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Agilent Technologies 5975 Series Operating Manual Download Page 93

 

4

Operating in EI Mode

5975/5977 Series MSD Operating Manual

93

Figure 24.

The GC/MSD interface

Ionization 
chamber

Analyzer 
chamber

Heater/Sensor 
assembly

MSD

GC oven

Heater sleeve

Insulation

Column

Column end protrudes 1 to 2 mm into the ionization chamber.

Summary of Contents for 5975 Series

Page 1: ...Agilent 5975 5977 MSD for OpenLAB CDS Operating Manual ...

Page 2: ...ity and fitness for a particular purpose Agilent shall not be liable for errors or for incidental or consequen tial damages in connection with the furnishing use or performance of this document or of any information con tained herein Should Agilent and the user have a separate written agree ment with warranty terms covering the material in this document that conflict with these terms the warranty ...

Page 3: ... 1 Introduction Chapter 1 describes general information about the 5977B Series MSDs including a hardware description general safety warnings and hydrogen safety information 2 Installing 7890 7820 6890 6850 GC Columns Chapter 2 shows you how to prepare a capillary column for use with the MSD install it in the GC oven and connect it to the MSD using the GC MSD interface 3 Intuvo 9000 GC Column Maint...

Page 4: ...77 90103 for more details on how to install this information on your computer 5975 5977 Series MSD prior to the 5977B MSD Users of Agilent MSD instruments manufactured prior to the 5977B should refer to the documentation delivered to them when their MSD was purchased The information in this manual is intended to supplement that documentation Information included here will help you more effectively...

Page 5: ... 16 Hydrogen Safety 19 GC precautions 19 Precautions 21 Safety and Regulatory Certifications 23 Intended Use 26 Cleaning Recycling the Product 26 Accidental Liquid Spillage 26 Moving or Storing the MSD 26 To Replace the Primary Fuses 27 2 Installing 7890 7820 6890 6850 GC Columns Columns 30 To Install a Capillary Column in a Split Splitless Inlet 32 To Condition a Capillary Column 35 To Install a ...

Page 6: ...s Components 54 To Replace an Intuvo GC Column 55 To Replace an Intuvo 9000 GC Gasket 59 To Install a Column Guard or Jumper Chip 60 To Replace the 9000 GC MS Tail 64 To Condition an Intuvo Capillary Column 68 To Install the Interface Tip Seal 70 The GC MS Interface for a 9000 Series GC 72 4 Operating in EI Mode Operating the MSD from the DS 76 Operating the MSD from the GC Control Panel 77 Config...

Page 7: ...lling Column Flow 95 Venting the MSD 96 Set MS Analyzer Temperatures 97 Enable the GC MS Interface and Oven 99 View MSD Temperatures and Vacuum 100 To Run an Autotune 102 To Open the MSD Covers 103 Vent the MSD 104 To Pump Down the MS 106 To Move or Store the MSD 109 5 General Maintenance Before Starting 112 Maintaining the Vacuum System 116 Maintaining the Analyzer 117 To Open the Analyzer Chambe...

Page 8: ... 139 To Connect Disconnect Wiring from the EI XTR SS and Inert Sources 140 To Disassemble the EI SS or EI Inert Source 141 To Disassemble the EI XTR Source 144 To Clean an EI XTR SS or Inert Source 147 To Assemble an EI SS or Inert Source 151 To Assemble the EI XTR Source 154 To Replace a Filament in an EI XTR SS or Inert Source 157 To Install the EI XTR SS or Inert Source 159 To Replace the Elect...

Page 9: ...t Safety Warnings 16 Hydrogen Safety 19 Safety and Regulatory Certifications 23 Intended Use 26 Cleaning Recycling the Product 26 Accidental Liquid Spillage 26 Moving or Storing the MSD 26 To Replace the Primary Fuses 27 This chapter describes general information about the MSD including a hardware description general safety warnings and hydrogen safety information ...

Page 10: ...able on the Inert MSD model and a high efficiency source HES The serial number label displays a product number that indicates what type of MSD you have See Table 1 Table 1 Available high vacuum pumps Model name Product number Description Ionization mode Type 5977B MSD Diff Pump G7080B Diffusion pump EI SS 5977B MSD Turbo Pump G7081B Turbo pump EI SS 5977B Inert MSD EI Turbo G7077B Turbo pump MSD E...

Page 11: ...nylphosphine calibrant DIP Direct insertion probe DS Data System EI Electron ionization EM Electron multiplier detector EMV Electron multiplier voltage EPC Electronic pneumatic control eV Electron volt GC Gas chromatograph HED High energy dynode refers to detector and its power supply HES High Efficiency Source New generation EI source constructed from inert material Inert Standard EI source const...

Page 12: ...erfluoro 5 8 dimethyl 3 6 9 trioxydodecane calibrant PFHT 2 4 6 tris perfluoroheptyl 1 3 5 triazine calibrant PFTBA Perfluorotributylamine calibrant Quad Quadrupole mass filter RF Radio frequency RFPA Radio frequency power amplifier SS Stainless steel Torr Unit of pressure 1 mm Hg Turbo Turbomolecular pump WUI Web user interface XTR EI Extractor source Table 2 Abbreviations continued Abbreviation ...

Page 13: ...urces available Standard source in SS material Standard source in Inert material XTR source HES Independently MSD heated hyperbolic Quad HED EM Independently GC heated GC MSD interface Physical description The 5977B Series MSD housing is approximately 41 cm high 30 cm wide and 54 cm deep The weight is 39 kg for the diffusion pump mainframe 44 kg for the standard EI turbo pump mainframe and 46 kg f...

Page 14: ...column flow mL min 1 1 to 2 Maximum recommended gas flow mL min Total gas flow into the MSD column flow plus reagent gas flow if applicable Based on helium gas use For other gases the maximum flow will vary 1 5 4 Maximum gas flow mL min Expect degradation of spectral performance and sensitivity 2 6 5 Max column id 0 25 mm 30 m 0 53 mm 30 m Inert ion sources available Yes Yes GC compatibility 6890 ...

Page 15: ...Series MSD Operating Manual 15 MSD Hardware Description Figure 1 5977B Series GC MSD system shown with an Agilent 7890B GC ALS 7890B GC 7890B GC control panel 5977B Series MSD MSD power switch GC power switch System status LED ...

Page 16: ...n the instrument The internal wires and cables connected to these boards The wires for any heater oven detector inlet or valve box If one of the primary fuses has failed the MSD will already be off but for safety switch off the MSD and unplug the power cord It is not necessary to allow air into the analyzer chamber WARNING All these parts are shielded by covers With the covers in place it should b...

Page 17: ...including the column nuts attaching the column to a GC inlet GC MS interface or GC detector The GC detector The GC valve box The foreline pump The diffusion pump The heated MSD ion source interface and quadrupole Always cool these areas of the system to room temperature before working on them They will cool faster if you first set the temperature of the heated zone to room temperature Turn the zon...

Page 18: ...mic fibers To avoid inhaling fiber particles we recommend the following safety procedures Ventilate your work area Wear long sleeves gloves safety glasses and a disposable dust mist respirator Dispose of insulation in a sealed plastic bag Wash your hands with mild soap and cold water after handling the insulation WARNING Combustible materials or flammable nonflammable wicking material placed under...

Page 19: ...tic cover for the MSD transfer line located on the GC left side panel In the unlikely event of an explosion this cover may dislodge WARNING The use of hydrogen as a GC carrier gas or detector fuel gas is potentially dangerous WARNING When using hydrogen H2 as the carrier gas or fuel gas be aware that hydrogen can flow into the GC oven and create an explosion hazard Therefore ensure that the supply...

