass was accidentally deleted Once a method has been saved there is no way to undo any previous actions It is always wise to keep a backup of important methods so the user can easily return to a n earlier unchanged version of the method The Spectra window shows graphically the information that is in the Masses table The main table is the actual Target List The Compound Name column is where the name of a target compound is entered This column can accept any typed in name The Retention Time column shows the retention time for a compound The Retention Minimum
159. ph Data Logger Figure 5 83 Real Time Plots screen 3 There are three types of plots 102 OTHER OPERATIONS a TIC Graph This displays the TIC in near real time as it is running on a connected instrument The user can zoom in and out on the plot but has no control over the starting stopping or other aspects of the data To view the data after a run has completed the user must download the data to the computer using the File Manager and can then open the data using Data Review b Spectra Graph This graph shows a single scan from the last downloaded scan Like the TIC graph the user can zoom in and out on the data but has no control of starting stopping or other aspects of the data To view the data after a run has completed the user must download the data to the computer using the File Manager and can then open the data using Data Review c Data Logger The data logger is used to log selected reading from the instrument d The following image shows the Real Time Plots button bar CAE Enable disable data logging AlB JBF Write Logging Data To File Figure 5 84 Real Time Plots button bar e To use the Data Logger feature it needs to be enabled To turn on logging right click on the Data Logger window and select logging then select Enabled or click the Enable disable data logging button on the button bar The following image shows the popup menu that is used to enable or disable data logging Logging Edit Data Logger It
160. r formula 152 Necessary 106 netCDF File 116 New Method 92 93 96 New Method Name 94 NIST 82 86 110 124 139 140 141 150 154 169 NIST 08 82 169 Overlay 143 Overlay Files 124 127 130 parameters 1 5 58 174 176 177 178 179 225 229 password button 68 69 70 Performance Validation 94 109 110 111 112 114 146 183 186 187 188 189 192 193 194 195 196 197 198 230 231 post run results table 47 Power 228 power button 223 previous results 52 Print Chart 117 Procedure button 53 Rate 184 RAW 85 115 116 147 Reconstructed lon Chromatogram 119 124 Remote Files 96 Remove the ion trap RF module 206 Rename Method 93 96 reset button 182 restart procedure 52 Retention Index 103 110 111 150 152 Retention Time Calibrations tab 101 102 Retention Time Calibrations table 110 111 RF 6 199 207 208 209 213 214 215 216 217 218 219 220 RIC 86 119 124 125 126 127 142 RIC chart 126 RIC lons 125 RIC Reconstructed lon Chromatogram 142 Save Method 92 93 94 SD card 174 182 Send a Method to an Instrument 98 Send and activate 98 165 Send Mass Spec Settings To instrument 145 Send Method to Instrument 93 Septum replacement 222 set date time button 67 settings 62 66 67 68 69 70 174 176 179 184 186 190 195 229 Spectra Graph 158 split screen 45 split splitless injection 55 SPME 1 2 3 8
161. r will not be used when line power is connected With the correct adapters the power supply can be connected to external power from 100 250 volts 50 60 Hz AC The following figure shows the power supply connected to the back of the instrument 113 OTHER OPERATIONS Figure 6 3 External power supply connected to the TRIDION Changing the carrier gas cartridge The standard helium carrier gas cartridge for the TRIDION will provide carrier gas for as many as 300 runs at 25 psi 175 kPa operating pressure 1 Turn the TRIDION instrument off 2 Using the cartridge tool remove the old helium cartridge by unscrewing it counter clockwise 3 Attach the new helium cartridge tightly by hand by screwing it in clockwise Operating with an alternate carrier gas source 1 For stationary non portable operation an alternate external carrier gas supply line can be connected to the back of the TRIDION 2 Ifahelium cartridge is attached to the instrument an external helium cylinder may also be attached to the instrument at the same time The internal pressure of the helium cartridge is regulated to 65 7 PSI As long as the external helium cylinder has a pressure of 80 PSI or greater the helium in an attached cartridge will be preserved and can be used after disconnecting from the external helium source 3 The external helium fitting that connects to the TRIDION is a quick connection type of fitting that attaches to 1 16 PEEK tubing
162. rary This option allows the user to export a library to a file This library can then be loaded onto the instrument and can be used for unknown searches in the CHROMION software See the instructions in this manual for the Target List Deconvolution Parameters tab for how to use the exported library files g Import Library This option allows the user to import a library file This can be used to import libraries that are exported from the NIST data base or that have been previously exported from the CHROMION software h Export Selected Compound to Current Target List The option immediately exports the currently highlighted compound to the currently open Target List To undo this action open the Target List and delete the compound that was just added i Add Compound This option opens a default library that contains a list of compounds The user can select any of these compounds by highlighting them in the list and clicking the Add Compound button The filtering options can be used to sort the default compound list To select multiple compounds click on the name of a compound then press and hold down the shift key then click the name of the bottom compound that is to be selected Then click the Add Compound button to move the compounds into the currently open library Alternatively hold down the control key and click on the compounds to be added Once the compounds have been highlighted click on the Add Compound button to add the selected compounds
163. rce MaximumlonizationChange 100 None None Factor MassSpectrometer lonSource MeanBound 0 63 MassSpectrometer lonSource FullWidthHalfMax 0 5 MassSpectrometer MassAnalyzer HardSolventDelay MassSpectrometer MassAnalyzer AmplitudeAVoltage MassSpectrometer MassAnalyzer AmplitudeAVoltage MassSpectrometer MassAnalyzer StepAVoltage MassSpectrometer MassAnalyzer StepBVoltage MassSpectrometer MassAnalyzer RampMaxVoltage CoolTime 0 12 30 72 MassSpectrometer MassAnalyzer Milliseconds MassSpectrometer MassAnalyzer ScanTime 0 12 32 Milliseconds MassSpectrometer TrapHeater Temperature 125 180 Degrees C MassSpectrometer Detector HighVoltageVoltage 1250 Volts 2200 MassSpectrometer Detector HardSolventDelay MassSpectrometer Detector RFPhase Specific DO NOT for each CHANGE trap MassSpectrometer VacuumChamber Helium FlowRate 100 275 Arbitrary Reset the on board computer 1 There is a reset button and an emergency shutdown button on the TRIDION 2 The reset is used to restart the CPU without turning off the system power This is used in cases where the instrument has stopped operating and the user wants to restart the computer without losing vacuum or temperature 3 The emergency shutdown button turns of the system power immediately This would be used if the user notices a situation where they think the system is running away thermally or for any situation 121 LIBRARIES where the user wants the
