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7000/7010 Series TQ GC/MS Operating Manual

129

6

Operating in CI Mode

Setting Up Your MS to Operate in CI Mode    130

Operating the CI MS    131

High Vacuum Pressure in CI Mode    132

Other Reagent Gases    133

CI Autotune    135

The CI Flow Control Module    137

To Operate the Reagent Gas Flow Control Module    139

To Set a Reagent Gas Flow    141

To Perform a CI Autotune    142

To Pumpdown and Switch from EI to CI Mode    144

This chapter provides information and instructions for operating the 
7000/7010 Series TQ GC/MS system in CI mode. Most of the information in the 
preceding chapter is also relevant.

Most of the material is related to methane CI, but one section discusses the use of 
other reagent gases. 

The software contains instructions for setting the reagent gas flow and for 
performing CI autotunes. Autotunes are provided for positive CI (PCI) with methane 
reagent gas and for negative CI (NCI) with any reagent gas.

If you are using the 

Agilent Intuvo 9000 Gas Chromatograph

 with your MS, 

Chemical Ionization (CI) is not currently supported.

Содержание 7010 Series

Страница 1: ...Agilent 7000 7010 Series Triple Quadrupole Operating Manual ...

Страница 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 ...

Страница 3: ...mn Chapter 3 shows you how to install an Agilent Intuvo column connect a flow path from the column through the MS transfer line and into the ion source and maintain the column guard chip 4 Installing 7890 GC Columns Chapter 4 shows you how to prepare Agilent 7890 GC capillary columns for use with the MS install it in the GC oven and connect it to the MS using the GC MS interface 5 Operating in EI ...

Страница 4: ...k See the Agilent 7000 7010 Series TQ GC MS System Quick Start document for information on finding and installing the documentation located on this USB and DVDs To Install Your Hardware Library Insert the disk into your DVD drive and follow the prompts This can be installed by anyone who has authority to copy information onto the receiving computer To Install Your Software Library Insert the memor...

Страница 5: ...rtant Safety Warnings 19 Many internal parts of the MS carry dangerous voltages 19 Electrostatic discharge is a threat to MS electronics 19 Many parts are dangerously hot 20 The oil pan under the rotary vane foreline pump can be a fire hazard 20 Hydrogen Safety 21 Dangers unique to GC MS operation 21 Hydrogen accumulation in an MS 22 Precautions 23 Safety and Regulatory Certifications 24 EMC 25 In...

Страница 6: ... GC MS Interface Using the Self Tightening Column Nut 37 To Install a Capillary Column in the GC MS Interface Using a Standard Column Nut 42 To Install the GC MS Interface Tip Seal 45 The GC MS Interface for an 8890 Series GC 47 3 Installing Intuvo 9000 GC Column Columns 50 Conditioning Intuvo columns 51 Tips and hints 51 Handling the Intuvo 9000 GC Column and Bus Components 52 To Replace an Intuv...

Страница 7: ...face Using the Self Tightening Column Nut 81 To Install a Capillary Column in the GC MS Interface Using a Standard Column Nut 86 To Install the GC MS Interface Tip Seal 89 The GC MS Interface for an 7890 Series GC 91 To Calibrate the Column 93 5 Operating in EI Mode Operating the MS from the Data System 96 Set the IP Address and View TQ Parameters with the WUI 97 To change the network settings of ...

Страница 8: ...12 To Set the Mode for the Optional JetClean System 113 To Set the JetClean Parameters for the Clean Only Mode 114 To Set the CC Gas Flow Rates 115 To Autotune the MS for EI Mode 117 To Open Left Side Panel for Access to the Analyzer Chambers 119 To Pumpdown the MS 120 To Vent the MS 124 To Set the GC MS Interface Temperature from the 7890 GC 126 To Save a Method on the 7890 GC 127 6 Operating in ...

Страница 9: ... Pumpdown and Switch from EI to CI Mode 144 7 General Maintenance Before Starting 148 Scheduled maintenance 148 Tools spare parts and supplies 149 High voltage precautions 149 Dangerous temperatures 149 Ion source cleaning 151 Ammonia 151 Electrostatic discharge 151 Maintaining the Vacuum System 153 Periodic maintenance 153 Other procedures 153 More information is available 153 Maintaining the Ana...

Страница 10: ...o Assemble the EI HES 177 To Assemble the EI XTR Source 182 To Install the EI HES 185 To Install the EI XTR Source 187 To Remove a Filament from the EI XTR Source 189 To Install a Filament on the EI XTR Source 191 To Remove the EI HES Filaments 192 To Install the EI HES Filaments 194 To Close the Front Analyzer Chamber 195 To Remove Left Rear Cover 196 To Open the Rear Analyzer Chamber 198 To Repl...

Страница 11: ...o the EI XTR Source 216 To Connect or Disconnect 7010 Series CI Source Wiring 217 To Connect or Disconnect 7000 Series CI Source Wiring 218 To Switch from the CI Source to an EI XTR Source 219 To Remove the 7000 Series CI Source 220 To Remove the 7010 Series CI Source 221 To Switch from the EI HES to the CI Source 222 To Install the CI EI XTR Source Radiator 223 To Switch from the CI Source to the...

Страница 12: ...12 7000 7010 Series TQ GC MS Operating Manual To Install a CI Source Filament 240 ...

Страница 13: ...y Warnings 19 Hydrogen Safety 21 Safety and Regulatory Certifications 24 Intended Use 28 Cleaning Recycling the Product 28 Accidental Liquid Spill 28 Moving or Storing the MS 28 This section provides general information about the 7000 7010 Series Triple Quad TQ Gas Chromatograph GC Mass Spectrometer MS including a hardware description general safety warnings and hydrogen safety information ...

Страница 14: ...ID Collision induced dissociation CSB Ceramic source board DC Direct current EI Electron impact 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 id Inside diameter Inert Standard EI source constructed of inert materials LAN ...

Страница 15: ... Positive chemical ionization PFDTD Perfluoro 5 8 dimethyl 3 6 9 trioxydodecane calibrant PFTBA Perfluorotributylamine calibrant Quad Quadrupole mass filter RF Radio frequency RFPA Radio frequency power amplifier Torr Unit of pressure 1 mm Hg TQ Triple Quad quadrupole Turbo Split flow turbomolecular vacuum pump XTR EI Extractor source Table 1 Abbreviations continued Abbreviation Definition ...

Страница 16: ...ng the ion source in place under vacuum CI and EI modes available PCI NCI EI Two independently MS heated hyperbolic Quads Single hexapole CC HED EM Independently GC heated GC MS interface with interface tip seal Independently GC controlled CC gas flows Physical description The 7000 7010 Series TQ GC MS is a rectangular box approximately 47 cm high 35 cm wide and 86 cm deep The weight is 59 kg for ...

Страница 17: ...em HED with high sensitivity electronics Bipolar HED power supply for PCI and NCI operation A required methane isobutane gas purifier is provided It removes oxygen water hydrocarbons and sulfur compounds The CI MS system has been optimized to achieve the relatively high source pressure required for CI while still maintaining high vacuum in the CC quadrupoles and detector Special seals along the fl...

Страница 18: ...Description 18 7000 7010 Series TQ GC MS Operating Manual 7000 7010 Series Triple Quadrupole Hardware Description Figure 1 7000 7010 Series TQ GC MS system with 8890 GC ALS 7000 7010 Series TQ MS MS power switch 8890 GC Drawer GC power switch System status LED ...

Страница 19: ... in the instrument The internal wires and cables connected to these boards The wires for any heater oven detector inlet or valve box Electrostatic discharge is a threat to MS electronics The printed circuit boards in the MS can be damaged by electrostatic discharge ESD Do not touch any of the boards unless it is absolutely necessary If you must handle them wear a grounded wrist strap and take othe...

Страница 20: ...working on it Theoilpanundertherotaryvaneforelinepumpcanbe afirehazard Oily rags paper towels and similar absorbents in the oil pan could ignite and damage the pump and other parts of the MS WARNING Be careful when working behind the instrument During cool down cycles the GC emits hot exhaust that can cause burns WARNING The insulation around the inlets detectors valve box and the insulation cups ...

Страница 21: ...e unique to GC or GC MS operation Dangers include but are not limited to Combustion of leaking hydrogen Combustion due to rapid expansion of hydrogen from a high pressure cylinder WARNING The use of hydrogen as a GC carrier gas detector fuel gas or in the optional JetClean system is potentially dangerous WARNING When using hydrogen H2 as the carrier gas or fuel gas be aware that hydrogen gas can f...