Page 20: ...ttings should always be either connected to a column or have a cap or plug installed Table 4 Hydrogen accumulation mechanisms Mechanism Results MS turned off A mass spectrometer can be shut down deliberately It can also be shut down accidentally by an internal or external failure There is a safety feature that will shut down the flow of carrier gas in the event of an MSD foreline pump shut down Ho...

Page 21: ... In some GCs a power failure may cause the carrier gas flow to be set to maximum As a result hydrogen may accumulate in the mass spectrometer Table 4 Hydrogen accumulation mechanisms continued Mechanism Results WARNING Once hydrogen has accumulated in a mass spectrometer extreme caution must be used when removing it Incorrect startup of a mass spectrometer filled with hydrogen can cause an explosi...

Page 22: ...its source every time shutoff valves in an MSD are closed Do not heat the capillary column without carrier gas flow Turn off the hydrogen at its source if a power failure occurs If a power failure occurs while the GC MSD system is unattended even if the system has restarted by itself 1 Immediately turn off the hydrogen at its source 2 Turn off the GC 3 Turn off the MSD and allow it to cool for 1 h...

Page 23: ...ries MSD is designed and manufactured under a quality system registered to ISO 9001 The 5977B Series MSD is RoHS compliant Information The Agilent Technologies 5977B Series MSD meets the following IEC classifications Equipment Class I Laboratory Equipment Installation Category II Pollution Degree 2 This unit has been designed and tested in accordance with recognized safety standards It is designed...

Page 24: ...tic compatibility This device complies with the requirements of CISPR 11 Operation is subject to the following two conditions This device may not cause harmful interference This device must accept any interference received including interference that may cause undesired operation See accompanying instructions for more information Indicates a hot surface Indicates hazardous voltages Indicates earth...

Page 25: ...et so that the device and the radio or television are on separate electrical circuits 4 Ensure that all peripheral devices are also certified 5 Ensure that appropriate cables are used to connect the device to peripheral equipment 6 Consult your equipment dealer Agilent Technologies or an experienced technician for assistance Changes or modifications not expressly approved by Agilent Technologies c...

Page 26: ...with a damp lint free cloth For recycling contact your local Agilent sales office Accidental Liquid Spillage Do not spill liquids on the MSD If liquid is accidentally spilled on the MSD first cut the power Once the MSD is disconnected from all power sources dry all affected parts If the liquid spillage affects the electronics wait at least 24 hours depending upon the ambient humidity While waiting...

Page 27: ... MSD and unplug the power cord It is not necessary to allow air into the analyzer chamber 2 Turn one of the fuse holders counterclockwise until it pops out The fuse holders are spring loaded See Figure 2 on page 28 3 Remove the old fuse from the fuse holder 4 Install a new fuse in the fuse holder 5 Reinstall the fuse holder WARNING Never replace the primary fuses while the MSD is connected to a po...

Page 28: ...977 Series MSD Operating Manual 6 Repeat steps 3 through 5 for the other fuse Always replace both fuses 7 Reconnect the MSD power cord to the electrical outlet 8 Pumpdown the MSD Figure 2 Primary fuses Primary fuses in holders ...

Page 29: ... Column Nut 36 To Install a Capillary Column in the GC MS Interface Using a Standard Column Nut 41 To Install the Interface Tip Seal 44 To Calibrate Column Flow Linear Velocity 46 The GC MSD Interface for a 7890B Series GC 49 Before you can operate your GC MSD system you must select install and condition a GC column This chapter shows you how to install and condition a column For correct column an...

Page 30: ...ditioning columns Conditioning a column before it is connected to the GC MSD interface is essential See To Condition a Capillary Column on page 35 A small portion of the capillary column stationary phase is often carried away by the carrier gas This is called column bleed Column bleed deposits traces of the stationary phase in the MSD ion source This decreases MSD sensitivity and makes cleaning th...

Page 31: ...res for the 5977B Series MSDs may be different from that for previous MSDs Using the procedure from another instrument may not work and may damage the column or the MSD Always use carrier gas that is at least 99 9995 pure Because of thermal expansion new ferrules may loosen after heating and cooling a few times Check for tightness after two or three heating cycles or use the self tightening column...

Page 32: ...7 mm id for 0 20 mm id columns 5062 3516 0 40 mm id for 0 25 mm id columns 5181 3323 0 5 mm id for 0 32 mm id columns 5062 3514 0 8 mm id for 0 53 mm id columns 5062 3512 Inlet column nut 5181 8830 for Agilent 7890 Series and 7820 Magnifying loupe Septum may be old used inlet septum To install columns in other types of inlets refer to your GC User Information WARNING The GC operates at high temper...

Page 33: ...om the column nut 3 Use the column cutter to score the column 2 cm or more from the end 4 While holding the column break the column end off at the score 5 Inspect the end for jagged edges or burrs If the break is not clean and even repeat steps 3 and 4 6 Wipe the outside of the free end of the column with a lint free cloth moistened with methanol CAUTION Always wear clean gloves while handling any...

Page 34: ...ven with the bottom of the column nut 12 Tighten the column nut an additional 1 4 to 1 2 turn The column should not slide with a gentle tug 13 Start carrier gas flow 14 Verify flow by submerging the free end of the column in isopropanol Look for bubbles See also For more information about installing a capillary column refer to Optimizing Splitless Injections on Your GC for High Performance MS Anal...

Page 35: ... Increase the temperature at a rate of 10 to 15 C min 5 Hold at the maximum temperature for 30 minutes 6 Set the GC oven temperature to 30 C and wait for the GC to become ready 7 Attach the column to the GC interface See To Install a Capillary Column in the GC MS Interface Using the Self Tightening Column Nut on page 36 WARNING Do not condition your capillary column with hydrogen Hydrogen accumula...

Page 36: ... 20542 See Figure 6 on page 38 Not used with EI SS or Inert source Tip seal spring G7005 20024 Column cutter ceramic 5181 8836 or diamond 5183 4620 Flashlight Magnifying loupe Gloves clean Large 8650 0030 Small 8650 0029 Self Tightening column nut for GC MS interface 5190 5233 Ferrules Vespel 0 27 mm id for 0 10 mm id columns 5062 3518 0 37 mm id for 0 20 mm id columns 5062 3516 0 40 mm id for 0 2...

Page 37: ...e column against the column cutter with your thumb break the column against the edge of the column cutter 8 Inspect the end for jagged edges or burrs If the break is not clean and even repeat steps 6 and 7 9 Wipe the end with alcohol CAUTION Always wear clean gloves while handling any parts that go inside the GC or the analyzer chambers WARNING The analyzer GC MS interface and other components in ...

Page 38: ... the column extends about 1 mm For an EI HES Installation See Figure 6 the column extends 4 to 5 mm Use the flashlight and magnifying loupe if necessary to see the end of the column inside the analyzer chamber Do not use your finger to feel for the column end Figure 5 Installing a capillary column in the GC MS interface for an EI EXT SS or Inert source Figure 6 Installing a capillary column in the...

Page 39: ... 13 Check the GC oven to ensure that the column does not touch the oven walls 14 Install the tip seal and spring on the GC MS interface See To Install the Interface Tip Seal on page 44 Do not use a tip seal or spring with an EI SS or Inert source The interface socket on these sources does not allow the tip seal installation to fit See Figure 44 on page 142 Figure 7 Installing a capillary column in...