164. re parts of the Compound Details tab a Compound This field contains the following information i Compound Name ii CAS 98 OTHER OPERATIONS vi vii Formula Molecular formula Retention Index Molecular Weight Group User assigned information for sorting the compounds MSDS This option allows the user to set up a link to an external file The field displays the path to the linked file Right clicking on the field allows the user to add a new link or remove an existing link The field is labeled MSDS but can be linked to any file and will use the Windows configuration to select the program that will be used to try to open the file Compound lon List This is the list of ions for the compound They can be edited by highlighting the field and typing in a new value The user can add or delete an ion by using the right click menu Structure Image This field is used to view an image The image can be any image that is a supported type The supported file types are BMP JPEG GIF and PNG The user can add remove or view a file by using the right click menu 6 Spectrum This is a graphical view of the information that is contained in the Compound Ion List It cannot be edited and is only available for viewing 7 The following image shows the Library Editor button bar with popup labels _ AMDISNISTEPACW ji RAe Oa A asd Select Library AMDISNISTEPACW Jia znv lis BOF LO AMDISNISTEPACW id avis BOP BO
165. rs ce ene oesie a a a a ance A E A O E a 110 K E E 111 6 igre ge o go 0 geen ene cee ee A E E Cn re er men nee 112 POWElSUDIIY and DANGI Y ceea cordeencc eters erect 112 Changing THE DAMS FY emina ae N RE 113 Operating with external POWEL ccccccsececceeceeceesesseeeesseeeesseeesaaeess 113 Changing the Carrier gas cartridge ccccccsesceeeeeceeeeeeeaeeeseeeeeeaees 114 Operating with an alternate Carrier GAS SOUICE ccceccceeceeeeeeeeeeees 114 Removing replacing the SD Card ccccccccseeceeseeeeeeeeeeseeeeesaeeesaeeeeeas 115 How to bake out the GC injection port and column 00008 115 Advanced ODS AO INS ease se ects Soh See iE R sere Hotere E EEA 117 Accessing the Advanced screen on the TRIDION cccceeee eee 117 Viewing current calibration points and operating parameters 118 Viewing calibration points and operating parameters on TRIDION screen 118 Viewing calibration points and operating parameters by retrieving the method file FrOM the INSTTUMENT corir a a a 118 Loading operational settings onto the TRIDION ceeeeee 118 Check or monitor the operating parameters during a run 000 119 Recommended Operating Parameters cccccccccccsseceeeseeeeseeeeeeseeeeeessaees 120 Reset the On board COMPUTEL ccceccceecceeeeceeeceeeeeeeeseeesaeeeaeeesaees 121 Delete all sample data from the SD Car
166. run The following image shows the screen that is displayed when the Split Screen option is selected from the run screen 27 INSTRUMENT OPERATION 10 11 Taraet4E Torion Technologie 20sample04 2012 04 1 4 Sample 35000 0 28000 0 21000 0 14000 0 7000 0 0 0 105 4 M 0 0 ai he 42 1 63 2 84 3 i Plot View Stop Run Figure 4 26 Screen shown during a run using the Split Screen With the Split Screen option selected during a run the total ion chromatogram TIC is plotted at the top of the screen and the mass spectra are shown on the bottom plot The spectra plot shows the most recently collected spectra unless the cursor is positioned at a specific scan location earlier in the TIC plot In that case the spectra displayed in the spectra window correspond to the selected scan in the TIC plot Selecting the Plot View option will return the screen to displaying chromatographic data only Selecting the Stop Run button stops the analysis and the screen changes to an intermediate screen The intermediate screen is shown at the end of any run while they system is returning to a ready state The intermediate screen is described later in the chapter The Diagnostics button opens the Status Diagnostics screens that are described later in this chapter On the touch screen data the user can drag a square around a section to zoom in on The following image shows the screen as a square is being dragged around a section to zoom
167. s 63 WA OU LSI estates E EEE E E A E E 64 Farget WES UO Seeria a N 64 Farget HSE Ta Daen aa tues a A tus 65 Deconvolution Parameters Tab cccccceccsseceeeseeseeeeeeeeeteeeeeeseeseeeeaess 66 Target Bit SCAUC I reneo tyneshar csi deeundabadeidcs eapdedah adhtadsedsaeisbu cetacean ceeeleeces 66 Unkown IGENTINCATON zurira aera acetate weak OTE 67 Penormance Valdai ciesaivsesesenssuseseanoenevosdasnesonsnesensestionnweatimanneamegaaiedes 68 TOO ae E A A 71 Overview or Data THEVICW anona vondiastanciosade a a asad eniawed eitvaeiaaelaamiaanes 71 Data Review Button Bafr sessesesesesseseseseseesesesesesseseseseesesesesesseseseseesesesesesseseseseseeseseseseesese 73 Detail on Use of Data Review Functions ccccccceecceceeeceeeeeeeesaeeeeessaneees 80 RIC Reconstructed lon Chromatogram ssesesessssesessesesessesesessesesessesesessesesessesesess 80 Overlay Files erone 82 IDECOMVOIMEOM art cai ae eon A 84 NIST S al Ch pciiini a EOAR 89 EOIN Chalte eenaa a E O tadastdcavudesiabiasniteeaastedees 91 MASS Spectrometer veccecnccdsanceevesuuwrncossenntsedevaucedausaevedenateqaebvantvedieanceareneweseenss 92 File MANAG Cl correu bananas Ges iuestb ia tenaddsstamsatea mess hts unas stun tidaeniet tumdceltiniasns 95 HDAV EONO Gamemn ee mm nee creer re etree rsn ae eter ttn mre ae a ect mt 97 RealTime PIOl Siccasecaenicetsdetadananet e 102 Toning VV ZN serseri a add tontiateinencatmbanisteies 106 MING WCW GM ocean ce
168. s on adsorption to extraction and desorption from injection the SPME fiber Adsorption depends on the partition coefficient of the target chemical between the fiber coating and the sample matrix Detection also depends on the volatility and molecular mass of the target chemical 45 500 amu Sample headspace vapors from liquid or solid samples Place the liquid or solid sample into a vial Leave sufficient volume headspace above the sample for Sampling vapors when the SPME fiber is fully extended from the CUSTODION syringe needle 1 Cap the vial with a septum cap BASIC OPERATIONS 2 Insert the CUSTODION needle through the sample vial septum Caution Be certain that the SPME fiber is retracted inside the CUSTODION needle i e protective needle CAUTION before piercing it through the sample vial septum Caution Be careful not to bend the flexible SPME needle when piercing the septum CAUTION Caution Try to keep the CUSTODION syringe needle above the surface of the sample to prevent uptake of CAUTION liquid onto the SPME fiber by capillary action 3 Depress the CUSTODION plunger to extend the fiber into the headspace sample Note Depress the plunger until you hear or feel a click and then release the plunger 4 After the desired extraction time depress the plunger to retract the fiber into the syringe needle 5 Remove the CUSTODION syringe needle from the sample vial Caution Be certain that the SP