Страница 22: ...tely It can also be shut down accidentally by an internal or external failure A MS shutdown does not shut off the flow of carrier gas As a result hydrogen may slowly accumulate in the MS MS automated shutoff valves closed The MSs are equipped with automated shutoff valves for the calibration vial optional JetClean system and the reagent gases Deliberate operator action or various failures can caus...

Страница 23: ...ated in a MS extreme caution must be used when removing it Incorrect startup of a MS filled with hydrogen can cause an explosion WARNING After a power failure the MS may start up and begin the pumpdown process by itself This does not guarantee that all hydrogen has been removed from the system or that the explosion hazard has been removed WARNING You MUST ensure the top thumbscrew on the front ana...

Страница 24: ... MS and allow it to cool for 1 hour 4 Eliminate all potential sources of ignition in the room 5 Open the vacuum manifold of the MS to atmosphere 6 Wait at least 10 minutes to allow any hydrogen to dissipate 7 Start up the GC and MS as normal When using hydrogen gas check the system for leaks to prevent possible fire and explosion hazards based on local Environmental Health and Safety EHS requireme...

Страница 25: ...의하시기 바라 며 가정외의 지역에서 사용하는 것을 목적으 로 합니다 Information The Agilent Technologies 7000 7010 Series TQ GC MS meets the following IEC classifications Equipment Class I Laboratory Equipment Installation Category II and Pollution Degree 2 This unit has been designed and tested in accordance with recognized safety standards and is designed for use indoors If the instrument is used in a manner not specified by...

Страница 26: ...omagnetic 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...

Страница 27: ...t the device and the radio or television are on separate electrical circuits Ensure that all peripheral devices are also certified Ensure that appropriate cables are used to connect the device to peripheral equipment Consult your equipment dealer Agilent Technologies or an experienced technician for assistance Changes or modifications not expressly approved by Agilent Technologies could void the u...

Страница 28: ...n with a damp lint free cloth For recycling contact your local Agilent sales office Accidental Liquid Spill In case of an accidental liquid spill first turn off the MS and remove the power cord from the buildings electrical power supply Then call your local Agilent service representative for assistance Only Agilent trained technicians should service the electrical components inside an MS Moving or...

Страница 29: ... Install a Capillary Column in the GC MS Interface Using the Self Tightening Column Nut 37 To Install a Capillary Column in the GC MS Interface Using a Standard Column Nut 42 To Install the GC MS Interface Tip Seal 45 The GC MS Interface for an 8890 Series GC 47 This chapter shows you how to select install and condition a GC column which must be performed before you operate your MS ...

Страница 30: ...aken Use the flow calculator in the Agilent Instrument Utilities software and Table 3 to determine an acceptable column flow EI and CI systems also have different column outlet flow pressures See Table 7 on page 106 for EI mode and Table 10 on page 132 for CI mode Table 3 Gas flows Feature Gas flows High vacuum pump Split flow turbo Optimal He column gas flow mL min carrier gas 1 to 2 Reagent gas ...

Страница 31: ... your application will help reduce leaks from the assembly Tips and hints The column installation procedure for the 7000 7010 Series TQ GC MS is different from that for previous MSs Using the procedure from another instrument may not work and may damage the column or the MS You can remove old ferrules from column nuts with an ordinary pushpin Always use carrier gas that is at least 99 9995 pure Be...

Страница 32: ...30 for use with Vespel ferrules 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 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 Magnifying loupe Septum may be old used inlet septum To install columns in other types of inlets refer to your GC user information Pro...

Страница 33: ...cutter with your thumb break the column against the edge of the column cutter 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 7 Position the septum under the column nut so that the column extends 4 to 6 mm past the end of the ferrule See Figure 3 on pa...

Страница 34: ...ghten the nut an additional 1 4 to 1 2 turn The column should not slide with a gentle tug 12 Start the carrier gas flow 13 Verify flow by submerging the free end of the column in isopropanol Look for bubbles CAUTION Never use a wrench to tighten a self tightening nut This may result in damage to the nut or instrument Figure 3 Installing a capillary column for a split splitless inlet Insulation cup...

Страница 35: ...perature to the maximum temperature limit for the column 4 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 Install the column in the GC MS interface WARNING Do not condition your capillary column with hydrogen Hydrogen accumulation in the GC oven can result in an explos...

Страница 36: ...Column 36 7000 7010 Series TQ GC MS Operating Manual See also For more information about installing a capillary column refer to Optimizing Splitless Injections on Your GC for High Performance MS Analysis Agilent Technologies publication number 5988 9944EN ...

Страница 37: ...ded Interface tip seal G3870 20542 See Figure 4 and Figure 5 on page 39 Knurled tip seal retainer G3870 20547 Tip seal spring G7005 20024 Column cutter ceramic 5181 8836 or diamond 5183 4620 Flashlight Magnifying loupe Gloves clean lint free 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 i...

Страница 38: ...column cutter to score the column 2 cm from the end 8 While holding the column against the column cutter with your thumb break the column against the edge of the column cutter 9 Inspect the end for jagged edges or burrs If the break is not clean and even repeat steps 6 and 7 CAUTION Always wear clean gloves while handling any parts that go inside the GC or the analyzer chambers WARNING The analyze...

Страница 39: ...umn extends about 1 to 2 mm See Figure 4 For an EI HES Installation the column extends about 4 to 5 mm See Figure 5 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 4 Installing a capillary column in the GC MS interface for an EI XTR or a CI source Column extends 1 2 mm Tip seal GC...

Страница 40: ...ouch the oven walls 14 Install the tip seal spring and knurled tip seal retainer on the GC MS interface Align gently slide and screw the knurled tip seal retainer into the tip seal holder See Figure 4 and Figure 5 on page 39 Figure 6 Installing a capillary column in the GC MS interface Self tightening column nut GC MS interface GC inlet Self tightening inlet nut CAUTION Use care when placing the t...

Страница 41: ... 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 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 front analyzer chamber See To Clos...

Страница 42: ...ning column nut explained in the previous section Materials needed Interface tip seal G3870 20542 See Figure 4 and Figure 5 on page 39 Tip seal spring G7005 20024 Knurled tip seal retainer G3870 20547 Column cutter ceramic 5181 8836 or diamond 5183 4620 Flashlight Magnifying loupe Gloves clean lint free Large 8650 0030 Small 8650 0029 Interface column nut 05988 20066 Ferrules 0 3 mm id for 0 10 mm...

Страница 43: ...nut 7 Use the column cutter to score the column 2 cm from the end 8 While holding the column against the column cutter with your thumb break the column against the edge of the column cutter 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 analyzer chamber operate at very high te...

Страница 44: ...mn does not touch the oven walls 13 Check the nut s tightness after one or two heat cycles retighten as appropriate 14 Install the tip seal spring and knurled tip seal retainer on the GC MS interface Align gently slide and screw the knurled tip seal retainer into the tip seal holder See Figure 4 and Figure 5 on page 39 15 Gently check the alignment of the ion source and the interface tip seal When...

Страница 45: ...r HES is installed See Figure 7 on page 46 2 Remove the interface tip seal spring and knurled tip seal 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 holder finger tight CAUTION Electrostatic discharges to analyzer components are conducted to the side boar...

Страница 46: ...ept 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 Figure 7 GC MS interface tip seal Interface tip seal Knurled tip seal retainer Tip seal holder CAUTION Forcing the analyzer closed if these parts are misaligned will damage...

Страница 47: ... of the interface passes through the side 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 8 The GC MS interface for an 8890 Series GC Ionization chamber...

Страница 48: ...r thermocouple in the interface monitors the temperature The interface tip seal assembly is also required when using the EI XTR source or the HES The interface should be operated in the 250 to 350 C range Subject to that restriction the interface temperature should be slightly higher than the maximum GC oven temperature but never higher than the maximum column temperature When operating in CI mode...

Страница 49: ...00 GC MS Tail 62 To Condition an Intuvo Capillary Column 66 To Install the GC MS Interface Tip Seal 68 The GC MS Interface for a 9000 GC 70 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...

Страница 50: ...lumn flows vary greatly with temperature requiring measurements of the actual flow to be taken Use Table 4 to determine an acceptable column flow and also refer to Table 7 Influence of carrier and CC gas flows on ion vacuum gauge readings on page 106 Table 4 Gas flows Feature Gas flows High vacuum pump Split flow turbo Optimal He column gas flow mL min carrier gas 1 to 2 CC gas flow 3 to 4 Maximum...