Page 40: ...spring tension from the interface tip seal 16 You can align the ion source and interface tip seal by wiggling the side plate on its hinge If the door still will not close contact your Agilent Technologies service representative 17 Close the analyzer chamber door See To Close the Analyzer Chamber on page 162 CAUTION Forcing the analyzer door closed if these parts are misaligned will damage the tip ...

Page 41: ...elf Tightening Column Nut on page 36 Materials needed Interface tip seal G3870 20542 See Figure 5 on page 38 and Figure 6 on page 38 Not used with EI SS or Inert source Tip seal spring G7005 20024 Not used with SS or Inert EI source Column cutter ceramic 5181 8836 or diamond 5183 4620 Flashlight Magnifying loupe Gloves clean Large 8650 0030 Small 8650 0029 Interface column nut 05988 20066 Ferrules...

Page 42: ...olumn against the column cutter with your thumb break the column against the edge of the column cutter 8 Inspect the end for jagged edges or burrs If the break is not clean and even repeat steps 6 and 7 9 Wipe the end with alcohol CAUTION Always wear clean gloves while handling any parts that go inside the GC or the analyzer chambers WARNING The analyzer GC MS interface and other components in the...

Page 43: ...ll the tip seal and spring on the GC MS interface See To Install the Interface Tip Seal on page 44 Do not use a tip seal or spring with an EI SS or Inert source The interface socket on these sources does not allow the tip seal installation to fit See Figure 44 on page 142 16 Gently check the alignment of the ion source and the interface tip seal When the ion source is aligned correctly the analyze...

Page 44: ...an EI SS or Inert source is installed 2 Place the tip seal spring over the end of the interface 3 Remove the interface tip seal from the ion source storage box and place it over the end of the interface 4 Gently check the alignment of the analyzer and the interface CAUTION Electrostatic discharges to analyzer components are conducted to the side board where they can damage sensitive components Wea...

Page 45: ...cept the spring tension from the interface tip seal 5 You can align the analyzer and interface by wiggling the side plate on its hinge If the analyzer still will not close contact your Agilent Technologies service representative CAUTION Forcing the analyzer closed if these parts are misaligned will damage the seal or the interface or the ion source or keep the sideplate from sealing ...

Page 46: ... monitor m z 28 2 Press Prep Run on the GC keypad 3 Inject 1 µL of air into the GC inlet and press Start Run 4 Wait until a peak elutes at m z 28 Note the retention time 5 In OpenLAB select Method layouts and click Agilent GC Configuration Columns 6 Select your installed column from the table 7 Click Calibrate to display the Calibrate Column dialog 8 Click Calc Length in the If unretained peak hol...

Page 47: ...ferent than those used in your method 10 Enter the recorded retention time in the Holdup Time field Move the cursor to another parameter s field and the calibrated column length appears 11 Click OK to save the changes and exit the dialog 12 Click OK on the Calibrate Columns dialog to save the calibration With capillary columns such as those used with the MSD linear velocity is often measured rathe...

Page 48: ...rage linear velocity Average linear velocity cm s where L Length of the column in meters t Retention time in seconds Calculation for volumetric flow rate Volumetric flow rate mL min where D Internal column diameter in millimeters L Column length in meters t Retention time in minutes 100 L t 0 785 D 2 L t ...

Page 49: ... of the GC and extends into the oven This end is threaded to allow connection of the column with a nut and ferrule The other end of the interface fits into the ion source The end of the capillary column extends slightly past the end of the column guide tube and into the ionization chamber Figure 10 GC MSD interface for a 7890B GC with EI XTR HES and CI sources Ionization chamber Analyzer chamber H...

Page 50: ...C The interface temperature should be slightly higher than the maximum GC oven temperature but never higher than the maximum column temperature The GC MSD interface can be used with both EI and CI sources The EI XTR HES and CI sources require a tip seal assembly The tip seal and spring interfere with and must be removed when using the EI SS and Inert sources See To Install a Capillary Column in th...

Page 51: ... the 9000 GC MS Tail 64 To Install the Interface Tip Seal 70 The GC MS Interface for a 9000 Series GC 72 This chapter shows you how to install an Agilent Intuvo column connect a flow path through the GC MS Interface into the ion source and maintain the column guard chip If you are using the Agilent Intuvo 9000 Gas Chromatograph with your MS Chemical Ionization CI and the JetClean system are not cu...

Page 52: ...mended flow will result in degradation of mass spectral and sensitivity performance Remember that column flows vary greatly with temperature requiring measurements of the actual flow to be taken Use Table 6 to determine an acceptable column flow Table 6 Gas flows Feature Gas flows High vacuum pump Turbo Optimal He column gas flow mL min carrier gas 1 to 2 Maximum recommended gas flow mL min Total ...

Page 53: ... oxygen in the carrier gas when the column is heated To minimize column bleed all capillary columns should be conditioned before they are installed in the GC MS interface See To Condition an Intuvo Capillary Column on page 68 Tips and hints Always use carrier gas that is at least 99 9995 pure Always wear clean gloves when handling a component s click and run connectors Always wear clean gloves whe...

Page 54: ...tead the Intuvo 9000 GC click and run connections use a sealing system based on contact between flat surfaces Compared to traditional ferrule seals these connections are leak free and easy to make When making these seals follow a few simple guidelines Do not touch the click and run sealing surfaces with bare skin or dirty gloves Skin oils and dirt can contaminate the flow path surfaces Use only th...

Page 55: ...panel select Maintenance Column Perform Maintenance Install Column Start Maintenance This procedure cools the inlet detector column Guard Chip and other components in the flow path heated zones to 40 C and configures the GC Follow the on screen GC prompts 2 From MassHunter Data Acquisition Vent the MS See Vent the MSD on page 104 3 If you are using hydrogen or other flammable gas as a carrier gas ...

Page 56: ... bus door and remove it by lifting the door vertically off its hinge pins 6 Lower the oven door 7 Using the Intuvo torque driver rotate all four column clamps off the column s retainer ring Figure 11 9000 GC front door bus door oven door and Intuvo torque driver Bus door Oven door Intuvo torque driver Front door ...

Page 57: ... connectors to the bus and store for later use 10 Remove and store the column for later use in accordance with the column manufacturer s recommendations 11 Replace the gasket with a new gasket rated for the maximum column temperature expected with your method See To Replace an Intuvo 9000 GC Gasket on page 59 Figure 12 9000 GC column and related parts SmartID key Column clamps Retainer ring Compre...

Page 58: ...4 Insert the column s attached Intuvo SmartID Key into the lower USB connection shown 15 Secure the new column by rotating the 1 c tab of the 4 column clamps over the column retaining ring using the Intuvo torque driver 16 Verify that the column s click and run fittings sit flat against the gasket 17 Loosely install the two compression bolts 18 Tighten the compression bolts until you hear a click ...

Page 59: ...s All chips must be installed before installing the new gasket 3 Carefully remove the new gasket from its packaging Inspect the gasket to be sure it is not deformed The two round lobes are the sealing surfaces 4 Carefully insert the round gasket lobes into the bus click and run fitting Note that the gasket is double sided 5 Place the hole in the gasket over the alignment stud in the bus fitting an...

Page 60: ...temperatures 350 C 5190 9072 Intuvo gasket nickel 5 pk for temperatures 350 C to 450 C 5190 9073 Intuvo torque driver stored on oven door 5190 9571 7 16 inch open end wrench Procedure 1 Prepare the GC for maintenance From the GC panel select Maintenance Inlets Guard Chip Prepare for Maintenance Replace Liner and Guard Chip Start Maintenance This procedure cools the inlet detector column Guard Chip...