169. s primarily of a fused silica or metal rod that is approximately one centimeter in length and a tenth of a millimeter in diameter The rod is typically coated with a polymeric material called a sorbent The rod and sorbent together are referred to as the SPME fiber The chemical properties of the sorbent determine the classes of compounds that selectively absorb or adsorb onto the fiber Solvents should not absorb preferentially over target chemicals otherwise a different sorbent or solvent may be necessary 1 The SPME fiber is stored inside a protective needle called the SPME needle The fiber is extended out of the SPME needle during the extraction and desorption of a sample The SPME needle is connected to a spring loaded plunger that extends and retracts the fiber The complete apparatus is called the SPME syringe 2 Each chemical is extracted into the SPME coating according to its equilibrium distribution between the coating on the fiber and the liquid or gas phase around the fiber This equilibrium depends on the chemical nature of the polymeric phase the solvent the temperature and the volume of both the polymeric phase and the solvent Extraction can take under a minute depending on sample volume and concentration Equilibration of the fiber with its surrounding matrix usually requires a longer period of time several minutes to several hours After equilibrium has been achieved the concentrations of target chemicals on the fiber and in th
170. se poor analytical results or hardware failure if changed during an analytical run 4 Turn on the TRIDION 5 Using CHROMION software attach to an instrument 118 LIBRARIES 6 Open the Mass Spectrometer screen under the Tools section 7 Ifthe instrument is attached the settings table will already be populated 8 Adjust the setting that needs to be changed and select the send button at the top of the screen Refer to the software chapter for details about the Mass Spectrometer screen Check or monitor the operating parameters during a run The user may open Advanced mode and check or monitor the actual voltages currents temperatures and other settings at any time 1 Turn onthe TRIDION 2 Open the Advanced screen see the section called Advanced screens in the Instrument Operation chapter of this manual 3 Select the Status Diagnostics button 4 Select any of the tabs on the screen to view the parameters Ve Sled Torion B Vi versions Gas Chromatography Mass Spectrometry Status Edit GUI Version 1 0 0 4132 1 Analog PCB Rev Analog PCB DAO PCB Rev DAQ PCB GC PCB Rev GC PCB RF PCB Rev Power PCB Power PCB Rev RF PCB Battery PCB Rev Figure 7 2 Status Diagnostics screen sowing the Versions tab 119 LIBRARIES Recommended Operating Parameters Table 7 1 Recommended Operating Parameters Major Group Name Value T F Min Unit Max Control SolventDelay
171. section Of the spectra WINdOW sssessseseseesseessersseessseosseosseosssesseesseessseossees 30 Figure 4 32 Screen Showing the ZOOM out FUNCTION csssssssssecscsssecscsssecscsssssecsssssecsssssecssscsecssassecssscsecscsssecucaesesscasseescnsssescess 31 Figure 4 33 Current procedure has Ended SCreeN ssssscsssssscscsssscscsssscscsssssscssscsscsssssscussssecscsesecscsesecsescsecscsesecscseseescacseescnessencees 31 VU SS PV AC eases eia RE a 32 Figure 4 35 Version tab of the status diagnostics SCFEON ccsssssscscsssscscssscscssscsscssscsscessesscscscsecscsesecsesesecscsesecscsesscucsessecasssescess 33 Figure 4 36 Gas Chromatography tab of the Status Diagnostics screen sssssscessssscecscsssscsssssecsescsececsssscesscsssecsssseseacssescees 33 Figure 4 37 Mass Spectrometer tab of Status Diagnostics screen ssscsssssscscsssssecscsssecssssseccseseseesesecscscsscscsesssscsessecssssescecs 34 Figure 4 38 Status tab of the Status DiagGnOstics SCrEON csssecscsssscscssscscssscsssssssesssesscssscsecsssssecscscsecscsssecscsesesscasssescesasencees 34 Figure 4 39 Edit tab of the Status DiagQnoOstics screen sssssscsssssecscscsscscssssscsssssscscsesscsssesecsesesecscsesecsssesecussesecucsesseucseseencasssescees 35 Figure 4 40 Enter Password SClee ivisccsssccccscsecasacesesecceccessccessseccccasccesasesacasecssusessesasaceussacsesasesesesacassescsesesassdcasoscsasecasscsascsssecedsosacegieesaece 35 Figure 4 41 Screen that is displa
172. ser may choose a different folder for run data to be stored in To change the data storage folder touch the drop down arrow in the Folder field and highlight the desired folder Sample Concentration 1 6 When the instrument is being run the split flow settings in the GC method are used automatically Occasionally users may come across samples with very low concentrations to very high concentrations where the split flow should change but the user does not want to restart the SOP in order to change the method In this case the user may choose an appropriate sample concentration which will change the split flow without interrupting the SOP From the home screen as shown in the above image a user would choose the following Sample Concentrations to have the following effect on the Split Flow High opens both the 10 ml and 50 ml split valves Med opens the 10 ml and closes the 50 ml split valves Low closes both the 10 ml and 50 ml split valves Method follows the activated GC method settings Choose Start Run to begin the run Once the user chooses Start Run the screens prompt the user to perform an injection as shown previously in this section The injection screens are the same as when running a performance validation The following image shows the screen that is displayed during a sample run Target4E t Torion Te 20sample03 2012 04 1 3 Sample a _ a Split Screen Figure 4 25 Screen shown during a sample
173. ses table can be opened and edited Overlay Files 1 Select Overlay File List This opens a dialog box that allows the user to select files that will be displayed in the overlay files graph 2 Selecting the Overlay Files button opens the following window ti prea Date 3 2 2072 14849 AM 0 z E E O E Figure 5 56 Data File Overlay Setup table 82 OTHER OPERATIONS 10 11 This window allows the user to choose which data files to overlay Overlaying data files allows the user to view the data in a way that the user can see subtle differences between two or more data files The Enable check box allows the user to turn off and on the visibility of a data file in the overlay view window without removing it from the file list The Edit button allows the user to select a single data file to include in the overlay view window The first line in the table shows the path and name of the currently open data file Another file can be added by clicking the Edit button The Windows open file dialog box will open and the user can then navigate to the location of the data file they want to view in the overlay screen After selecting the file click the open button to add the file to the list The Multi Select button opens the following window Look ir My Recent Documents Desktop 5 My Documents E caf E cosoooKo cDF E co6009QL0 cDF E cosongmo cE