Страница 51: ...mn bleed to an insignificant amount that won t adversely contaminate the ion source See To Condition an Intuvo Capillary Column on page 66 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 when handling a gasket Always wear clean gloves when handling the 9000 GC MS Tail WARNING ...

Страница 52: ...he ferrule and the fitting Instead 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 ...

Страница 53: ...lect 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 To Vent the MS on page 124 3 If you are using hydrogen or other flammable gas as a carrier gas close ...

Страница 54: ...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 See Figure 10 Figure 9 9000 GC front door bus door oven door and Intuvo torque driver Bus door Oven door Intuvo torque driver Front door ...

Страница 55: ...mn s click and run 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 57 Figure 10 9000 GC column and related parts SmartID key Column clamps Re...

Страница 56: ...lumns in the GC 14 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 ...

Страница 57: ...let or detector chips 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 i...

Страница 58: ...t polyimide 5 pk for 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 detec...

Страница 59: ... for 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 See Figure 11 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 Gua...

Страница 60: ...p from the inlet base 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 ...

Страница 61: ...010 Series TQ GC MS Operating Manual 61 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 ...

Страница 62: ... inch open end wrench Procedure 1 Vent the MS See To Vent the MS on page 124 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 Wa...

Страница 63: ...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 See Figure 13 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 back a few millimeters A magnet will hold the heater assembly away from...

Страница 64: ...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 14 MS tail heater assembly clamp open with 9000 GC MS Tail removed Figure 15 9000 GC MS Tail removed from GC MS Interface Ferrule release hole Transfer line Bus click and run connection...

Страница 65: ...erface Align gently slide and screw the tip seal into the tip seal holder See To Install the GC MS Interface Tip Seal on page 68 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 sour...

Страница 66: ...r as recommended by the column manufacturer Allow carrier gas to flow through the column at room temperature for 5 minutes 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 within limits 6 Program the column temperature to increase from 120 C to the maximum temper...

Страница 67: ...uvo 9000 GC Column To Condition an Intuvo Capillary Column 7000 7010 Series TQ GC MS Operating Manual 67 7 Hold at the maximum temperature for 30 minutes The column is conditioned and ready to be used with your method ...

Страница 68: ... or HES is installed See Figure 16 on page 69 2 Remove the interface tip seal spring and knurled tip seal 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 holder finger tight CAUTION Electrostatic discharges to analyzer components are conducted to the side b...

Страница 69: ...xcept 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 Figure 16 GC MS interface tip seal Interface tip seal Knurled tip seal retainer Tip seal holder CAUTION Forcing the analyzer closed if these parts are misaligned will dam...

Страница 70: ... 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 along its ...

Страница 71: ... The 9000 GC MS Tail temperature can be set from the Agilent MassHunter GC MS Acquisition software or from the GC A sensor thermocouple in the interface monitors the temperature The GC MS interface 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 GC MS interface temperature should ...

Страница 72: ...3 Installing Intuvo 9000 GC Column The GC MS Interface for a 9000 GC 72 7000 7010 Series TQ GC MS Operating Manual ...

Страница 73: ...pillary Column in the GC MS Interface Using the Self Tightening Column Nut 81 To Install a Capillary Column in the GC MS Interface Using a Standard Column Nut 86 To Install the GC MS Interface Tip Seal 89 The GC MS Interface for an 7890 Series GC 91 To Calibrate the Column 93 This chapter shows you how to select install and condition a GC column which must be performed before you operate your MS ...

Страница 74: ...aken Use the flow calculator in the Agilent Instrument Utilities software and Table 5 to determine an acceptable column flow EI and CI systems also have different column outlet flow pressures See Table 7 on page 106 for EI mode and Table 10 on page 132 for CI mode Table 5 Gas flows Feature Gas flows High vacuum pump Split flow turbo Optimal He column gas flow mL min carrier gas 1 to 2 Reagent gas ...

Страница 75: ... your application will help reduce leaks from the assembly Tips and hints The column installation procedure for the 7000 7010 Series TQ GC MS is different from that for previous MSs Using the procedure from another instrument may not work and may damage the column or the MS You can remove old ferrules from column nuts with an ordinary pushpin Always use carrier gas that is at least 99 9995 pure Be...

Страница 76: ...30 for use with Vespel ferrules 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 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 Magnifying loupe Septum may be old used inlet septum To install columns in other types of inlets refer to your GC user information Pro...

Страница 77: ...utter with your thumb break the column against the edge of the column cutter 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 7 Position the septum under the column nut so that the column extends 4 to 6 mm past the end of the ferrule See Figure 19 on pa...

Страница 78: ...ghten the nut an additional 1 4 to 1 2 turn The column should not slide with a gentle tug 12 Start the carrier gas flow 13 Verify flow by submerging the free end of the column in isopropanol Look for bubbles CAUTION Never use a wrench to tighten a self tightening nut This may result in damage to the nut or instrument Figure 19 Installing a capillary column for a split splitless inlet Insulation cu...

Страница 79: ...perature to the maximum temperature limit for the column 4 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 Install the column in the GC MS interface WARNING Do not condition your capillary column with hydrogen Hydrogen accumulation in the GC oven can result in an explos...

Страница 80: ...Column 80 7000 7010 Series TQ GC MS Operating Manual See also For more information about installing a capillary column refer to Optimizing Splitless Injections on Your GC for High Performance MS Analysis Agilent Technologies publication number 5988 9944EN ...

Страница 81: ...ed Interface tip seal G3870 20542 See Figure 20 and Figure 21 on page 83 Knurled tip seal retainer G3870 20547 Tip seal spring G7005 20024 Column cutter ceramic 5181 8836 or diamond 5183 4620 Flashlight Magnifying loupe Gloves clean lint free 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 ...

Страница 82: ... column cutter to score the column 2 cm from the end 8 While holding the column against the column cutter with your thumb break the column against the edge of the column cutter 9 Inspect the end for jagged edges or burrs If the break is not clean and even repeat steps 6 and 7 CAUTION Always wear clean gloves while handling any parts that go inside the GC or the analyzer chambers WARNING The analyz...

Страница 83: ...mn extends about 1 to 2 mm See Figure 20 For an EI HES Installation the column extends about 4 to 5 mm See Figure 21 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 20 Installing a capillary column in the GC MS interface for an EI XTR or a CI source Column extends 1 2 mm Tip seal ...

Страница 84: ...uch the oven walls 14 Install the tip seal spring and knurled tip seal retainer on the GC MS interface Align gently slide and screw the knurled tip seal retainer into the tip seal holder See Figure 20 and Figure 21 on page 83 Figure 22 Installing a capillary column in the GC MS interface Self tightening column nut GC MS interface GC inlet Self tightening inlet nut CAUTION Use care when placing the...

Страница 85: ... 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 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 front analyzer chamber See To Clos...

Страница 86: ...ing column nut explained in the previous section Materials needed Interface tip seal G3870 20542 See Figure 20 and Figure 21 on page 83 Tip seal spring G7005 20024 Knurled tip seal retainer G3870 20547 Column cutter ceramic 5181 8836 or diamond 5183 4620 Flashlight Magnifying loupe Gloves clean lint free Large 8650 0030 Small 8650 0029 Interface column nut 05988 20066 Ferrules 0 3 mm id for 0 10 m...

Страница 87: ... cm from the end 8 While holding the column against the column cutter with your thumb break the column against the edge of the column cutter 9 Inspect the end for jagged edges or burrs If the break is not clean and even repeat steps 6 and 7 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 compone...

Страница 88: ... s tightness after one or two heat cycles retighten as appropriate 14 Install the tip seal spring and knurled tip seal retainer on the GC MS interface Align gently slide and screw the knurled tip seal retainer into the tip seal holder See Figure 20 and Figure 21 on page 83 15 Gently check the alignment of the ion source and the interface tip seal When the ion source is aligned correctly the front ...

Страница 89: ... HES is installed See Figure 23 on page 90 2 Remove the interface tip seal spring and knurled tip seal 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 holder finger tight CAUTION Electrostatic discharges to analyzer components are conducted to the side boar...

Страница 90: ...pt 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 Figure 23 GC MS interface tip seal Interface tip seal Knurled tip seal retainer Tip seal holder CAUTION Forcing the analyzer closed if these parts are misaligned will damage...