Page 61: ...r the JetClean system close the manual gas supply valve to the instrument before turning off the MS power 5 If installed remove the ALS injector from the inlet 6 Remove the inlet cover 7 Open the GC front door 8 Open the bus door and remove it by lifting the door vertically off its hinge pins 9 Pull the compression bolt access plate out to allow the torque driver to access the Guard chip compressi...

Page 62: ...15 Install a new Guard Chip The larger end of the Guard Chip inserts into the inlet base first then the smaller end is rotated into the bus connection lifting its tab over the boss and into the bus mounting slot 16 Finger tighten the compression bolt 17 Raise the Guard Chip heater 18 Finger tighten the Guard Chip screw in the inlet base 19 Tighten the Guard Chip screw in the inlet base with a 7 16...

Page 63: ...rating Manual 63 20 Tighten the Guard Chip compression bolt using the provided torque driver until you hear one click 21 Install the inlet cover 22 Install the bus door on its hinges and close it 23 Close the GC front door 24 If removed install the ALS injector ...

Page 64: ...end wrench Procedure 1 Vent the MS See Vent the MSD on page 104 When prompted set the temperature for the ion source quads inlet detector column Guard Chip 9000 GC MS Tail and other components in the flow path heated zones to 40 C 2 If you are using hydrogen or other flammable gas as a carrier gas close the manual gas supply valve to the instrument before turning off the MS power 3 Wait until the ...

Page 65: ... bus door and remove it by lifting the door vertically off its hinge pins 9 Using the Intuvo torque driver remove the compression bolt that secures the 9000 GC MS Tail click and run bus connection Also remove the bolt from the empty bus connection 10 Open the MS tail heater assembly by loosening the thumb screw at the top of the clamp and rotating the clamp down 11 Push the MS tail heater assembly...

Page 66: ... the click and run connection into the bus connection 15 Check that the 9000 GC MS Tail click and run fitting sits flat against the gasket in the bus connection 16 Screw the 9000 GC MS Tail column nut to the transfer line threaded connector finger tight then use a inch wrench to tighten the nut an additional 20 to 30 degrees 17 Loosely install the two compression bolts Figure 16 MS tail heater ass...

Page 67: ...Interface Tip Seal on page 70 25 Gently check the alignment of the ion source and the interface tip seal When the ion source is aligned correctly the front analyzer chamber can be closed all the way with no resistance except the spring tension from the interface tip seal 26 You can align the ion source and interface tip seal by wiggling the side plate on its hinge If the door still will not close ...

Page 68: ...o Replace an Intuvo GC Column on page 55 2 Set a minimum velocity of 30 cm s or as recommended by the column manufacturer Allow gas to flow through the column at room temperature for 15 to 30 minutes to remove air 3 Increase the column temperature to 120 C 4 Hold at the this temperature for 30 minutes 5 Use MassHunter to run an air and water check Proceed to the next step if the air and water are ...

Page 69: ...to increase from 120 C to the maximum temperature limit for the column at a rate of 10 to 15 C min 7 Hold at the maximum temperature for 30 minutes The column is conditioned and ready to be used with your method CAUTION Never exceed the maximum column temperature in the GC MS interface the GC oven or the inlet ...

Page 70: ...ee Figure 18 2 Remove the interface tip seal spring and knurled nut retainer from the ion source storage box In this order slide the spring tip seal and knurled tip seal retainer over the column sleeve 3 Thread the knurled tip seal retainer into the tip seal hold finger tight CAUTION Electrostatic discharges to analyzer components are conducted to the side board where they can damage sensitive com...

Page 71: ...he way with no resistance except the spring tension from the interface tip seal 5 You can align the analyzer and interface by wiggling the side plate on its hinge If the analyzer still will not close contact your Agilent Technologies service representative CAUTION Forcing the analyzer closed if these parts are misaligned will damage the seal or the interface or the ion source or keep the sideplate...

Page 72: ...nut The 9000 GC MS Tail includes a swagged ferrule and column nut for attaching to the GC end of the GC MS Interface The 9000 GC MS Tail transports the column effluent from a heated column bus connector in the GC through the heated GC MS Interface and exits slightly past the end of the column guide tube and into the ionization chamber The 9000 GC MS Tail maintains temperature at several points alo...

Page 73: ... from the Agilent MassHunter GC MS Acquisition software or from the GC A sensor thermocouple in the interface monitors the temperature The transfer line tip seal assembly is required when using the EI XTR source or the HES The 9000 GC MS Tail should be operated in the 250 to 350 C range Subject to that restriction the transfer line temperature should be slightly higher than the column temperature ...

Page 74: ...3 Intuvo 9000 GC Column Maintenance 74 5975 5977 Series MSD Operating Manual ...

Page 75: ... Status LED 91 The GC MSD Interface 92 Before You Turn On the MSD 94 Pumping Down 95 Controlling Temperatures 95 Controlling Column Flow 95 Venting the MSD 96 Set MS Analyzer Temperatures 97 Enable the GC MS Interface and Oven 99 View MSD Temperatures and Vacuum 100 To Run an Autotune 102 To Open the MSD Covers 103 Vent the MSD 104 To Pump Down the MS 106 To Move or Store the MSD 109 This chapter ...

Page 76: ...temperatures tuning and venting the MSD These tasks are described in this chapter Additional information is described in the manuals and online help supplied with the OpenLAB CDS software CAUTION The software and firmware are revised periodically If the steps in these procedures do not match your OpenLAB CDS refer to the manuals and online help supplied with the software for more information ...

Page 77: ... OpenLAB CDS software You can access functions such as venting and setting temperatures right from the GC control panel Limited features are available from the GC control panel The OpenLAB CDS software is the full featured controller for most instrument control operations MSD designated key on the GC control panel The MS Aux Det key on the 7890B GC control panel allows access to control and config...

Page 78: ... MSD menu 2 Press the down arrow to scroll to HiVac Pressure or Turbo Speed of full Foreline Pressure To vent the MSD from the GC control panel 1 With the MSD pumped down press MS Aux Det to bring up the 5977B MSD menu 2 Press the down arrow to scroll to Start MSD Vent Press Off No to cancel the vent cycle and pump down the MS 3 Press ON Yes to start the venting cycle 4 When prompted open the vent...

Page 79: ...er the new IP address for the MSD then press Enter to complete the entry 3 Wait for the GC to display the new IP address Reboot the MSD or proceed to the gateway address with the down arrow button 4 Press the down arrow to scroll to GW and use the GC keypad to enter the new gateway address for the LAN and press Enter to complete the entry 5 Press the down arrow to scroll to SW and use the GC keypa...

Page 80: ...nu 2 Press the down arrow to scroll to MSD BOOTP 3 To enable BOOTP press On Yes To disable BOOTP press Off No 4 Wait for the MSD to confirm the change on the GC control panel 5 Reboot the MSD See above To enable disable LVDS on MSD 1 Press Config and then press MS Aux Det to bring up the CONFIGURE MS DETECTOR menu 2 Press the down arrow to scroll to Lvds communication If you want to enable the LVD...

Page 81: ...etwork settings of the MSD This procedure assumes that the operator has access to a PC located on the same LAN subnet as the MSD 1 Open the top hinged cover on the MSD for accessing the analyzer to view the eModule mini display readout 2 Press the MSD On Off switch to start the instrument When the instrument has completed its startup initialization it displays the current IP address information in...