174. sessessessesseoseoseoseeseessensesseoseoseoseoseosroseoseosseseesressesresseoseoseoseoseoseoseoseeseeseess 57 Figure 5 14 Method successfully saved dialog bOX ssesssessesssesseessesseesseossesseessesseesseoseesseoseesseoseesseoseeoseenseoseesseoseesseoseesseossessees 58 Figure 5 15 Save As dialog bOX Cree ttt ee eer tT 58 Figure 5 16 Rename Method dialog DOX esac ccc seca ccc cececceccescerccescurcceseuccseseucesescuveseacureseaaurastacqraseasqcaseaaqcasestqcansacqeaneatqcesessnceree 59 Figure 5 17 Export Method file location dialog DOX sesssssssssesesscscsssssssscscscscsssssscecsesssssssessesessassesesecsesesssesesecseseassesesesseaeass 59 Figure 5 18 Method successfully exported to a file dialog s ssesssesseessesssesseossesseessesseesseoseesseoseesseosesseesesseesseoseesseoseesseoseessees 59 Figure 5 19 Send Method dialog BOX ssssessssssscsssssscscsesscscsssscscsssscscsssesscsssecscssacsscsesesecscsesecscsesesuesesecscsesesscseseeucsesesscseseeucaesseacecs 60 Figure 5 20 Method successfully sent and activated dialog DOX ss sssesssessesssesseessesseessesseesseoseesseoseesseessesseesseoseesseoseesseoseessees 60 Figure 5 21 You are not connected to an instrument dialog bOX ssesssessesssesseessesseessesssesseossesscossesseesseoseesseoseesscossesseossessees 60 Fiore S 22 Method BULON Ba sieaa EE a a et tta i EAA 61 Figure 5 23 Gas Chromatograph button bar with descriptions s sssesesesssessseesseesssessseosseosseesee
175. sscucncncscscsenessncsensnsnscsasasavasasasasasascscsesesescsesesenenenededsasasdsacasasncncncecacacacsssssesses 112 Figure 6 2 Empty battery compartMent sssesssessesssesseessesssesseossesseossesscesseoseesseoserescossesseosresscesseoseesseoseesstosersseossesseesseoseesseoseesseess 113 Figure 6 3 External power supply connected to the TRIDION uu ssssesesscsssssssesecscscsssssesecscsescsssesecscsesesesesesscscscsesesecsescess 114 Figure 6 4 a o7 e qe ai aicil a6 na ai allimmerrererer spre perreeeresreverereeererecereercerrerrce reerrer errr et reveret reerretreereey rerreryrerertrctrrrrrrtrrvererreveret RRS 115 Figure 7 1 Advanced SCLEEN csesscssssssesscscsssssssesscscscsssssescsescassesesscsessassesesscseseassesesscsessacsssesscsessassesecscseseacassesscseseasaesesscseseaeaesesecseseass 117 Figure 7 2 Status DiagnoOstics screen SOWING the Versions tab sesessesssesseessesssessesssesscessesseesseoseesseoseesseosseoseesseoseesseoseesseess 119 Figure 7 3 Reset and emergency shutdown buttons e essessessessesseseoseeseeseessessesseoseosesseoseoseoseoseesreneesseoseoseoseosesseoseoseoseeseeseese 122 Figure 7 4 Chromatogram of the CALION Performance Validation MiX sss sesesssessseesssesssessseosseesseesseesseroseeosseosseesseesseesss 123 Figure 7 5 Uncalibrated bin data for bromoform masses 171 173 and 175 ss sssessesssesseessesseessesseesseossesseossesseesseoseessesss 124 Figure 7 6 Calibrated mass data for bromoform mass
176. sseroseeosseosseosseeseesseesserssseossees 61 Foure 5 24 Gas Chromatograph COMUNON escccescsedcccescecescctscessscecccscescedssesccicceicciccesc sscesensscesessocescerocescezece ceetexecestexecesccnecesccnecesssissiiceiced 62 Figure 5 25 Gas Chromatograph Retention Time Calibration sssscsssssscecsssscscsssssscsssssecsssssecsssssecessssecssesscecssssccesseescees 63 Figure 5 26 Target List buttons with CAPTIONS ee ssssssececsstcsesesececscecscscsesecscscsssescsesscscsesescsesecscassescsecscscseaesesececseaesescsesecneacacees 64 aeee TEE e E AEEA AET 65 Figure 5 28 Deconvolution Parameters SCreen ssessseeseseseseesseesserssersseeosseosseesseesseesserssseosseosseosseesseeoseroserosseosseosseesseesseroserosseossees 67 Figure 5 29Peilormance Validation Wilh COW ssscsesccecseecesesexeescseecevenccseveocsctvencsctcosss2e ccarscecesrace A 68 Figure 5 30 Performance Validation screen showing an error in data entry ssesssesseessesseesseoseesseessesseessesseesseoseesseoseessees 69 Figure 5 31 Performance Validation Remove Compound dialog DOX s sssesssessseesssesssessseosseesseesseesseessseosseosseoseesseesseesssesssees 69 Figure 5 32 Performance Validation showing Masses for lt BromoforM gt e sssessssesssesssessseesseessersserosseosseosseouseesseesseessseossees 70 Figure 5 33 Performance Validation screen showing an error in data entry ssesssesseessesseesseoseesseessesseesseoseesseoseesseoseessees 71 Figure 5 34 Performance Va
177. ssesseossesscossesseosseoseosscoseesscossesscosreoseosseoseesscossesscoseesscoseesseoseessees 93 Figure 5 73 Open Mass Spec Settings dialog bOX essessessesseoseoseoseosrosrosresresresseoseoseoseossosrosrosresresreoreoreoseoseoseoseossosresresresresress 93 Figure 5 74 Save Mass Spec Settings As dialog DOX ssesssesseessesseessesseesseossesseensesseeseoseeseoseeoseosresseossesseesesseesseoseesseoseesseoseessees 94 FPOe a Fe IVa AO ear R RE 95 Figure 5 76 File Manager Create Directory and Rename Directory dialog DOX ssessessessesseeseeseeseessessessessesseoseoseoseeseeseess 96 Figure 5 77 Library Editor Library Contents taD vescscocscecececesessecceacececscseveesseseseseeesescsesasacataseseseseneseececececscscsccucatesesesesecescscccccscsesesteess 97 Figure 5 78 Library Editor Compound Details tab uu sssssssssscscsesecscsssssscscsesscsesesscecsesecsesesecucsesecucsesecscsesecscsesesucseseescasseencees 98 Figure 5 79 Library Editor button bar with Compound Details tab Open ss sssessssesssesssessseesseessersseroseeosseosseeuseesseesseessseossess 99 Figure 5 80 Library Editor button bar with the Compound Details tab open s sssssesssessesssesseessesseesseossesseessesseesseoseesseoss 101 Figure 5 81 Link MSDS file location dialog sxcsececscesececsestscescstasccesceccceecececescascccscanaecseuteaeseuececccueceesccucaeecescaencescqensescesuecseasaseceuececeueeadsen 101 Figure 5 82 Library Editor Add Compound Image dialog DOK esessss
178. ssscscsssecscessseccscsssscsesscscssseccsesecscsesesscsesesecseaseecseaes 102 Poe S o R NNE PO a eA 102 Figure 5 84 Real Time Plots button bafr sssessssesssesssessseesseesseessseosseosseesseesseesseesssrosseossceussesserssseosseosseosseesseesseroseroserosseosseesseresersss 103 Figure 5 85 Enable Data Logger dialog BOX ssssssscsssssssssssssssssssssssssssssssssssssssssssssesesesesesescscscscscscscscscscscseacseseacacaeacacacacacasecs 103 Figure 5 86 Real Time Plots Data Logger Items dialog bOX ssessessessesseseessessessessessesseoseoseoseeseeseeneessesseoseoseoseoseoseoseoseoseeseesse 105 Figure 5 87 Tuning Wizard screen sesesssessseesseesssessressseesseesseesseeosseosreosseesseesssesseeossrosseosseeesseoserosseossrosseosseesseesseeoserosseosseosseessereseesss 106 Foure 5 33 Tunng Wizard DUTON Dai ersa 107 Figure 5 89 Tuning Wizard open performance validation INI file dialog DOX s ssesssesssesseessesseessesseesseossesseonsesseesseoseessesss 107 Figure 5 90 Tuning Wizard showing a system that has passed all tests ssssssesssessesssesseessesseesseoseesseossesseesseoseesseoseesseess 108 Figure 5 91 TightVNC viewer installation showing selection of Viewer Only option s ssssesssesssesseesseesssessseosseesseesseesss 110 Figure 5 92 Dialog box that opens when running TightVNC ViEWET cccsssssesesessccsssssesesscsssssssesecsesssssssssecseseassssesecsescees 111 Figure 6 1 TRIDION battery indicator lights sccscscsccscussss