Страница 91: ... of the interface passes through the side 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 24 The GC MS interface for an 8890 Series GC Ionization chambe...

Страница 92: ...r thermocouple in the interface monitors the temperature The interface tip seal assembly is also required when using the EI XTR source or the HES The interface should be operated in the 250 to 350 C range Subject to that restriction the interface temperature should be slightly higher than the maximum GC oven temperature but never higher than the maximum column temperature When operating in CI mode...

Страница 93: ...the Instrument Control panel select Instrument GC Configuration 6 Select the Configuration tab 7 Select the Column tab click Inventory and verify that the column you are using is in inventory Select the column to be calibrated and click Install Selected Column 8 Highlight the column in the inventory list and select Calibrate 9 Select Calc Length 10 In the Calculate Column Length dialog enter the r...

Страница 94: ...brate the Column 94 7000 7010 Series TQ GC MS Operating Manual 11 When the new column length appears click OK to save the changes 12 Click OK on the Calibrate Columns dialog to save the calibration Figure 25 Calculate Column Length dialog ...

Страница 95: ...m Status 107 To Set the MS Analyzer s Temperatures 109 To Set the GC MS Interface Temperature from MassHunter 111 To Configure CC Gas 112 To Set the Mode for the Optional JetClean System 113 To Set the JetClean Parameters for the Clean Only Mode 114 To Set the CC Gas Flow Rates 115 To Autotune the MS for EI Mode 117 To Open Left Side Panel for Access to the Analyzer Chambers 119 To Pumpdown the MS...

Страница 96: ...dditional information is described in the manuals and online help supplied with the MassHunter GC MS Acquisition software Your 7000 TQ operates in EI mode using the EI XTR Ion Source Assembly and your 7010 TQ operates in EI mode using the EI HES Source Assembly which provides higher sensitivity when ionizing the sample CAUTION The software and firmware are revised periodically If the steps in thes...

Страница 97: ...assHunter GC MS Acquisition software use These procedures assume that the operator has access to a PC located on the same LAN subnet as the TQ To change the network settings of the TQ The GC firmware does not support LVDS communications with the 7000 7010 series TQ MS at this time so you must use the Web User Interface WUI to configure the TQ network settings 1 Press the MS On Off switch to start ...

Страница 98: ...ust be an Agilent 7890B or 7890A with the latest firmware for DCOMM support 5 Enter the IP Address Gateway IPA and Subnet Mask for the TQ 6 Click Submit to assign this IP address to the TQ Agilent recommends attaching a label to the TQ recording these NetConfig parameters 7 Close the browser page when you are done 8 Run the Agilent GC MS Instrument Configuration program To configure the TQ for DCO...

Страница 99: ...ration program edit the TQ IP address using these new parameters View the TQ parameters This procedure allows you to monitor TQ parameters without running the MassHunter GC MS Acquisition software It is useful when manually pumping down the TQ and monitoring the instrument s status 1 Press the MS On Off switch to start the instrument 2 Enter the instrument IP address into a PC web browser URL to d...

Страница 100: ... GC MS Operating Manual 3 Click Instrument Status to display the TQ turbo pump speed zone temperatures high vacuum pressure TQ faults net configuration parameters and smart card firmware version See Figure 29 4 When done close the browser Figure 29 WUI instrument status ...

Страница 101: ...atus of the instrument using color codes and LED On Off timing See Table 6 Table 6 Front panel Instrument Status LED codes Instrument status LED code Ready Solid green Acquiring data Blinking green 2 sec Not ready Solid yellow JetClean Acquire Clean operation Blinking magenta JetClean Clean Only operation Solid magenta Ready and not connected to DS Solid blue Start up prior to FW load Blinking red...

Страница 102: ...ean system supply the carrier gas and JetClean system supply shutoff valves must be closed The top thumbscrew on the front analyzer side plate and the top thumbscrew on the rear analyzer side plate must both 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...

Страница 103: ... heater The MS will shut down if it cannot pumpdown correctly Using the MS monitors the data system can display Motor speed for turbo pump MS Analyzer chamber pressure vacuum Foreline pump pressure Controlling Temperatures MS temperatures are controlled through the data system The MS has independent heaters and temperature sensors for the ion source the MS1 mass filter and the MS2 mass filter You ...

Страница 104: ...n page 93 Controlling CC Flow The CC gas flow rate is controlled by an EPC module located in the GC The CC gas flow is a combination of two gases mixed at the EPC outlet and sent in a single tubing line to the MS Typically these two gases are nitrogen and helium though only nitrogen is used when hydrogen is the carrier gas The gas flow rates to the GC CC EPC are controlled by the Agilent MassHunte...

Страница 105: ...ol below 100 C before you vent the MS A temperature of 100 C is hot enough to burn skin always wear cloth gloves when handling analyzer parts WARNING If hydrogen is used as a carrier gas or JetClean system supply the carrier and JetClean system supply shutoff valves must be closed before turning off the MS power If the foreline pump is off hydrogen will accumulate in the MS and an explosion may oc...

Страница 106: ...oubleshooting air leaks and other vacuum problems Table 7 Influence of carrier and CC gas flows on ion vacuum gauge readings CC Gas On N2 1 5 He 2 25 CC Gas Off CC Gas On N2 1 5 He off Column Flow mL min Rough Vac High Vac Rough Vac High Vac Rough Vac High Vac 0 5 1 58 10 1 1 11 10 4 8 82 10 2 6 05 10 7 1 36 10 1 1 31 10 4 0 7 1 61 10 1 1 10 10 4 9 92 10 2 7 75 10 7 1 39 10 1 1 31 10 4 1 1 66 10 1...

Страница 107: ... of a single instrument parameter They can be added to the standard instrument control window Monitors can be set to change color if the actual parameter varies beyond a user determined limit from its setpoint Procedure 1 Select Method Edit Monitors to display the Select Monitors dialog See Figure 30 The available monitors may change due to the configuration of the GC and MS Figure 30 Select Monit...

Страница 108: ...ve the selection to the Selected Monitors column 6 In the Available Monitors column select MS Source Temp and click Add to move the selection to the Selected Monitors column 7 In the Available Monitors column select Foreline Pressure and click Add to move the selection to the Selected Monitors column 8 Select any other monitors you want and add them to the Selected Monitors column 9 Click OK The n...

Страница 109: ...Source tab to display the ion source parameters 2 Enter the temperature setpoint in the Source Temp field See Table 8 for recommended setpoints 3 Select the MS1 tab to display the MS1 parameters See Figure 32 on page 110 4 Enter the temperature setpoint in the MS1 Quad Temp field See Table 8 for the recommended setpoint 5 Select the MS2 tab to display the MS2 parameters 6 Enter the temperature set...

Страница 110: ...rface ion source and the MS1 quadrupole heated zones interact The analyzer heater may not be able to accurately control temperature if the setpoint for one zone is much different from that of an adjacent zone The software will not allow you to exceed 200 C for the quadrupole or 350 C for the source Figure 32 MS1 parameters ...

Страница 111: ...hermal Aux 2 3 Click the heater On check box and type the setpoint in the Value C column The typical setpoint is 280 C The limits are 0 C to 400 C A setpoint below ambient temperature turns off the interface heater 4 Click Apply to download setpoints or click OK to download setpoints and close the window 5 To make the new settings part of the method select Save from the Method menu Figure 33 Setti...

Страница 112: ... page 115 2 Select Instrument GC Parameters from the Instrument Control panel 3 Click the Configuration icon then select the Modules tab to display the screen See Figure 34 4 From the Collision Cell EPC Quench Gas drop down menu select the quench gas 5 From the Collision Cell EPC Collision Gas drop down menu select the collision gas 6 Click OK to save the configuration Figure 34 Configure CC gas ...

Страница 113: ...Clean System 1 Click the MS Parameters icon in the Instrument Control view 2 Click Source Cleaning from the Triple Quadrupole MS Method Editor navigation panel 3 Select a mode from the Operation dropdown menu See Figure 35 For detailed information on the JetClean system see the JetClean Operating manual Figure 35 TQ MS Method Editor Source Cleaning panel ...

Страница 114: ... for the Clean Only Mode 1 Click the MS Parameters icon in the Instrument Control view 2 Select Source Cleaning from the Triple Quadrupole MS Method Editor navigation panel 3 Select Clean Only from the Operation dropdown menu See Figure 36 4 Enter the parameters supplied by your method developer 5 Save the method Figure 36 JetClean set to Clean Only mode ...