Page 82: ...n EI Mode 82 5975 5977 Series MSD Operating Manual 5 Click Set Real Time Clock or Edit NetConfig and go to Edit NetConfig MSD network configuration See Figure 22 Figure 21 WUI main menu Figure 22 WUI Edit NetConfig ...

Page 83: ...t you can recover the previous settings by clicking Return to Main Menu and then returning here 8 Click Submit to upload this net configuration to the MSD A dialog opens to confirm that the network configuration process has started See Figure 23 9 Click OK to close the dialog and wait for the prompt requesting to Manually reboot of the MSD SmartCard to activate the new Settings 10 Use the MSD on o...

Page 84: ...u Status mode requires no interaction and simply displays the current status of the MSD instrument or its various communication connections If you select Menu then No Cancel you will be returned to the Status mode Menu mode allows you to query various aspects of the GC MSD and to initiate some actions like running a method or sequence or preparing to vent the system To access a particular menu opt...

Page 85: ... you cycle through all available menus the display automatically returns to Status mode Pressing Menu then No Cancel will always display the Status mode Pressing No Cancel twice will always return to the Status mode Use Yes Select to accept the current value Use No Cancel to return to the Status mode ...

Page 86: ...lable timestamp The Agilent OpenLAB CDS software is not running Loading Method method name Method parameters are being sent to the MSD Loading MSD Firmware The MSD s firmware is being initialized The following messages alternately appear on the LCP if the MSD does NOT complete its bootup sequence properly Server not Found Check LAN Connection Seeking Server Bootp Query xxx These messages indicate ...

Page 87: ...n is in progress data is being acquired to the designated data file To view system status during startup 1 The following messages are displayed on the LCP display during startup Press sideplate Loading OS Press sideplate Loading MSD Firmware 2 Continue to press the sideplate of the MSD until the MSD Ready message appears This helps the instrument to pump down more quickly LCP Menus To access a par...

Page 88: ...gh previous messages up to 20 Release ChemStation Disassociates OpenLAB CDS from the MSD Connection Status Displays the LAN connection status for the MSD Remote connected to an OpenLAB CDS online session Local not connected to an OpenLAB CDS online session Name of Instrument Displays the name of the instrument if connected to an OpenLAB CDS online session The name of the instrument is the name ass...

Page 89: ...ilter temperature CI Reagent Displays CI reagent gas and flow rate if installed NOTE MS parameters cannot be set from the LCP while an online OpenLAB CDS session is connected to the MSD Table 10 Network menu Action Description MSD IP via BootP Displays the IP address for the MSD Gateway IP Address Displays the gateway IP address for the MSD Subnet Mask Displays the subnet mask for the MSD ChemStat...

Page 90: ...el Displays the version of the LCP Log amplifier Displays version information Sideboard Displays the sideboard type Mainboard Displays the mainboard type Serial number Is assigned to the MSD by OpenLAB CDS Table 12 Controller menu Action Description Reboot controller Starts the LAN MS control card Test LCP Initiates a diagnostic test of the two line display Test HTTP link to GC MSD ChemStation Che...

Page 91: ...g the GC control panel or the web user interface WUI from a web browser Front Panel Instrument Status LED This section only applies to the 5977B MSD Earlier 5975 5977 MSD models do not have this feature Through the front panel Instrument Status LED the operator can view the current status of the instrument using color codes and LED on off timing Table 13 Front panel Instrument Status LED codes Ins...

Page 92: ... interface is heated by an electric cartridge heater Normally the heater is powered and controlled by Thermal Aux 2 heated zone of the GC The interface temperature can be set from OpenLAB or from the gas chromatograph A sensor thermocouple in the interface monitors the temperature The GC MSD interface should be operated in the 250 to 350 C range Subject to that restriction the interface temperatur...

Page 93: ... 5977 Series MSD Operating Manual 93 Figure 24 The GC MSD interface Ionization chamber Analyzer chamber Heater Sensor assembly MSD GC oven Heater sleeve Insulation Column Column end protrudes 1 to 2 mm into the ionization chamber ...

Page 94: ...hydrogen is used as carrier gas carrier gas flow must be off and the front sideplate thumbscrew must be loosely fastened The foreline pump exhaust is properly vented WARNING The exhaust from the foreline pump contains solvents and the chemicals you are analyzing If using the standard foreline pump it also contains traces of pump oil If you are using toxic solvents or analyzing toxic chemicals remo...

Page 95: ...ling Temperatures MSD temperatures are controlled through the data system The MSD has independent heaters and temperature sensors for the ion source and quadrupole mass filter You can adjust the setpoints and view these temperatures from the data system or from the local control panel Normally the GC MSD interface heater is powered and controlled by the Thermal Aux 2 heated zone of the GC The GC M...

Page 96: ...ng speed WARNING Make sure the GC MSD interface and the analyzer zones are cool below 100 C before you vent the MSD A temperature of 100 C is hot enough to burn skin always wear cloth gloves when handling analyzer parts WARNING If you are using hydrogen as a carrier gas the carrier gas flow must be off before turning off the MSD power If the foreline pump is off hydrogen will accumulate in the MSD...

Page 97: ... ion source and quadrupole heated zones interact The analyzer heaters may not be able to accurately control temperatures if the setpoint for one zone is much different from that of an adjacent zone 3 Click Download tune file to download these temperature setpoints to the MS and change the current control temperatures to these values 4 Click Save the tune parameters to make these temperature settin...

Page 98: ...4 Operating in EI Mode 98 5975 5977 Series MSD Operating Manual 6 Release Tune Control Figure 25 Set the Quad and Source temperatures ...

Page 99: ...ting Manual 99 Enable the GC MS Interface and Oven Procedure 1 Click Method Instrument Setup GC Aux Heaters 2 Select On for Thermal Aux 2 3 Click Oven and select On 4 Click Download Method to enable these temperature zones in the GC 5 Save the method ...

Page 100: ...he windows area and click MSD to display the MSD s actuals values including the source and quad temperatures and quad manifold vacuum pressure WARNING If you are using hydrogen as a carrier gas do not turn on the Micro Ion vacuum gauge if there is any possibility that hydrogen has accumulated in the analyzer chamber Read Hydrogen Safety on page 19 before operating the MSD with hydrogen carrier gas...

Page 101: ...line help in the Data Acquisition software for information on troubleshooting air leaks and other vacuum problems The vacuum can also be read on the 7890B GC control panel or from the Manual Tune Parameters view in OpenLAB Table 14 Ion vacuum gauge reading Column flow rate mL min Optional Gauge reading Torr Performance turbo pump Gauge reading Torr Diffusion pump Foreline reading mTorr Diffusion p...

Page 102: ...ntrol and select Tune Autotune The tune file used by the current method is loaded 2 To use a different tune file click Open a tune file and select it 3 Check Quick Tune if relative abundances of the 3 masses are at acceptable values unless a full autotune is needed 4 Optionally to send the Autotune report to the printer in the Reports area select Print Report 5 Click Start autotune The autotune pr...

Page 103: ... forward and lift off the MSD To open the analyzer cover Pull the handle on the side of the MSD to the left and down to release the magnetic latch and open the cover The cover is held in place by its hinges CAUTION Do not use excessive force or the plastic tabs that hold the cover to the mainframe will break off Figure 28 Analyzer covers Analyzer window cover Handle Analyzer cover WARNING Do not r...