179. system blank b Run a performance validation c Run Samples up to 20 samples 2 Once an SOP has finished it starts from the beginning 3 If users want to create a different SOP they need contact Torion Technologies Status bar 1 The top section of most screens on the instrument is the status bar 2 The status bar contains three icons in the upper right hand corner The image below shows the status bar displayed i Target4E BB Torion Technologies 1 SystemBlank Data File Location Folder 2012 04 11 File Name 20sample01 2012 04 11 08 07 33 N Sample Concentration O High Medium O Low Method Advanced Start Run Previous Results Figure 4 4 Status bar displayed at the top of the screen 3 The icon furthest to the right displays whether the instrument is ready to perform a run The instrument is ready to run when a green circle with a check mark inside is displayed 4 The icon in the middle displays the of helium left in the helium cartridge If the instrument is attached to laboratory helium the icon will display that the cartridge is empty or have a value of 1 5 The icon on the left displays the amount of battery power left or if the instrument is plugged into AC power 6 To view the status of the instrument choose any of the icons in the upper right hand corner of the screen and an expanded view of the instrument status will appear as shown in the image below 16 INSTRUMENT OPERATION
180. tch Faces Edge of Board Figure 8 19 Trap orientation on RF board 2 Position the trap assembly so that the notches in the electrodes face away from the RF coil and toward the edge of the board 3 Install the trap mounting screws Tighten them snuggly but do not over tighten the screws Trap final reassembly 1 Install the EGUN mount Use the following image to orient the EGUN mount on the trap EGUN Mount Screws Einsel Lens Pin Top End Cap Electrode Wire and EGUN Mount Screw Figure 8 20 EGUN mount orientation 2 One of the screws on the EGUN mount is also used to hold the Top End Cap Electrode Wire 145 SERVICE 3 Install the other two screws first then install the screw with the Top End Cap Electrode Wire Slide the Top End Cap Electrode Wire onto the connector on the RF board 4 Slide the Red and Black Filament wires onto the connectors on the RF board Install the black wire onto the FIL pin and the red wire onto the FIL pin 5 Use the 1 8 hex nut driver to make sure the nuts on top of the filament are still tight 6 Slide the RTD wires onto the pins on the RF board 7 Connect the white RTD wire onto the RTD pin and the black RTD wire onto the RTD pin 8 Connect the heater wires to the heater connections on the RF board The labels show HTR and HTR These labels are for convenience in trouble shooting There is no plus or minus orientation for the heater Connect one of the heater wires to the H
181. tery 8 57 170 171 172 blank 10 126 174 CALION 183 184 186 187 191 192 193 carrier gas cartridge 8 172 CAS 150 151 CDF 85 115 116 117 147 change the system password 68 CHROMION 82 83 84 87 88 89 90 91 95 108 126 130 154 168 169 174 177 178 184 186 187 191 194 195 CHROMION G8 82 CHROMION AP 130 142 187 191 195 Compound Details 151 153 154 155 Compound lon List 152 Compound Name 107 150 151 continue button 25 26 193 control software 52 54 CSV 115 143 162 Current calibration 177 Currently Loaded Method On Instrument 95 CUSTODION 1 3 10 11 12 13 18 225 Data Logger 158 159 161 Data Review 84 85 86 115 116 117 118 122 123 124 158 187 188 191 date time field 67 Deconvolution Control Center 130 131 133 134 135 136 137 139 Deconvolution Parameters 105 107 108 131 136 154 Deconvolution Spectra 121 139 Detector 58 detector voltage 226 227 229 Detector Voltage 58 Diagnostics 179 180 223 227 diagnostics button 45 53 177 179 Diff 143 edit tab 57 Einsel lens cleaning procedure 216 Electron multiplier detector replacement 218 164 emergency shutdown button 182 Evaluate the masses 191 Export Charts 141 142 Export GC Settings to File 101 Export Method 93 97 external helium 173 174 external power 223 External power 172 Filament 58 199 216 Filament Current
182. the other graphs the cursor still functions in the zoom mode To select an area use the mouse to drag a box over the area of the TIC you want to sum A yellow box will be visible on the TIC Each mass associated with the scans in the highlighted area will be added together and can be displayed by opening the Summed graph To clear the selected region place the cursor in the yellow highlighted area by clicking on the area with the mouse Then click the right mouse button to open the right click menu Then select Clear Region and choose either Under Cursor Summed or All option to clear the selected area The Under Cursor option only clears the region where the cursor line is located If the cursor is not in a highlighted region than choosing the Under Cursor option will not have any effect The Summed option will clear all of the yellow Summed regions but will leave the blue Background regions The All option clears all selections regardless of type The following image shows the right mouse click dialog box with the Clear Region menu expanded Cursor Mode gt er Cs Show Points Summed Peak 9 All Print Chart Figure 5 50 Data Review right click dialog with Clear Region menu expanded a Background Select When the cursor is set to this mode it is only functional in the TIC In all of the other graphs the cursor still functions in the zoom mode To select an area use the mouse to drag a box over the area of the TIC you want as backgrou
183. thod to Instrument button 133 SERVICE 8 Service This chapterdescribes how to perform certain service operations on the TRIDION Trap service tools and materials 1 The following table contains a listing of the tools provide in the instrument tool bag Not all of these tools provided are used for cleaning the trap but all of the tools needed are part of the tool kit Table 9 1 Tool list and descriptions Part Number Ss Tool Description 4340 0058 Gauge DOWEL PIN 0 0580 OD X 2 L SST EGUN alignment tool 6420 0056 5 64 Hex driver 2 for trap screws 6420 0060 Flat head screwdriver 0 078 wide blade RF tuning 6420 0064 3 32 Hex driver 4 GC screws 6420 0068 7 64 x 50 hex driver 6 Vacuum cap screws 6420 0080 3 16 open end wrench 4 nuts for trap electr standoffs 6420 0081 1 8 nut driver 0 nut for filament nuts 6420 0094 1 4 and 5 16 open end wrench for PEEK tubing nuts 6420 0095 5 32 nut driver 2 for EGUN nuts 6420 0096 T10 TORX driver 3 16 blade diameter for white RF board cover 6450 0018 Tweezers 7 Curve Filament C clip 2 The materials tools and working surface should be thoroughly cleaned to remove any contaminants Any user that will be handling any parts internal to the vacuum chamber needs to be wearing lint free laboratory gloves O ring Handling Cleaning Installation and Removal 1 Tools and Supplies a Dust of