Страница 115: ... Click the N2 Collision Gas On check box to allow the N2 collision gas flow 6 Click Apply to download the setpoints or OK to download the setpoints and close the window 7 To make the new settings part of the method select Save from the Method menu NOTE Helium should only be used as a quench gas in the CC when it is also used as the carrier gas When hydrogen is being used as the carrier gas turn of...

Страница 116: ...5 Operating in EI Mode To Set the CC Gas Flow Rates 116 7000 7010 Series TQ GC MS Operating Manual Figure 37 Setting CC gas flow rate ...

Страница 117: ... necessary load a new tune file by clicking on the Files and Report tab then click Load in the Tune File area Select an etune u based tune file for an EI XTR source or an HES_atune U based tune file for a HES and click OK 5 Click the Autotune tab and select EI high sensitivity autotune for an EI HES or XTR source See Figure 38 on page 118 6 Select the Tune from default settings check box if you ar...

Страница 118: ...rinted To stop the autotune before it completes the automatic parameter selection click Abort Autotune The parameters from the last successful autotune are used 10 Review the Tune Report If the results are acceptable and you did not select the Save tune file when done check box save the autotune by clicking the Files and Report tab then click Save Refer to the manuals or online help provided with ...

Страница 119: ... only be opened to access the front and rear analyzer chambers or the analyzer side plates This is necessary to pumpdown clean or change the ion source replace a filament or replace the EM horn If you need to open the left side panel follow this procedure See Figure 39 Procedure Pull gently on the front left window and allow the left side panel to slide forward and down Figure 39 The left side pan...

Страница 120: ...ed in the introduction to this chapter before starting up and pumping down the MS Failure to do so can result in personal injury WARNING If hydrogen is used as a carrier gas or JetClean system supply the carrier and JetClean system supply shutoff valves must be closed before turning off the MS power If the foreline pump is off hydrogen will accumulate in the MS and an explosion may occur Read Hydr...

Страница 121: ... 40 The foreline pump will make a gurgling noise This noise should stop within a minute If the noise continues there is a large air leak in your system probably at the side plate seal the interface column nut or the vent valve 9 Start the Agilent MassHunter GC MS Acquisition software If the TQ was configured for both an EI and a CI source you are prompted for the ion source type that is currently ...

Страница 122: ...o load high temperature settings for the ion source and MS1 and MS2 quads 13 Click Yes to set the source MS1 MS2 at 230 150 150 or click No to set them at 100 100 100 14 The Pumpdown dialog displays See Figure 41 You are prompted to make sure the vent valve is closed 15 Click OK to close the Pumpdown manual step dialog and start the Pumpdown Figure 41 Pumpdown status ...

Страница 123: ... Mode on page 117 or To Perform a CI Autotune on page 142 19 If using the JetClean system prepare the hydrogen system for use Refer to the JetClean Operating manual for warnings regarding hydrogen safety CAUTION Within 10 to 15 minutes the turbo pump speed should be up to 80 The pump speed should eventually reach 95 If these conditions are not met the MS electronics will shut off the foreline pump...

Страница 124: ... load the Fast Vent method to turn off the GC oven and interface heaters the source and quad heaters and the turbo pump If your system does not support DCOMM or if DCOMM has been disabled when prompted you must set the GC MS interface heater and the GC oven temperatures to ambient room temperature 5 Turn off the MS by pressing the power switch See Figure 1 on page 18 6 Unplug the MS power cord WAR...

Страница 125: ...counterclockwise only 3 4 turn or until you hear the hissing sound of air flowing into the analyzer chamber See Figure 42 Do not turn the knob too far or the O ring may fall out of its groove WARNING Allow the analyzers to cool to near room temperature before touching them CAUTION Always wear clean gloves while handling any parts that go inside the analyzer chambers Figure 42 The MS vent valve kno...

Страница 126: ... Scroll to Initial time Enter a value and press Enter 4 Scroll to Rate 1 Enter 0 to end the program here or enter a positive value to create a temperature program If you want the new setpoint saved with a method stored on the GC press OK to save the method You can also upload the GC method to the MassHunter Workstation to save the new setpoints made at the GC keypad When a new method is loaded all...

Страница 127: ...ecific method number 2 Press Store and On Yes to store the new method using the chosen number Alternatively press Off No to return to the stored methods list without saving the method A message is displayed if a method with the number you selected already exists 3 Press On Yes to replace the existing method or Off No to return to the stored methods list without saving the method ...

Страница 128: ...5 Operating in EI Mode To Save a Method on the 7890 GC 128 7000 7010 Series TQ GC MS Operating Manual ...

Страница 129: ...hapter provides information and instructions for operating the 7000 7010 Series TQ GC MS system in CI mode Most of the information in the preceding chapter is also relevant Most of the material is related to methane CI but one section discusses the use of other reagent gases The software contains instructions for setting the reagent gas flow and for performing CI autotunes Autotunes are provided f...

Страница 130: ...se the highest purity methane and other reagent gases if applicable Methane must be at least 99 9995 pure Always verify the MS is performing well in EI mode before switching to CI Ensure the CI source and GC MS interface tip seal are installed Ensure the reagent gas plumbing has no air leaks This is determined in PCI mode checking for m z 32 after the methane pretune Ensure the reagent gas inlet l...

Страница 131: ...be optimized for your specific analyte See Table 9 Start the system in CI mode When starting up the system you may begin in either PCI or NCI mode Depending upon the application use the following reagent gas flowrates during system startup PCI mode set reagent gas flow to 20 1 mL min NCI mode set reagent gas flow to 40 2 mL min Table 9 Temperatures for CI operation Ion source Front analyzer Rear a...

Страница 132: ...uum gauge is calibrated for nitrogen so these measurements are not accurate but are intended as a guide to typical observed readings See Table 10 They were taken with the following set of conditions Note that these are typical PCI temperatures Source temperature 300 C Front quad temperature 150 C Rear quad temperature 150 C Interface temperature 280 C to 320 C Helium carrier gas flow 1 mL min Tabl...

Страница 133: ...actions encountered are described in general in the Agilent 7000 7010 Triple Quadrupole GC MS Concepts Guide If you are not experienced with CI we suggest reviewing that material before you proceed Isobutane CI Isobutane C4H10 is commonly used for CI when less fragmentation is desired in the CI spectrum This is because the proton affinity of isobutane is higher than that of methane hence less ener...

Страница 134: ...ure of 5 ammonia and 95 helium or 5 ammonia and 95 methane is used as a CI reagent gas This is enough ammonia to achieve good CI while minimizing its negative effects Carbon Dioxide CI Carbon dioxide is often used as a reagent gas for CI It has obvious advantages of availability and safety CAUTION Use of ammonia affects the maintenance requirements of the MS See Chapter 7 General Maintenance start...

Страница 135: ...fter the source is changed from EI to CI or vented for any other reason the MS must be purged and baked out for at least 2 hours before tuning Longer bakeout is recommended before running samples requiring optimal sensitivity CAUTION Always verify MS performance in EI before switching to CI operation Table 11 CI tune default settings Parameter Methane Isobutane Ammonia Ion polarity Positive Negati...

Страница 136: ...ng Manual Front quad temp 150 C 150 C 150 C 150 C 150 C 150 C Rear quad temp 150 C 150 C 150 C 150 C 150 C 150 C Interface temp 280 C 280 C 280 C 280 C 280 C 280 C Autotune Yes Yes No Yes No Yes Table 11 CI tune default settings continued Parameter Methane Isobutane Ammonia ...

Страница 137: ...hane CH4 and one other gas The software refers to them as Gas A and Gas B respectively If you are not using a second gas cap the other fitting to prevent accidental admission of air to the analyzer Supply reagent gases at 25 to 30 psi 170 to 205 kPa The shutoff valve prevents contamination of the flow control module by atmosphere while the MS is vented or by PFTBA during EI operation The MS monito...

Страница 138: ...ng For detailed information on the JetClean system refer to the JetClean Operating manual installed on your PC along with this manual The Open and Closed states are shown in the monitors as Opened and Closed Table 12 CI system MFC state Result Gas A flow Gas B flow Purge with Gas A Purge with Gas B Pump out flow module Standby vented or EI mode Gas A Open Closed Open Closed Closed Closed Gas B Clo...

Страница 139: ...g Manual 139 To Operate the Reagent Gas Flow Control Module Procedure 1 In Instrument Control panel select the MS Tune icon to display the Triple Quadrupole MS Tune window Select the Manual Tune tab then select the Ion Source tab to display the ion source parameters See Figure 44 Figure 44 CI flow control ...