Page 104: ...1 Select Method MSD Maintenance Vent Pump Down and click Vent to begin the process Follow the instructions presented 2 When prompted turn the vent valve knob counterclockwise only 3 4 turns or until you hear the hissing sound of air flowing into the analyzer chamber Figure 29 Vent the MSD ...

Page 105: ...arrier gas flow must be off before turning off the MSD power If the foreline pump is off hydrogen will accumulate in the MSD and an explosion may occur Read Hydrogen Safety on page 19 before operating the MSD with hydrogen carrier gas CAUTION Be sure the GC oven and the GC MSD interface are cool before turning off carrier gas flow to prevent damage to the column ...

Page 106: ... switch 5 Press lightly on the metal box of the analyzer quad driver board to ensure a correct seal WARNING Make sure your MSD meets all the conditions listed in the introduction to this chapter page 92 before starting up and pumping down the MSD Failure to do so can result in personal injury WARNING If you are using hydrogen as a carrier gas do not start carrier gas flow until the MSD has been pu...

Page 107: ... does not match the source used in the current method s tune file you are prompted to enter a method with the correct ion source type Load the correct method for your source type 8 Enable Tune Control and click Maintenance 9 Click Pump Down to start this procedure 10 You are prompted to turn on the transfer line heater and the GC oven Click OK when you have done so Figure 32 Pump down the MSD CAUT...

Page 108: ...tatus and the MSD actual parameters in comparison to criteria required for pump down completion is shown 12 Wait for the MS to reach thermal equilibrium After the message Okay to run appears wait 2 hours for the MS to reach thermal equilibrium Data acquired before the MS has reached thermal equilibrium may not be reproducible 13 When the pumpdown is finished click OK to clear the pump down status ...

Page 109: ...age 104 2 Remove the column and install a blank ferrule and interface nut 3 Tighten the vent valve 4 Move the MSD away from the GC see the 5977B Series MSD Troubleshooting and Maintenance Manual 5 Unplug the GC MSD interface heater cable and LVDS cable if used from the GC 6 Open the analyzer cover See To Open the MSD Covers on page 103 7 Finger tighten the side plate thumbscrews Figure 33 Side pla...

Page 110: ...SD can now be stored or moved The foreline pump cannot be disconnected it must be moved with the MSD Make sure the MSD remains upright and is never tipped on its side or inverted CAUTION Do not overtighten the side plate thumbscrews Overtightening will strip the threads in the analyzer chamber It will also warp the side plate and cause leaks CAUTION The MSD must remain upright at all times If you ...

Page 111: ...s 135 To Install the EI HES Filament 137 To Install the EI HES 138 To Remove the EI XTR SS or Inert Source 139 To Connect Disconnect Wiring from the EI XTR SS and Inert Sources 140 To Disassemble the EI SS or EI Inert Source 141 To Disassemble the EI XTR Source 144 To Clean an EI XTR SS or Inert Source 147 To Assemble an EI SS or Inert Source 151 To Assemble the EI XTR Source 154 To Replace a Fila...

Page 112: ...ance schedule Task Frequency Check the foreline pump oil level Every week Check the calibration vial s Every 6 months Replace the foreline pump oil Every 3 months for CI MSDs using ammonia reagent gas Every 6 months Replace the diffusion pump fluid Every year Change the dry foreline pump tip seal Every year Check the dry foreline pump As needed Tune the MSD As needed Change the foreline pump exhau...

Page 113: ...ween these boards Wires and cables between these boards and the connectors on the back panel of the MSD Some connectors on the back panel for example the foreline power receptacle Normally all of these parts are shielded by safety covers As long as the safety covers are in place it should be difficult to accidentally make contact with dangerous voltages Some procedures in this chapter require acce...

Page 114: ...h the standard foreline pump This trap stops only pump oil droplets It does not trap any other chemicals If you are using toxic solvents or analyzing toxic chemicals do not use this oil trap For all foreline pumps install a hose to take the exhaust from the foreline pump outdoors or into a fume hood vented to the outdoors For the standard foreline pump this requires removing the oil trap Be sure t...

Page 115: ...tic wrist strap and take other antistatic precautions The wrist strap should be connected to a known good earth ground If that is not possible it should be connected to a conductive metal part of the assembly being worked on but not to electronic components exposed wires or traces or pins on connectors Take extra precautions such as a grounded antistatic mat if you must work on components or assem...

Page 116: ...eline pump seals once a year Failure to perform these tasks as scheduled can result in decreased instrument performance It can also result in damage to your instrument Other procedures Tasks such as replacing a foreline vacuum gauge or Micro Ion vacuum gauge should be performed only when needed Refer to the Agilent 5977B Series MSD Troubleshooting and Maintenance manual and the online help in Agil...

Page 117: ...ter GC MS Acquisition software provides more extensive information Precautions Cleanliness Keep components clean during analyzer maintenance Analyzer maintenance involves opening the analyzer chamber and removing parts from the analyzer During analyzer maintenance procedures take care to avoid contaminating the analyzer or the interior of the analyzer chamber Wear clean gloves during all analyzer ...

Page 118: ...urbed In the event of extreme contamination it can be cleaned but such cleaning should only be done by a trained Agilent Technologies service representative The HED ceramic insulator must never be touched More information is available If you need more information about the locations or functions of analyzer components refer to the Agilent 5977B Series MSD Troubleshooting and Maintenance Manual Man...

Page 119: ...he MSD on page 104 2 Open the left side panel CAUTION Electrostatic discharges to analyzer components are conducted to the quad driver board where they can damage sensitive components Wear a grounded antistatic wrist strap and take other antistatic precautions See Electrostatic discharge on page 115 before you open the analyzer chamber WARNING The analyzer GC MS interface and other components in t...

Page 120: ...ew on the front side plate should only be fastened if hydrogen or other flammable or toxic substances are used for carrier gas or during CI operation 4 Gently swing the side plate out CAUTION In the next step if you feel resistance stop Do not try to force the side plate open Verify that the MS is vented Verify that both the front and rear side plate screws are completely loose Figure 34 The analy...

Page 121: ...essary See To Connect Disconnect Wiring to the EI HES on page 123 5 Using the source finger grip pull the ion source out of the source radiator The source contacts have spring loaded pins so some force must be applied to pull the source out WARNING The analyzers GC MS interface and other components in the analyzer chamber operate at very high temperatures Do not touch any part until you are sure i...

Page 122: ...e 122 5975 5977 Series MSD Operating Manual Figure 35 The analyzer chamber for the HES MSD Ceramic source board Ion source Thumbscrew Source heater and temperature sensor wires Source radiator Source finger grip Thumbscrew ...

Page 123: ...030 Small 8650 0029 Pliers long nose 8710 1094 Tweezers 8710 2460 Procedure 1 Use tweezers or needle nose pliers to connect disconnect the ceramic board wire leads red white black and gray at the source connectors See Figure 36 Figure 36 Wiring between the ceramic source board and the EI HES Repeller Filament common Filament 1 Filament 2 Ceramic source board ...

Page 124: ... the dual filament from the filament block by lifting the source body up off of the filament block while holding the filament block so that the dual filament will not fall and become damaged 4 Remove the finger grip from the filament block 5 Use a T6 Torx screwdriver to remove the two screws securing the source mount to the source body 6 Use the finger grip to remove the source mount from the lens...

