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3 Spectra
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Tutorial

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03-954143-55:Rev. 1

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Содержание 210-MS

Страница 1: ...Varian Inc 2700 Mitchell Drive Walnut Creek CA 94598 1675 USA 03 954143 55 Rev 1 1 of 33 210 MS and 220 MS GC MS Ion Trap Mass Spectrometer Installation Procedure ...

Страница 2: ...reline Pump 9 DS 42 Pump 9 Powering Up the MS 11 Baking Out the GC MS 11 Preliminary Tuning 12 Monitoring the System 12 Adjusting the RF Ramp 13 Adjusting Cal Gas 15 Auto Tuning 16 Auto Tuning 16 Testing Specifications 17 Specification Table 17 EI Methodology 17 Acquiring OFN 18 Reviewing the Data 18 Calculating the Signal to Noise Ratio 20 Library Searching 22 CI Methodology 25 Installing Liquid ...

Страница 3: ...ive 29 Creating a Sample List 29 Activating and Running a Sample List 29 Reviewing Results 30 Basic Source Maintenance 30 Checklist for Familiarizing the User Representative 31 Appendix 2 Spare Parts 32 Kits Assemblies Boards and Cables 32 Trap Components 32 Pumps 33 03 954143 55 Rev 1 3 of 33 ...

Страница 4: ...h the 431 GC and the 450 GC 1 System unpacking setup and checking 2 hours 2 Power up pump down demo 4 hours 3 Verification of GC MS System Operation 2 hours 4 EI checkout and demo 1 hours 5 Additional customer familiarization 4 hours Option Installation 1 Autosampler installation check out familiarization 1 5 hours 2 CI ionization mode demo familiarization 0 5 hour 3 MS MS demo 0 5 hour Enter inst...

Страница 5: ...tting up and starting the GC MS ensure that all parts and kits were delivered and are complete Review with the customer the contents of the accessory kits and their functions Report all shipping damage or missing parts to the Customer Service department Phone 925 939 2400 Fax 925 945 2360 email orders csb varianinc com Varian 2700 Mitchell Drive Walnut Creek CA 94598 Note any shipping damage or mi...

Страница 6: ...MP ONLY connector at the rear of the MS To minimize vibrations put the foreline pump on the floor not on the bench 8 Connect the power cords of the MS the GC and the PC into the appropriate outlets 9 Connect the GC to the MS as follows 431 GC Connect the sync cable to the back of the GC at J2 sync analog out and to the back of the MS at J43 Remote Option 450 GC Connect the sync cable under the GC ...

Страница 7: ...ck of 210 220 GC MS 10 Connect the USB cable to the rear of the MS at J42 USB and to a USB port on the PC 11 Connect a crossover Ethernet cable to the GC and to the PC Be sure to connect the Ethernet cable using the side connector of the Tee and NOT the terminators 03 954143 55 Rev 1 7 of 33 ...

Страница 8: ...35300 provided in the MS Accessory Kit Re install the partially less than half filled vial into the MS and tighten the mounting screws The vial must be inserted far enough into the pneumatic block to engage the O ring Store the remaining FC 43 in the vials provided in the accessory kit Be careful not to overfill the Cal Gas vial to avoid FC 43 contamination that can interfere with system performan...

Страница 9: ...n the MS NOTE Leave a significant service loop of column detached from the column cage so the GC and MS can be easily separated 1 Disengage the transfer line by removing the clip to remove it completely from the manifold 2 Position the column in the transfer line so the end of the column extends 0 5 to 1 mm past the end of the transfer line and leave a big enough loop so the MS and the GC can be e...

Страница 10: ...ump under the bench Do not lengthen the vacuum hoses to prevent degrading the vacuum The foreline pumps must be connected to a ventilation system NOTE You may observe foam when you look at the oil level The oil may foam until sufficient oil collects on the filter to create a seal and then it will stop foaming 03 954143 55 Rev 1 10 of 33 ...

Страница 11: ...d to it 6 Check that the status screen displays both MS and GC 7 The turbo pump speed should reach 100 between 1 to 2 minutes The turbo current should be less than 350 mA when the turbo reaches 100 8 Check for high mass noise using the daily check method If OK then check air water There should be a big 18 peak and no 28 peak Turn off trap If OK bakeout MS overnight Baking Out the GC MS 1 Ensure th...

Страница 12: ...bakeout familiarize the customer with the system 10 After bakeout reset the manifold bakeout temperature to 80 C and then click Save Preliminary Tuning Before doing preliminary tuning ensure that the MS has returned to Analysis temperatures and the GC column flow rate is set to 1 mL min Monitoring the System 1 After bakeout monitor the following in the Diagnostics tab Heated Zones Operating Condit...

Страница 13: ...g the RF Ramp 1 In the Adjustments tab in Manual Control click Adjust RF Tuning 2 Adjust the RF tuning rod to minimize the Highest value in the upper right corner of the Counts area 03 954143 55 Rev 1 13 of 33 ...

Страница 14: ...CAL GAS VENT CI GAS RF ADJUSTMENT 3 Click Save Results when finished 03 954143 55 Rev 1 14 of 33 ...

Страница 15: ...e display shows that the Cal Gas pressure is OK 4 Click Save Results when finished NOTE The Cal Gas adjustment varies with differences in auto tune settings filament emission current system sensitivity and system background levels Check this adjustment after auto tuning editing the filament emission current or when system sensitivity or background levels change 03 954143 55 Rev 1 15 of 33 ...

Страница 16: ...lier Tune FC 43 Mass Calibration Trap Function Calibration 3 Click Start Auto Tune The values generated are for both EI and CI 4 Check the event message display line by line to review the results of each auto tune function 5 Investigate and resolve auto tune parameters that did not pass and rerun them Run the following tunes once every two weeks for mass assignment Adjust RF Tuning Mass Calibratio...