Страница 140: ...volumetric flow for the selected reagent gas The actual transmitted by the flow controller is shown next to this entry A good value for PCI is 20 and 40 is a good value for NCI Set Opens the selected reagent gas supply valve and controls the reagent gas flow to the entered setpoint Off Turns off the reagent gas flow Purge Opens the selected reagent gas valve for 6 minutes to clear the system of un...

Страница 141: ... flow setpoint in the CI Gas Flow field This value is entered as a percentage of maximum flow rate The recommended flow is 20 for a PCI source and 40 for an NCI source 4 Click Set The Flow Set indication is displayed The reagent gas is flowing into the ion source at the rate displayed next to the setpoint 5 Click the Files and Reports tab then click Save to save your changes to the currently loade...

Страница 142: ...ce for a positive CI source or NCI source for a negative CI source 5 Click on Methane if you are using methane as the reagent gas or click on Ammonia if using the gas attached to the reagent gas controllers B port as the reagent gas 6 If a log file and associated data files of the tune are required click the Files and Reports tab and in the Log Files section click Browse to create a directory and ...

Страница 143: ...ing the newly generated tune parameters 10 Select the Print autotune report check box to automatically print a tune report 11 Click Autotune to start the autotune The Status line displays the current step in the autotune process and the plot of the tuned parameter for that step is shown in the top graph If specified at the completion of the autotune a Tune Report is printed To stop the autotune be...

Страница 144: ...n See To Pumpdown the MS on page 120 After the software prompts you to turn on the GC MS interface heater and GC oven perform the following steps 2 Load a PCI tune file by clicking on the Files and Report tab then click Load in the Tune File area Select a PCI tune file and click OK Always start up and verify system performance in PCI mode before switching to NCI 3 In Instrument Control view select...

Страница 145: ...Ion Source CI tab and then in the CI Reagent Gas Control area select Gas Valve A for Methane gas See Figure 46 8 Set Gas A methane to 20 9 Set the GC MS interface to 280 C 10 Let the system bake out and purge for at least 2 hours If you will be running NCI for best sensitivity bake out the MS overnight 11 Click the MS Tune icon in the Instrument Control panel to display the Triple Quadrupole MS Tu...

Страница 146: ...also gives higher noise abundance This is adjusted for data acquisition by setting the EMV in the method Peakwidth target Higher peakwidth values give better sensitivity lower values give better resolution Maximum emission current Optimum emission current maximum for NCI is very compound specific and must be selected empirically Optimum emission current for pesticides for example may be about 200 ...

Страница 147: ...le the EI HES 165 To Disassemble the EI XTR Source 168 To Clean the EI HES 171 To Clean the EI XTR Source 174 To Assemble the EI HES 177 To Assemble the EI XTR Source 182 To Install the EI HES 185 To Install the EI XTR Source 187 To Remove a Filament from the EI XTR Source 189 To Install a Filament on the EI XTR Source 191 To Remove the EI HES Filaments 192 To Install the EI HES Filaments 194 To C...

Страница 148: ...riations from normal operation and to take corrective action Table 14 Maintenance schedule Task Frequency Check the foreline pump oil level Every week Check the calibration vial s Every 6 months Replace the foreline pump oil Or as needed Every 6 months Replace dry scroll pump tip seals Every year Tune the MS As needed Check the foreline pump As needed Clean the ion source As needed Check the carri...

Страница 149: ...cables between the boards Wires and cables between the boards and the connectors on the back panel of the MS 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...

Страница 150: ...t from the foreline pump outdoors or into a fume hood vented to the outdoors This requires removing the oil trap Comply with your local air quality regulations The fluids in the foreline pump also collect traces of the samples being analyzed All used pump fluid should be considered hazardous and handled accordingly Dispose of used fluid as specified by your local regulations WARNING Never touch th...

Страница 151: ...nia from getting into the flow module Electrostatic discharge All of the printed circuit boards in the MS contain components that can be damaged by ESD Do not handle or touch these boards unless absolutely necessary In addition wires contacts and cables can conduct ESD to the electronics boards to which they are connected This is especially true of the WARNING When replacing pump fluid use appropr...

Страница 152: ...utions 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 assemblies that have been removed from the MS This i...

Страница 153: ... or as needed depending upon the type of gases being used in the lab 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 an ion vacuum gauge should be performed only when needed Refer the Agilent 7000 7010 Series Triple Quad GC MS Troubleshooting and Maintenance Manual an...

Страница 154: ...e help in the MassHunter Workstation software provides more extensive information Precautions Cleanliness Keep components clean during analyzer maintenance Analyzer maintenance involves opening either analyzer chamber and removing parts from the analyzers During analyzer maintenance procedures avoid contaminating the analyzers or interior of the analyzer chambers Wear clean gloves during all analy...

Страница 155: ... In general the mass filters should never be disturbed In the event of extreme contamination they can be cleaned but such cleaning should only be done by a trained Agilent Technologies service representative More information is available If you need more information about the locations or functions of analyzer components refer to the Agilent 7000 7010 Series Triple Quad GC MS Troubleshooting and M...

Страница 156: ... for Access to the Analyzer Chambers on page 119 3 Loosen the front analyzer side plate thumbscrews if they are fastened See Figure 47 on page 158 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 before you open the analyzer chamber S...

Страница 157: ...ipping The top thumbscrew 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 See Figure 47 on page 158 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 plat...

Страница 158: ...8 7000 7010 Series TQ GC MS Operating Manual Figure 47 The front analyzer chamber on a 7010 MS Ceramic source board Ion source Side plate Post filter Front analyzer Chamber closed Quad driver boards Front analyzer side plate Thumbscrews Rear analyzer side plate ...

Страница 159: ... Figure 48 on page 160 4 Disconnect wiring from the EI HES Do not bend the wires any more than necessary See To Connect or Disconnect Wiring to the EI HES on page 161 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 contamination when w...

Страница 160: ... Manual 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 See Figure 48 Figure 48 The EI HES before removal Ion source Thumbscrew Source finger grip Thumbscrew ...

Страница 161: ...es and videos see To Remove the EI HES on page 159 or To Install the EI HES on page 185 Materials needed Gloves clean lint free Large 8650 0030 Small 8650 0029 Pliers long nose 8710 1094 Tweezers 8710 2460 Procedure Use tweezers or pliers to connect or disconnect the ceramic board wire leads red white black and gray at the source connectors See Figure 49 Figure 49 Wiring for the EI HES Repeller Fi...

Страница 162: ...ber See To Open the Front Analyzer Chamber on page 156 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 contamination when working in the analyzer chamber CAUTION Use an antistatic wrist strap and take other antistatic precautions befor...

Страница 163: ... any more than necessary See To Connect or Disconnect Wiring to the EI XTR Source on page 164 4 Remove the thumbscrews that hold the ion source in place See Figure 50 5 Pull the ion source out of the source radiator Figure 50 Removing the EI XTR source Ceramic source board Ion source Thumbscrews Source heater and temperature sensor wires Source radiator ...

Страница 164: ... the EI XTR Source on page 187 Materials needed Gloves clean lint free Large 8650 0030 Small 8650 0029 Pliers long nose 8710 1094 Tweezers 8710 2460 Procedure 1 Use tweezers or pliers to connect or disconnect the ceramic board wire leads at the source connectors 2 Use tweezers or pliers to connect or disconnect the source heater wire leads at the ceramic source board CSB See Figure 51 Figure 51 Wi...

Страница 165: ...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 body 7 Remove the repeller and ring heater sensor assembly from the source body...

Страница 166: ...his casing can break or crack it If this happens do not attempt to operate with a defective lens insulator it must be replaced Figure 52 Exploded parts view of the EI HES 1 2 8 16 17 15 9 4 3 11 10 6 5 7 13 12 14 8 12 Table 15 Parts list for EI HES Figure 52 Item number Item description Part number 1 Source finger grip G7002 20008 2 Filament block G7002 20019 3 Extractor lens 5 with 3 mm opening G...

Страница 167: ...g gold plated screw G7002 20083 9 Source body G7002 20084 10 Post extractor lens 2 3 G7004 20090 11 Post extractor lens 1 4 G7004 20004 12 M2 x 6 mm gold plated screw G7002 20109 13 Locking ring lens insulator G7002 20126 14 High efficiency 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...