Page 125: ...s casing can break or crack it If this happens do not attempt to operate with a defective lens insulator it must be replaced CAUTION Use care when removing the filament from the filament block Putting excessive stress on this can break or crack it If this happens do not attempt to operate with a defective filament it must be replaced Figure 37 Exploded parts view of the EI HES 1 2 8 16 17 15 9 4 3...

Page 126: ...64 5 Entrance lens assembly Extended HES 1 G7002 20165 6 Ion focus lens 2 G7002 20068 7 Lens insulator holder G7002 20074 8 M2 x 0 4 screw x 12 mm long gold plated screw G7002 20083 9 Source body G7002 20084 10 Post extractor lens 2 3 G7002 20090 11 Post extractor lens 1 4 G7002 20104 12 M2 x 6 mm gold plated screw G7002 20109 13 Locking ring lens insulator G7002 20126 14 High efficiency dual fila...

Page 127: ... grade Methylene chloride reagent grade Acetone reagent grade Ultrasonic bath Procedure 1 Disassemble the EI HES See To Disassemble the EI HES on page 124 2 Collect the following parts to be cleaned See Figure 38 on page 128 Filament mount Source mount does not get abrasively or ultrasonically cleaned Repeller Source body Extractor lens 5 Post extractor lens 1 4 Post extractor lens 2 3 Ion focus l...

Page 128: ...ith reagent grade methanol If that does not clean the insulators replace them Do not abrasively or ultrasonically clean the insulators Figure 38 EI HES parts to be cleaned Lens 1 2 3 4 5 Source body Repeller Source mount Filament block with bushings CAUTION The filaments source heater assembly and insulators cannot be cleaned ultrasonically Replace these components if major contamination occurs CA...

Page 129: ...away before ultrasonic cleaning If the methanol becomes cloudy or contains visible particles rinse again 6 Separate the parts that were abrasively cleaned from the parts that were not abrasively cleaned 7 Ultrasonically clean the parts each group separately for 15 minutes in each of the following solvents Methylene chloride reagent grade Acetone reagent grade Methanol reagent grade 8 Place the par...

Page 130: ...s engraved into the outer circumference of each lens a Starting with the entrance lens 1 set the lens into the end groove in the lens insulator and rotate the lens until you feel the ball seat into the circular recess b Insert the next 4 lenses in numerical order into the lens insulator The lens chamber open end always faces the entrance lens 1 Rotate each lens until you feel the ball seat into th...

Page 131: ...ers face the full opening extending to the end of the source body Verify that the ceramic is sitting flush at the end of the source body 4 Using the T6 Torx driver install and secure the gold plated setscrew and lock ring lens insulator that holds the lens assembly in place Figure 39 Assembled EI HES Align as shown CAUTION The ceramic insulator must be positioned flat against the source body when ...

Page 132: ...old plated screws using a T6 Torx screwdriver to secure the source mount to the source body 9 Thread the finger grip into the filament block 10 On the side of the filament block opposite the finger grip orient the dual filament ceramic holder so that it lines up with the flat of the filament block Fully insert the three filament leads into the filament block 11 Inset the filament block into the so...

Page 133: ...ber Item description Part number 1 Source finger grip G7002 20008 2 Filament block G7002 20019 3 Extractor lens 5 with 3 mm opening G7002 20061 4 Ceramic insulator for extractor G7002 20064 5 Entrance lens assembly Extended HES 1 G7002 20165 6 Ion focus lens 2 G7002 20068 7 Lens insulator holder G7002 20074 8 M2 x 0 4 screw x 12 mm long gold plated screw G7002 20083 9 Source body G7002 20084 ...

Page 134: ...iciency dual filament G7002 60001 15 Ring heater sensor assembly G7002 60043 16 Source mount 1 5 mm G7002 60053 17 Repeller assembly G7002 60057 Not shown HES assembly G7004 67055 Table 17 Parts list for EI HES Figure 41 continued Item number Item description Part number CAUTION Use care when inserting the lenses into the lens insulator casing Putting excessive stress on this casing can break or c...

Page 135: ...on page 104 2 Open the analyzer chamber See To Open the Analyzer Chamber on page 119 3 Remove the ion source and place it on a clean cloth on your work surface See To Remove the EI HES on page 121 CAUTION Always wear clean gloves to prevent contamination when working in the analyzer chamber WARNING The analyzer GC MS interface and other components in the analyzer chamber operate at very high tempe...

Page 136: ... filament block from the source 6 Remove the dual filament from the filament block by lifting the source body up off of the filament block while holding the filament block so that the dual filament will not fall and become damaged Figure 42 Replacing the dual filament Source mount Screw Filament block Dual filament CAUTION Use extra caution when removing the dual filament as it is extremely brittl...

Page 137: ...ament See To Remove the EI HES filaments on page 135 2 Insert the 3 pins on the dual filament through the rear of the filament block See Figure 42 on page 136 3 Place the filament block in the source mount 4 Use a T6 Torx screwdriver to tighten the screw securing the filament block to the source mount 5 Reinstall the ion source See To Install the EI HES on page 138 6 Close the analyzer chamber See...

Page 138: ...esistance is felt 2 Snap the source into place so that the source mount tabs are flush against the source mount attachment surface of radiator Some force is required to overcome the resistance of the electrical contacts spring loaded surfaces 3 Connect the EI HES wires See To Connect Disconnect Wiring to the EI HES on page 123 4 Install and hand tighten the source thumbscrews Do not overtighten th...

Page 139: ...ring from the EI XTR SS and Inert Sources on page 140 4 Remove the thumbscrews that hold the ion source in place See Figure 50 on page 159 5 Pull the ion source out of the source radiator WARNING The analyzers GC MS interface and other components in the analyzer chamber operate at very high temperatures Do not touch any part until you are sure it is cool CAUTION Always wear clean gloves to prevent...

Page 140: ...zers 8710 2460 Procedure 1 Use tweezers or needle nose pliers to connect disconnect the ceramic source board wire leads at the source connectors See Figure 43 2 Use tweezers or needle nose pliers to connect disconnect the source heater wire leads at the ceramic source board Figure 43 Wiring for the EI XTR Source Extractor lens Source heater Repeller Filament 1 Source RTD Filament 2 Ceramic source ...

Page 141: ...from the source 3 Loosen the two gold plated screws from the source heater block assembly and separate the repeller assembly from the source body The repeller assembly includes the source heater block assembly repeller and related parts 4 Remove the repeller nut and washers then remove the repeller from the source heater block assembly 5 Remove the repeller insulators and the repeller block insert...

Page 142: ... the EI SS or Inert source Figure 44 Item number Item description Part number SS Part number Inert 1 Gold plated set screw G1999 20022 G1999 20022 2 Gold plated screw G3870 20021 G3870 20021 3 Interface socket G1099 20136 G1099 20136 4 Source body G1099 20130 G2589 20043 5 Drawout cylinder G1072 20008 G1072 20008 6 Drawout plate 05971 20134 G2589 20100 7 4 turn filament G7005 60061 G7005 60061 8 S...

Page 143: ...ller insulator G1099 20133 G1099 20133 13 Repeller G3870 60172 G3870 60173 14 Flat washer 3050 0627 3050 0627 15 Belleville spring washer 3050 1301 3050 1301 16 Repeller nut 0535 0071 0535 0071 17 Source heater block assembly G3870 60180 G3870 60179 18 Repeller block insert G3870 20135 G3870 20135 Table 18 Parts list for the EI SS or Inert source Figure 44 continued Item number Item description Pa...