184. tion called GC baseline is noisy or drifts upwards or may be caused by the problems discussed in this section 156 TROUBLESHOOTING 2 Mass spectral noise may be the result of poor noise filtering or chemical contamination that convolutes the spectra 3 Noisy spectra can result from an incorrect detector voltage higher detector voltage increases sensitivity it also increases random noise The electron gun current may also be too high producing too many ions for the trap see the section called Recommended Operating Parameters 4 Noisy spectra can result from an old or faulty detector see the section called Electron multiplier detector replacement 5 Noisy spectra can result from a dirty ion trap see the section called Trap maintenance procedures on removing and cleaning the trap 6 Noisy spectra can result from impure carrier gas Replace the gas cartridge with a new cartridge or external gas line and follow the instructions in Bake out the GC injection port and column Note Noisy spectra may be improved with the noise filters included as instrument parameters Results are not reproducible 1 Results may be irreproducible when the operating parameters are outside the suggested ranges see the section called Recommended Operating Parameters or when the components are dirty or faulty Some suspected parameters include detector voltage electron gun current column and injector settings The suspected components may incl
185. to send message continues to appear restart the instrument and reestablish communication If the fill cannot be sent contact Torion for assistance 8 If there is no instrument connected the following dialog box will appear If this happens check your instrument connections Connect First Figure 5 21 You are not connected to an instrument dialog box 60 OTHER OPERATIONS 9 All of the functions of the Method menu are also available on the button bar that is located above the expanded navigation menu on the left side of the screen The following shows the button bar with the text for each of the buttons Figure 5 22 Method Button Bar 10 Clicking on a button activates the exact same activity at those described above Gas Chromatograph Gas Chromatograph Buttons 1 The following shows an image of the Gas Chromatograph buttons with pop up descriptions MB GE he Refresh AutoCalibration Data roce Copy AutoCalibration Data to Manual Calibration Data F FaoE IE IES Import GC Settings from File D B Export GC Settings to File Figure 5 23 Gas Chromatograph button bar with descriptions 2 Refresh AutoCalibration Data Clicking this button reads the auto calibration information for the retention times from an attached instrument It is used when the user suspects that the retention information has changed on an instrument after a method was last used and the user wants the method to reflect the changes 3 Copy Au
186. toCalibration Data to Manual Calibration Data This function allows the user to run an auto calibration run then if they want to make changes manually they can copy the auto calibration data to the manual calibration table and modify the information This button is only available in the Retention Time Calibrations tab 4 Import GC Settings from File This allows the user to import GC settings that have been exported from another method This button is only available in the Retention Time Calibrations tab 61 OTHER OPERATIONS 5 Export GC Settings to File This allows the user to export GC settings to a file so they can be imported into another method file GC Parameters tab 1 When an instrument is attached the settings for Gas Chromatograph are displayed as in the screen below GC Parameters Retention Time Calibrations Heaters and Pressure Injector 270 270 C Transfer line 270 250 C Column Begin temperature 50 a Begin hold time 10 Seconds End temperature 270 aC End hold time 60 Seconds 10 1 split on 0 Seconds 10 1 split off 0 Seconds 50 1 split on 0 Seconds 50 1 split off 60 Seconds Figure 5 24 Gas Chromatograph control 2 The Heaters section displays the set points for the gas chromatograph a Injector The temperature is normally set to 270 C The maximum temperature is 300 C b Transfer Line The temperature is normally set to 270 C The m
187. ton allows the user to give the settings table a new name The following image shows the dialog box aH Save Mass Spec Settings As Figure 5 74 Save Mass Spec Settings as dialog box d Delete Current Mass Spec Settings This button deletes the open settings table If the current table is the one that is on the instrument this option will not be available e Send Mass Spec Settings To instrument This will send the currently displayed settings to the instrument This action is immediate and cannot be undone Most of the settings will take immediate affect even if the instrument is performing an analysis This can useful for diagnostic purposes but as described in the previous caution sending parameters without understanding what they do can cause damage to the instrument 6 The only settings that normally need to be adjusted are the following a Hard Solvent Delay The hard solvent delay allows the user to turn off the mass spectrometer until a large solvent peak has eluted from the column This helps keep the instrument clean and keeps the visual scale of the peaks reasonable during the analysis To turn on the hard solvent delay find the following settings In the group MassSpectrometer find the Subgroup lonSource HardSolventDelay is the first choice Enter the time that the filament will be left off at the start of the run Typically 5 to 10 seconds Next find the Subgroup MassAnalyzer HardSolventDelay is the first item Enter the s
188. trometry MS is to measure the presence and abundance of a chemical s characteristic ion fragments according to the values of their mass to charge ratios m z MS involves several steps to generate a mass spectrum of a chemical ionization mass analysis and detection 2 lonization is necessary for producing electrically charged fragments i e ions A plot of the abundances of ions produced from a chemical as a function of m z is called a mass spectrum Each chemical has a characteristic mass spectrum that can be used as a chemical fingerprint to identify the chemical and differentiate it from other chemicals Soft ionization methods primarily produce 4 TUTORIAL detector signal molecular ions or ions related to the molecular ion e g abstraction of hydrogen or addition of hydrogen or other species Hard ionization processes yield fragments of the chemicals i FALA Riu bet j aT A L A d i aN el E Tf fT 20 an 60 20 jon 120 44006180 618006 200 720 240 260 2 0 J00 770 3O JESO JSO 400 420 44o 460 6480 S00 m z Figure 2 3 Mass spectrum obtained by the TRIDION showing the mass to charge m z of ionized fragments of diethyl phthalate Electron ionization is a hard ionization method in which the sample intersects an energetic e g 70 eV beam of electrons that are drawn from a current carrying filament The interaction of the chemicals in the sample and the electrons in the electron beam creates charged fragments The