Страница 168: ...rce See To Remove the EI XTR Source on page 162 2 Remove the filaments See To Remove a Filament from the EI XTR Source on page 189 3 Separate the source heater assembly from the source body by removing the two screws The source heater assembly includes the source heater repeller and related parts See Figure 53 and Table 16 on page 169 4 Disassemble the repeller assembly by removing the repeller nu...

Страница 169: ...ssembling the EI XTR source Table 16 Parts list for EI XTR source Figure 53 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 ...

Страница 170: ...n focus lens 05971 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 16 Parts list for EI XTR source Figure 53 continued Item Description Part number ...

Страница 171: ...l reagent grade Methylene chloride reagent grade Acetone reagent grade Ultrasonic bath Procedure 1 Disassemble the ion source See To Disassemble the EI HES on page 165 or To Disassemble the EI XTR Source on page 168 2 Collect the following parts to be cleaned if you are cleaning an EI HES See Figure 54 on page 172 Repeller Source body Extractor lens 5 Post extractor lens 1 4 Post extractor lens 2 ...

Страница 172: ...asively clean the discolorations where electrons from the filaments enter the source body 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 Figure 54 EI HES parts to be cleaned Source body Repeller Entrance lens 1 Ion focus lens 2 Post extract...

Страница 173: ...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 parts in a clean beaker Loosely cover the beaker with clean aluminum foil dull side down 9 Dry the cleaned parts in an oven at 100 C for 5 6 minutes CAUTION Always wear clean glo...

Страница 174: ...e Large 8650 0030 Small 8650 0029 Solvents Acetone reagent grade Methanol reagent grade Methylene chloride reagent grade Ultrasonic bath Preparation 1 Disassemble the EI XTR source See To Disassemble the EI XTR Source on page 168 2 Collect the following parts to be cleaned for an EI XTR source See Figure 55 on page 175 Repeller Repeller block insert Entrance lens Ion focus lens Extractor lens Sour...

Страница 175: ...parts is not necessary small scratches will not harm performance Also abrasively clean the discolorations where electrons from the filaments enter the source body 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 CAUTION The filaments source h...

Страница 176: ...er 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 clean beaker Loosely cover the beaker with clean aluminum foil dull side down 7 Dry the cleaned parts in an oven at 100 C for five to six minutes WARNING Al All of these solven...

Страница 177: ...e in the lens insulator and rotate the lens until you feel the ball seat into the circular recess on the back of the lens insulator b Insert the next 4 lenses in numerical order into the lens insulator The lens chamber open end always faces the extended entrance lens 1 Rotate each lens until you feel the ball seat into the circular recess It is easier to insert lens 5 on an angle because the lens ...

Страница 178: ...bers 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 See Figure 57 Figure 56 Assembled EI HES lens stack Grooves aligned CAUTION The ceramic insulator must be positioned flat ag...

Страница 179: ...ted screws using a T6 Torx screwdriver to secure the source mount to the source body 9 Thread the finger grip into the filament block See Figure 58 and Table 17 on page 180 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 Inse...

Страница 180: ...gure 58 Item number Item description Part number 1 Source finger grip G7002 20008 2 Filament block G7002 20019 3 Extractor lens 5 with 3 mm opening G7004 20061 4 Ceramic insulator for extractor G7002 20064 5 Entrance lens assembly Extended HES 1 G7004 20065 6 Ion focus lens 2 G7004 20068 7 Lens insulator holder G7002 20074 8 M2 0 4 screw 12 mm long gold plated screw G7002 20083 9 Source body G7002...

Страница 181: ...t extractor lens 1 4 G7004 20004 12 M2 6 mm gold plated screw G7002 20109 13 Locking ring lens insulator G7002 20126 14 High efficiency 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 67056 Table 17 Parts list for EI HES Figure 58 continued Item number Item description Part number ...

Страница 182: ...lens insulator to the extractor lens and slide them into the source body See Figure 59 on page 183 3 Slide the parts assembled in step 1 into the source body 4 Install the setscrew that holds the lenses in place 5 Assemble the repeller assembly by attaching the repeller repeller insulators washers and repeller nut onto the source heater assembly 6 Attach the repeller assembly to the source body wi...

Страница 183: ...mbling the EI XTR source Table 18 Parts list for EI XTR source Figure 59 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 ...

Страница 184: ...focus lens 05971 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 18 Parts list for EI XTR source Figure 59 continued Item Description Part number ...

Страница 185: ... on page 156 3 Align the ion source so that the slotted opening for the lens stack where the lens numbers are visible is on the right side Also position it so the two attachment tabs of the source mount align with the corresponding slots in the source radiator See Figure 60 Slide the ion source into the source radiator until resistance is felt CAUTION Always wear clean gloves when working in the a...

Страница 186: ...stance of the electrical contacts spring loaded surfaces 5 Connect the ion source wires See To Connect or Disconnect Wiring to the EI HES on page 161 6 Install and hand tighten the source thumbscrews Do not overtighten the thumbscrews See Figure 60 on page 185 7 Close the front analyzer chamber See To Close the Front Analyzer Chamber on page 195 8 Pumpdown the MS See To Pumpdown the MS on page 120...

Страница 187: ... the MS on page 124 2 Open the front analyzer chamber See To Open the Front Analyzer Chamber on page 156 3 Slide the ion source into the source radiator See Figure 61 on page 188 4 Install and hand tighten the source thumbscrews Do not overtighten the thumbscrews See Figure 61 on page 188 5 Connect the ion source wires See To Connect or Disconnect Wiring to the EI XTR Source on page 164 CAUTION Al...

Страница 188: ...lyzer chamber See To Close the Front Analyzer Chamber on page 195 7 Pumpdown the MS See To Pumpdown the MS on page 120 8 Tune the MS See To Autotune the MS for EI Mode on page 117 Figure 61 Installing the EI XTR source on a 7000 Series MS Ion source Thumbscrews Source radiator Source heater and temperature sensor wires ...

Страница 189: ...zer chamber See To Open the Front Analyzer Chamber on page 156 3 Remove the ion source See To Remove the EI XTR Source on page 162 4 Remove the screws holding the filaments to the ion source body See Figure 62 on page 190 5 Slide the filaments off the ion source assembly See Figure 62 on page 190 CAUTION Always wear clean gloves to prevent contamination when working in the analyzer chamber WARNING...

Страница 190: ...7 General Maintenance To Remove a Filament from the EI XTR Source 190 7000 7010 Series TQ GC MS Operating Manual Figure 62 Changing the EI XTR filament Screw Filament Ion source body ...

Страница 191: ...from the EI XTR Source on page 189 2 Place the new filament into its position on the ion source body See Figure 62 on page 190 3 Secure the filament to the ion source body with the screw 4 After installing the filament verify that it is not grounded to source body 5 Reinstall the ion source See To Install the EI XTR Source on page 187 6 Close the front analyzer chamber See To Close the Front Analy...

Страница 192: ...source and place it on a clean cloth on your work surface See To Remove the EI HES on page 159 4 Remove the screw securing the filament block to the source mount See Figure 63 5 Use the hand grip on the filament block to remove the filament block from the source CAUTION Always wear clean gloves to prevent contamination when working in the analyzer chamber WARNING The analyzer GC MS interface and o...

Страница 193: ...nual 193 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 CAUTION Use extra caution when removing the dual filament as it is extremely brittle ...

Страница 194: ... To Remove the EI HES Filaments on page 192 2 Insert the three pins on the dual filament through the rear of the filament block See Figure 63 on page 192 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 185 6 Close the front analyzer chamber Se...

Страница 195: ...hould slide into place with minimal pressure 3 Ensure the rear analyzer door is closed 4 Ensure the vent valve is closed 5 If hydrogen or an other flammable or toxic substance is used for carrier gas gently hand tighten the top thumbscrew on the front analyzer side plate 6 Pumpdown the MS See To Pumpdown the MS on page 120 7 Once the MS has pumped down close the left analyzer cover and replace the...

Страница 196: ...s the rear analyzer chamber follow these procedures to remove the rear cover See Figure 64 on page 197 Materials needed Screwdriver Torx T 10 and T 20 Procedure 1 Loosen the top screw of the rear cover It is captive so you will not be able to remove it entirely See Figure 64 on page 197 2 Lift the bottom flap of the cover out of the groove in the back of the MS to free the cover WARNING Do not rem...

Страница 197: ...7 General Maintenance To Remove Left Rear Cover 7000 7010 Series TQ GC MS Operating Manual 197 Figure 64 Removing covers Rear cover Analyzer window cover Left side panel Rear cover screw ...