Страница 17: ... A EI Methodology NOTE The MS comes with a CD containing factory test method and data files Use these method files to pass the installation sensitivity tests At the factory the diluted OFN standard is injected using a pressure pulse and splitless injection technique Retain the Test Files CD for your records 1 Ensure the MS temperatures are set as follows Trap 150 C Manifold 40 C Transfer Line 230 ...

Страница 18: ... barrel if using a Pressure Pulse 3 Strike the injector auto switch with the syringe barrel This ensures that the split valve has changed from open to close 4 Make a 1 µL manual injection of OFN Reviewing the Data 1 View a data file MS Data Review 2 Enter 272 in the Ions field of the MSDR window to display a single ion chromatogram of the m z 272 ion signal 03 954143 55 Rev 1 18 of 33 ...

Страница 19: ...3 Click and drag a zoom highlight box around the OFN m z 272 ion 4 Right click the apex scan of the 272 single ion chromatogram to display the Chromatogram menu 03 954143 55 Rev 1 19 of 33 ...

Страница 20: ... select Filtered Data Only 4 In the Filtering area select Smooth Data type 5 in the Point Smooth field select Savitsky Golay for the Smoothing Method enable Remove Spikes and type 4 for the Spike Threshold Factor 5 Click OK to enable these selections 6 Click the Noise tab select RMS for the Noise Calculation and click OK 03 954143 55 Rev 1 20 of 33 ...

Страница 21: ...pex scan of the 272 single ion chromatogram to display the Chromatogram menu 7 Click Calculate S N to generate the RMS signal to noise ratio The following shows both the menu and the S N data 03 954143 55 Rev 1 21 of 33 ...

Страница 22: ... menu select Edit Background Correction 3 Click Auto Background Correction The Background Correction Spectra Count is displayed 4 Click Done 5 Click the apex scan of the m z 272 single ion chromatogram to generate the spectrum BC in the upper right corner of the spectral window indicates that 03 954143 55 Rev 1 22 of 33 ...

Страница 23: ...e spectrum was background corrected 3 Spectra Averaged Background Corrected 6 From the Search menu select Library Search Active Spectrum 7 From the Library List select Tutorial 03 954143 55 Rev 1 23 of 33 ...

Страница 24: ...halene has the highest match score 500 9 Click the NIST Library Search button 10 Select Spectrum Search to edit the library search parameters Suggested library search parameters are displayed 03 954143 55 Rev 1 24 of 33 ...

Страница 25: ...20 MS CI option Installing Liquid CI 1 Condition the CI plumbing to remove air and water by opening the CI solenoids in Manual Control before introducing methanol into the CI plumbing 2 Install the Liquid CI Option on the back of the instrument as described in the hardware manual 03 954143 55 Rev 1 25 of 33 ...

Страница 26: ...Adjustments tab in Manual Control 2 Select the reagent Methanol from the drop down list 3 Click Adjust Cal Gas NOTE Minimize contamination by opening the CI needle valve only as needed 4 Click Save Results when finished 03 954143 55 Rev 1 26 of 33 ...

Страница 27: ...Acquiring BZP 1 Use the Inject Single Sample option to make a 1µL manual injection of test mix part number 393065201 2 Use a lower air gap to avoid sample loss through the tip of the needle 3 Ensure the syringe plunger is not forced out of the syringe barrel if a Pressure Pulse is used in the method 4 Ensure the split valve has changed from open to close before injecting by striking the injector a...

Страница 28: ...togram of the m z 183 ion 3 Click the apex scan to display the spectrum 4 Background correct the spectrum 5 Right click the apex scan and select Calculate Noise 6 The RMS signal to noise calculation is done on the scan closest to where you clicked Use 5 Point Savisky Golay smoothing An example follows 03 954143 55 Rev 1 28 of 33 ...

Страница 29: ...he checklist at the end of this section Creating a Sample List 1 Click Edit Automation Files on the MS Workstation tool bar 2 Click File New SampleList An empty sample list opens for the autosampler configured on the system Enter the sample information 3 Click Data Files to place files in the correct folder 4 Click RecalcList to create a RecalList 5 Save the SampleList The sample list is configure...

Страница 30: ...rom the tree on the left Basic Source Maintenance Loss of sensitivity over time is usually due to a dirty or poorly optimized trap and contaminated trap components Set up a schedule to routinely clean the trap and trap components The frequency of cleaning depends on the sample matrix and the number of samples injected 03 954143 55 Rev 1 30 of 33 ...

Страница 31: ...vacuum system starting and venting the pumps monitoring turbo speed Monitoring pressures in the manifold for normal and fault conditions Checking diagnostic for troubleshooting Performing an Auto Tune Acquiring data files as single runs and sample lists Integrating data using standard data files provided with the software Cleaning the trap components Performing routine foreline pumps maintenance 0...

Страница 32: ...The Silica Coated Spacers have a shiny mirror like finish on the inside surface Part Number Description 393055201 Gate Conductor 393055101 Gate 1492000900 Wavy Washer 393031501 Assembly Multiplier 393053501 Spacer Quartz 393010801 Transfer Line Wrench Analyzer Alignment Tool 393060191 Assembly Filament disk with wires 1499822800 Belleville Washer Small 393036000 Nut Hex 393654901 Filament Clip 393...

Страница 33: ...7001 393077002 Mechanical Pump 90 L min 115V Varian DS42 Mechanical Pump 90 L min 230V Varian DS42 392035800 Screen Turbo Pump V 81 392051800 7 ft Length Tygon Tubing 393076401 Turbo Molecular Pump V 81 9499305 Inland 31 Vacuum Pump Oil 393847701 Oil Mist Cartridge ...

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