189. ude the column injector port ion trap or the SPME syringe or fiber The sampling technique is also critical for reproducibility The following list provides possible solutions for correcting irreproducibility a Re extract and analyze the sample with a new SPME fiber or after cleaning the SPME fiber see the section called Prepare the CUSTODION SPME syringe for sampling b Allow the instrument to warm up for several minutes before analyzing a set of samples c Runa standard and verify that the mass spectrometer and chemical library calibrations are still good make adjustments as necessary and re filter the irreproducible data with the new calibrations d Evaluate the extraction procedure and eliminate any variations such as inconsistent extraction time temperature or agitation procedure There is no instrument signal 1 Lack of signal is typically observed when the electron gun filament burns out or when the detector malfunctions or needs replacement The signal will either be absent or appear as a baseline When this happens the instrument may be sent to Torion Technologies or the user may replace the filament or detector by following the instructions in the Service chapter 157 TROUBLESHOOTING Acquired mass spectra are not correct There are a few different things that may cause the acquired mass spectra to be incorrect For troubleshooting follow the steps below l 4 Perform 3 analytical runs using the CALION Sta
190. unds being analyzed Usually the temperature of the column is increased during an analysis to reduce the time of the analysis This is typically done with the capillary column installed in a convectively heated GC oven 4 The degree of separation of two chemicals that exit the capillary column at the detector is called resolution Two chromatographic peaks are completely resolved when the baseline signal is present between them otherwise they are only partially resolved Adequate resolution between peaks is necessary to allow the use of retention times for tentative chemical identification and to produce sufficiently accurate mass spectral fingerprints for positive identification Peaks with similar retention times may be resolved by reducing their peak widths or by changing their relative retention times 5 Low thermal mass LTM GC refers to a miniaturized form of GC in which the convectively heated column oven is replaced with direct electrical resistive heating of the capillary column LTM GC uses a conventional GC column that is intertwined with resistive heating and temperature sensing wires and wrapped with aluminum foil for greater heating efficiency The low thermal mass of this column heating arrangement allows for much smaller instrumentation and lower operating power as well as faster heating and cooling of the column The GC in the TRIDION is an LTM GC What is toroidal ion trap mass spectrometry TMS 1 The purpose of mass spec
191. uring normal use 1 Change the following parameters to 300 C Injector Temp Transfer Line Temp and Column Begin Temp by using the CHROMION software to edit the instrument settings in the Gas Chromatography screen Send and make active the modified method to the instrument 2 Start the standard SOP and run a blank run This will set the temperatures to the elevated setting in the modified method 3 settings to the previous settings and again run a system blank to switch the GC parameters back to normal operating temperatures and ensure that the bake out procedure cleaned the GC properly Caution Verify that the parameters have been restored on the TRIDION by viewing the temperature settings under Advanced gt gt Diagnostics gt gt GC CAUTION 116 LIBRARIES 7 Advanced Operations This chapter explains how to use operations that are intended for expert users These operations allow the user to adjust the way the TRIDION functions Because the TRIDION does have a default setting any changes will erase the previous settings All settings shouldbe savedonacomputer before changes are made Accessing the Advanced screen on the TRIDION 1 The Advanced screen provides access to information about the instrument parameters and the run time voltages and currents 2 The primary purpose of the Advanced screen is used to troubleshoot the instrument by inspecting the voltages currents and other settings during sample ana
192. with the button 5 An alternative option to run the instrument directly from a PC is to use tight VNC viewer Tight VNC viewer is not included with the software but is available for free downloaded from the internet Instructions on how to install and use the viewer are included in the Software chapter of this manual 6 The instrument has a stylus attached to facilitate operation of the touch screen The location of the stylus is shown in the following image Although the flow of this chapter is linear in the way it presents the user interface any of the buttons that appear either blue or green on any screen can be accessed from that screen If they are gray then they are disabled The screens that open are the same regardless of what screen they are accessed from Stylus Nn Utility Cover Touch Screen Display Status Lights __ GC Injection Port Operating Buttons fi Cooling Air Flow Cover Service Cover Figure 4 3 Instrument Parts 15 INSTRUMENT OPERATION Standard Operating Procedures 1 Once the instrument has established vacuum and proper operating temperatures the screen shown below is displayed which is Step 1 of the manufacturers Standard Operating Procedures The instrument functions using Standard Operating Procedures to simplify running the instrument and help prevent user error The TRIDION 9 comes from the manufacturer with one SOP written that performs the following functions a Runa
193. xport Peak to NIST c nist08 mssearch ioj x Peak Name Name Unknown spectrum 37 0320 seconds scan 246 in TAT 9 Validation G36 5D Card G36 Data CDP 0000045 cof Figure 5 69 Write Spectra to NIST File dialog box 90 OTHER OPERATIONS 5 The file name is the default file name set in the Preferences under the Edit menu The name can be changed from this screen The new name will be saved in the Preferences menu 6 The masses can be edited before being sent to the file 7 To remove an lon select it by clicking on the mass with the mouse Then click the red button with the minus sign and the mass will be removed There are no dialog boxes to warn that a mass will be removed If a mass is removed that the user did not want removed select cancel to close the dialog box and reselect the send spectra to NIST to reopen the dialog box with the original spectral content 8 To adda Mass click the green button with the plus sign This will add a blank line at the end of the table Type in the new mass with its relative intensity 9 The Append adds the spectra to the last created file as a new spectra The Overwrite option replaces the file with the single spectra This allows the operator to send multiple or single spectra to the NIST file for viewing in the NIST MS Search software 10 After selecting the OK button the following image shows the dialog box that is displayed indicating that the spectra have been written to the fil