Page 144: ...plated screws and separating the filaments from the source 3 Loosen the two gold plated screws on the source heater block assembly and separate the repeller assembly from the source body The repeller assembly includes the source heater block assembly repeller and related parts 4 Remove the gold plated setscrews from the side of the source body 5 Pull the entrance lens and ion focus lens to remove ...

Page 145: ...R source Table 19 Parts list for EI XTR source Figure 45 Item Description Part number 1 Setscrews G3870 20446 2 Screws G3870 20021 3 Source body G3870 20440 4 Extractor lens G3870 20444 5 Extractor lens insulator G3870 20445 6 Filaments G7005 60061 7 Spring washer 3050 1301 7 Flat washer 3050 0982 ...

Page 146: ...20143 11 Repeller insulator G1099 20113 12 Repeller G3870 60171 13 Flat washer 3050 0891 14 Belleville spring washer 3050 1301 15 Repeller nut 0535 0071 16 Source heater block assembly G3870 60177 17 Repeller block insert G3870 20135 Not shown EI XTR source assembly G7003 67720 Table 19 Parts list for EI XTR source Figure 45 continued Item Description Part number ...

Page 147: ... 8650 0030 Small 8650 0029 Solvents Acetone reagent grade Methanol reagent grade Methylene chloride reagent grade Ultrasonic bath Preparation 1 Disassemble the ion source See To Disassemble the EI SS or EI Inert Source on page 141 or To Disassemble the EI XTR Source on page 144 2 Collect the following parts to be cleaned for an EI SS or Inert source See Figure 46 on page 149 Repeller Interface soc...

Page 148: ... insert Source body Extractor lens Ion focus lens Entrance lens These are the parts that contact the sample or ion beam The other parts normally should not require cleaning CAUTION If insulators are dirty clean them with a cotton swab dampened with reagent grade methanol If that does not clean the insulators replace them Do not abrasively or ultrasonically clean the insulators ...

Page 149: ... cleaned Ion focus lens Entrance lens Drawout cylinder Interface socket Source body EI SS or EI Inert source parts to be cleaned EI XTR source parts to be cleaned Repeller Repeller block insert Entrance lens Ion focus lens Extractor lens Source body Repeller block insert Drawout plate Repeller ...

Page 150: ...cleaned from the parts that were not abrasively cleaned 5 Ultrasonically clean the parts each group separately for 15 minutes For dirty parts use all three solvents in the order shown cleaning 15 minutes with each of the following solvents Methylene chloride reagent grade Acetone reagent grade Methanol reagent grade For routine cleaning cleaning with methanol is sufficient 6 Place the parts in a c...

Page 151: ...sert c Install the repeller through the repeller insulators then put the flat washer followed by the belleville spring washer onto the end of the repeller shaft and secure finger tight with the repeller nut 2 Insert the drawout plate and the drawout cylinder into the source body 3 Assemble the ion focus lens entrance lens and lens insulators 4 Slide these assembled parts into the source body 5 Ins...

Page 152: ...5 14 14 14 2 2 16 16 16 8 12 12 12 10 2 8 8 7 17 18 3 8 8 7 12 13 4 6 5 11 9 Table 20 Parts list for the EI standard or EI Inert source Figure 47 Item number Item description Part number SSL Part number Inert 1 Gold plated set screw G1999 20022 G1999 20022 2 Gold plated screw G3870 20021 G3870 20021 3 Interface socket G1099 20136 G1099 20136 4 Source body G1099 20130 G2589 20043 5 Drawout cylinder...

Page 153: ...0126 11 Ion focus lens 05971 20143 05971 20143 12 Repeller insulator G1099 20133 G1099 20133 13 Repeller G3870 60172 G3870 60173 14 Flat washer 3050 0627 3050 0627 15 Belleville spring washer 3050 1301 3050 1301 16 Repeller nut 0535 0071 0535 0071 17 Source heater block assembly G3870 60180 G3870 60179 18 Repeller block insert G3870 20135 G3870 20135 Table 20 Parts list for the EI standard or EI I...

Page 154: ...nto the source body with the ion focus lens against the extractor lens 5 Install the two gold plated setscrews that holds the lenses in place 6 Assemble the repeller assembly a Install the repeller block insert into the source heater block assembly b Install the repeller insulators into the source heater block assembly and repeller block insert c Install the repeller through the repeller insulator...

Page 155: ... source Table 21 Parts list for EI XTR source Figure 48 Item Description Part number 1 Setscrews G3870 20446 2 Screws G3870 20021 3 Source body G3870 20440 4 Extractor lens G3870 20444 5 Extractor lens insulator G3870 20445 6 Filaments G7005 60061 7 Spring washer 3050 1301 7 Flat washer 3050 0982 ...

Page 156: ...20143 11 Repeller insulator G1099 20113 12 Repeller G3870 60171 13 Flat washer 3050 0891 14 Belleville spring washer 3050 1301 15 Repeller nut 0535 0071 16 Source heater block assembly G3870 60177 17 Repeller block insert G3870 20135 Not shown EI XTR source assembly G7003 67720 Table 21 Parts list for EI XTR source Figure 48 continued Item Description Part number ...

Page 157: ...Vent the MSD See Venting the MSD on page 96 2 Open the analyzer chamber See To Open the Analyzer Chamber on page 119 3 Remove the ion source See To Remove the EI XTR SS or Inert Source on page 139 4 Remove the gold plated screw and washer for the filaments See Figure 49 WARNING The analyzer operates at high temperatures Do not touch any part until you are sure it is cool Figure 49 Changing the fil...

Page 158: ...r on page 162 9 Pumpdown the MSD See To Pump Down the MS on page 106 10 Autotune the MSD See To Run an Autotune on page 102 11 In the Manual Tune dialog the Filament parameter allows you to enter 1 or 2 for the filament number Whichever number was present during the previous autotune enter the other filament number 12 Autotune the MSD again 13 Enter the filament number that gave the best results I...

Page 159: ...iator See Figure 50 2 Insert and hand tighten the source thumbscrews Do not overtighten the thumbscrews See Figure 50 3 Connect the ion source wires See To Connect Disconnect Wiring from the EI XTR SS and Inert Sources on page 140 4 Close the analyzer chamber See To Close the Analyzer Chamber on page 162 Figure 50 Installing the EI source Ceramic source board Ion source Thumbscrews Source heater a...

Page 160: ...e 8710 1094 Procedure 1 Vent the MS See Vent the MSD on page 104 2 Open the analyzer chamber See To Open the Analyzer Chamber on page 119 3 Open the retaining clip See Figure 51 on page 161 Lift the arm of the clip up and swing the clip away from the electron multiplier horn 4 Slide the blue signal wire from the connector in the sideplate 5 Remove the electron multiplier horn 6 Hold the new horn w...

Page 161: ... Operating Manual 161 9 Close the analyzer chamber See To Close the Analyzer Chamber on page 162 Figure 51 Replacing the EM horn on a Series II Detector Figure 52 Electron multiplier horn Retaining clip Electron multiplier horn Blue signal wire ...

Page 162: ...uctions 2 Swing the analyzer side plate closed 3 Ensure the vent valve is closed 4 If hydrogen or other flammable or toxic substance is used for carrier gas gently hand tighten the top thumbscrew on the analyzer side plate 5 Pumpdown the MSD See To Pump Down the MS on page 106 6 Once the MSD has pumped down close the left analyzer cover and replace the window cover 7 Tune the MSD CAUTION Do not fo...

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Page 164: ...www agilent com Agilent Technologies Inc 2019 First Edition January 2019 G7077 90031 G7077 90031 ...

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