194. y the helium source still has an adequate amount of helium If using the on board carrier gas cartridge check the He High Pressure of the system which will indicate if the cartridge is empty To do this i Access the Advanced screen see the Advanced Operations chapter for instructions ii Select the Status Diagnostics screen iii Select the Gas Chromatography tab and the following screen will be displayed Eki Injector Temp Split Splitless Settings Column Temp 10 1 On Transfer Line Temp 10 1 Off Carrier Gas Flow 50 1 On He YSO Pressure 50 1 Off He High Pressure Figure 10 1 Gas Chromatography tab iv Check the He High Pressure read back When the helium cartridge is full this reads approximately 2500 and 0 when it is empty If the cartridge is empty replace it with a new one see Change the carrier gas cartridge in the Other Operations chapter If using an external helium source verify that the source still has an adequate amount of helium and that the pressure regulator is set to 80 psi Also verify that none of the carrier lines and or connections are leaking Verify that the Merlin septum is not leaking If it is leaking replace it with a new one see section Septum Replacement in the Service chapter Acquired mass spectra are noisy 1 If the mass spectra are noisy the chromatogram will probably be noisy as well A noisy mass spectrum may result from some of the problems discussed in the sec
195. yed after selecting the manage files from the advanced SCIrEeN csssseseseceeeeees 36 Fourcade e O pE mana ee ee 36 Figure 4 43 screen showing methods selection MenU sssessesssesseessesssesseossesscessesssesscoseesscossesseosseoseesseoseesseoseesseoseesseosseeseessessees 37 Figure 4 44 Viewing method injection parameters essesssesseessesseesseossesseossesseesseoseesscoseesseosseoseosresseosseoseeseoseesseoseesssossesseessessees 38 Fig r 4 45 Viewing method column para Mete sssusa aaia aaaeaii a aaa 38 TROUBLESHOOTING Figure 4 46 Viewing attached library to CHOSEN Meth sesesssssssssscsecscscsssescsssscscscsesesececscsesssesececucscsesesececencacscseseeneacacees 39 Figure 4 47 Screen showing the system setting OPTIONS uuu sesececsssssesesecscscsssescsesscscscsesesececsesesesesecscscsesesesececscasscscsesecscaeacees 39 Figure 4 48 screen showing the date and time settings uu ssssessssssecsssecscsssssccsssecessesecscsesecscsesecucsesecsesesecscsessescseseescacseeecess 40 Figure 4 49 Screen showing the password Setting Screen cssssssssssscssscsscscsssssscsssssecssesecscsssesscsesecsesesesscsesecsesesesscsessencesesescees 41 Figure 4 50 Firmware updating See ssis ee 41 Figure 4 51 Install update error screen scssessesesscscsssssenessessssensenessenessonsenencencosensenencanessanaenencanensonaesencaeneonansencaeneoranseneseneoransenes 42 Figure 4 52 Bluetooth control screen pee ne nen nn ee 42 Figure 4 53 Previous
196. ype in the numeric values in the columns 70 OTHER OPERATIONS 13 Ifa value is entered that is not acceptable a red exclamation point will be shown in the column on the far left The following image shows an error in the last column of the table next to 172 809 In this case a letter has been entered into a numeric value only field Index Expected Minimum If this happens the software will not allow the user to change to another field until the error situation has been corrected DEJ Retention Time Calibrations a Toluene d8 759 32 8 BPFB 875 41 7 fsa Ta Dibromotetrafl 1100 65 6 Methyl Salicylate 1281 717 ei 4 1400 85 1 lt 1 4 x 4 lanl e Masses for lt Bromoform gt 174 908 1025 1175 co Ee a a aa Pe ens es eh Figure 5 33 Performance Validation screen showing an error in data entry 14 To remove a mass use the mouse to highlight the mass in the table then click the Remove Calibration Mass button which is the second button from the left with the trash can on it The following image shows the dialog box that opens after clicking on the Remove Calibration Mass button Removing Compound Mass Do you want to remove the mass as e Figure 5 34 Performance Validation Removing Compound Mass dialog box 15 Selecting yes will remove the mass from the table Tools 1 The Tools section of the navigation pane contains functions that are not part of a method Method
197. ystem blank run is performed es sssessssesssesssesssessseesseesserssseosseosseeseessersserssseossess 19 Figure 4 11 Results of a system blank run that contained CONTAMINANT peaks ss sssesesessseesseesseesseeosscosseosseesseesseessseossees 20 Figure 4 12 Contaminated System Blank run notice ssessssssecscsssecscsssececssscsecsssssecscsssecscsssecsssssecscsesecscsesscscassecscasssescasscescess 20 Figure 4 13 SOP step 2 Run Performance Validation SCre n csscsssssscscsssscscsssssscsssssecsssssssssssecessesecesessscsessesesssseecassseecees 21 Figure 4 14 Please Wait screen indicating that the GC column is still cooling to initial Set point ssessessessesseesees 21 Figure 4 15 Instructions ON how to perform AN injection csssesscsssecscsssecscsssecscsssssecscsesecscsesecscsssecscsesssecsesecucsesssscsessescasssescess 22 Foure tisha scien cl Mal lade q ee EE ae ee ee ee ee 22 Figure 4 17 Depress plunger then remove syringe screen sssssscssssscssesesesssssecesesesesesessssceccscscscscscscscscscscacscasasasacasasacesseeenes 23 Figure 4 18 Screen shown while running a Performance ValidatiOn ss sssessseesssesssesssessseesseessersseesseeosseosseosseesseessersssesssees 23 ae e a EE ee e ae o a i N A A Le 24 Figure 4 20 Calibration results screen when calibration fails sssssssesssessseesseesseesssessseosseosseesseessersserosseosseosseesseesseesserssseossees 24 Figure 4 21 Retry Performance Validat
198. ystemBlank Versions GUI Version 1 0 4428 2722 Analog OS Version 1 0 0 0 DAQ GC Driver Version 1 0 0 2 Figure 4 35 Version tab of the status diagnostics screen 2 With the Versions tab selected this screen shows all of the information about the versions of code used in the instrument This information is used by service personnel to ensure that all of the correct control software has been loaded onto the instrument 3 Selecting the Gas Chromatography tab opens the following screen Target4E a gt activated2012 04 16 13 35 40 L 9 T SJ 1 SystemBlank ad SS Injector Temp 269 64 Split Splitless Settings Column Temp 150 08 10 1 Gn Transfer Line Temp 269 96 10 1 Off Carrier Gas Setting 50 1 On He VSO Pressure 50 1 Off He High Pressure 117 63 Figure 4 36 Gas Chromatography tab of the Status Diagnostics screen 4 This tab shows the actual temperatures and pressures of the various components of the GC It also shows the Split Splitless Settings 5 Selecting the Mass Spectrometry tab displays the following screen 33 INSTRUMENT OPERATION Target4E Torion Technologies activated2012 04 16 13 35 40 1 S ystemBlank Mass Analyzer Settings Drive Voltage Drive Current Detector Voltage 0 234 0 031 Amplitude B Amplitude A Ion Source Target Turbo Pump Speed Turbo Pump Current Trap Heater Temp Figure 4 37 Mass Spectrometer tab of Status Diagnostics scr

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