Страница 198: ...pen Left Side Panel for Access to the Analyzer Chambers on page 119 4 Loosen the rear analyzer side plate thumbscrews if they are fastened See Figure 65 on page 200 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 before you open the ...

Страница 199: ...for the rear analyzer side plate should have their threads engaged during normal operation 5 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 ...

Страница 200: ...ear Analyzer Chamber 200 7000 7010 Series TQ GC MS Operating Manual Figure 65 The rear analyzer chamber Rear analyzer side plate Detector board Thumbscrews Chamber closed Collision cell Rear analyzer Detector Rear side plate Chamber open ...

Страница 201: ... 8710 1094 Procedure 1 Vent the MS See To Vent the MS on page 124 2 Open the rear analyzer chamber See To Open the Rear Analyzer Chamber on page 198 3 Slide the blue signal wire from the connector in the side plate See Figure 66 on page 202 4 Open the retaining clip See Figure 66 on page 202 Lift the arm of the clip up and swing the clip away from the EM horn 5 Remove the EM horn 6 Hold the new ho...

Страница 202: ...10 Series TQ GC MS Operating Manual 9 Close the rear analyzer chamber See To Close the Rear Analyzer Chamber on page 203 Figure 66 Replacing the EM horn on a Series 2 detector Figure 67 EM horn for a Series 2 detector Retaining clip EM horn Blue signal wire ...

Страница 203: ...both rear analyzer side panel thumbscrews and gently hand tighten them Do not over tighten the thumbscrews this can cause air leaks 4 Ensure the front analyzer side plate is closed 5 Ensure the vent valve is closed 6 Pumpdown the MS See To Pumpdown the MS on page 120 7 If hydrogen or any other flammable material is used for the carrier gas gently hand tighten the top thumbscrew on the front analyz...

Страница 204: ...7 General Maintenance To Close the Rear Analyzer Chamber 204 7000 7010 Series TQ GC MS Operating Manual ...

Страница 205: ...om the CI Source to an EI XTR Source 219 To Remove the 7000 Series CI Source 220 To Switch from the EI HES to the CI Source 222 To Install the CI EI XTR Source Radiator 223 To Switch from the CI Source to the EI HES 225 To Install a CI Source Filament 226 To Remove the CI Source Radiator from the 7010 Series TQ 227 To Disassemble the CI Source 229 To Clean the CI Source 232 To Assemble the CI Sour...

Страница 206: ...more frequently Always purge the MS with methane after using ammonia Install the ammonia with the tank in an upright position This will help prevent liquid ammonia from getting into the flow module To set up your MS for CI operation Setting up your MS for operation in CI mode requires special care to avoid contamination and air leaks Guidelines Before venting in EI mode for the installation of the...

Страница 207: ... EI XTR Source on page 164 5 Install the CI source See To Install the 7010 Series CI Source on page 211 6 Close the analyzer See To Close the Front Analyzer Chamber on page 195 7 Pumpdown and switch from EI to CI mode See To Pumpdown and Switch from EI to CI Mode on page 144 CAUTION Always verify MS performance in EI before switching to CI operation Always set up the CI MS in PCI first even if you...

Страница 208: ...e wires any more than necessary See To Connect or Disconnect EI HES Radiator Wiring on page 210 5 Use a T10 Torx screwdriver to loosen the two screws that secure the radiator to the analyzer and place the radiator in its storage container See Figure 68 on page 209 WARNING The analyzers GC MS interface and other components in the analyzer chamber operate at very high temperatures Do not touch any p...

Страница 209: ...8 CI Maintenance To Remove the EI HES Radiator 7000 7010 Series TQ GC MS Operating Manual 209 Figure 68 Removing the EI HES radiator Radiator screw Radiator screw HES radiator ...

Страница 210: ...es clean lint free Large 8650 0030 Small 8650 0029 Pliers long nose 8710 1094 Procedure 1 Use tweezers or needle nose pliers to connect or disconnect the green ground wire and the five lens wires from the radiator Do not bend the wires any more than necessary See Figure 69 2 Use tweezers or needle nose pliers to connect or disconnect the two purple source heater wires and the two gray RTD wires fr...

Страница 211: ... to the CI source See To Connect or Disconnect 7010 Series CI Source Wiring on page 217 6 Close the analyzer door See To Close the Front Analyzer Chamber on page 195 7 Pumpdown the MS See To Pumpdown the MS on page 120 8 Tune the MS See CI Autotune on page 135 CAUTION Electrostatic discharges to analyzer components are conducted to the side board where they can damage sensitive components Wear a g...

Страница 212: ... to the CI source See To Connect or Disconnect 7000 Series CI Source Wiring on page 218 6 Close the analyzer door See To Close the Front Analyzer Chamber on page 195 7 Pumpdown the MS See To Pumpdown the MS on page 120 8 Tune the MS See CI Autotune on page 135 CAUTION Electrostatic discharges to analyzer components are conducted to the side board where they can damage sensitive components Wear a g...

Страница 213: ...olumn from the GC MS Interface 9 Cut the column on the tapered side of the ferrule to remove the ferrule 10 Install the column into the GC MS interface See To Install a Capillary Column in the GC MS Interface Using the Self Tightening Column Nut on page 37 or To Install a Capillary Column in the GC MS Interface Using a Standard Column Nut on page 42 11 Remove the EI HES radiator from the storage c...

Страница 214: ... gold plated screws G7002 20110 See Figure 72 on page 215 2 Attach the wires to the radiator or CSB Do not bend the wires any more than necessary See To Connect or Disconnect EI HES Radiator Wiring on page 210 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 c...

Страница 215: ...8 CI Maintenance To Install the EI HES Radiator 7000 7010 Series TQ GC MS Operating Manual 215 Figure 72 Securing the EI HES radiator Radiator screw Radiator screw HES radiator ...

Страница 216: ...on page 156 4 Remove the CI source See To Remove the 7000 Series CI Source on page 220 5 Install the EI XTR source See To Install the EI XTR Source on page 187 6 Place the CI source in the storage container 7 Pumpdown the MS See To Pumpdown the MS on page 120 CAUTION Always wear clean gloves while touching the analyzer or any other parts that go inside the analyzer chamber CAUTION Electrostatic di...

Страница 217: ... Series CI Source on page 211 Materials needed Gloves clean lint free Large 8650 0030 Small 8650 0029 Pliers long nose 8710 1094 Tweezers 8710 2460 Procedure 1 Use tweezers or pliers to connect or disconnect the ceramic board wire leads red white black and gray at the source connectors See Figure 73 2 Use tweezers or pliers to connect or disconnect the source heater wire leads at the CSB Figure 73...

Страница 218: ... Install the 7000 Series CI Source on page 212 Materials needed Gloves clean lint free Large 8650 0030 Small 8650 0029 Pliers long nose 8710 1094 Tweezers 8710 2460 Procedure 1 Use tweezers or pliers to connect or disconnect the ceramic board wire leads at the source connectors See Figure 74 2 Use tweezers or pliers to connect or disconnect the source heater wire leads at the CSB Figure 74 Wiring ...

Страница 219: ...o Install the EI XTR Source on page 187 5 Place the CI source in the ion source storage box 6 If installing an EI SS or Inert source remove the interface tip seal and put it in the CI storage container 7 Pumpdown the MS See To Pumpdown the MS on page 120 8 Load your EI tune file and Tune the MS CAUTION Always wear clean gloves while touching the analyzer or any other parts that go inside the analy...

Страница 220: ...Series CI Source Wiring on page 218 4 Remove the two large thumbscrews that hold the ion source in place 5 Pull the ion source out of the source radiator and place it in its storage container 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 pre...

Страница 221: ...Series CI Source Wiring on page 217 4 Remove the two large thumbscrews that hold the ion source in place 5 Pull the ion source out of the source radiator and place it in its storage container 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 pre...

Страница 222: ...iator in the storage container 8 Remove the CI source radiator from the storage container 9 Install the CI source radiator See To Install the CI EI XTR Source Radiator on page 223 10 Remove CI source from the storage container 11 Install the CI source This requires shortening the column so that it protrudes from the transfer line by 1 to 2 mm See To Install the 7010 Series CI Source on page 211 12...

Страница 223: ...ng the two retained screws with a number T10 Torx screwdriver Make sure the insulators are in place under the screws 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 contamination when working in the analyzer chamber CAUTION Use an anti...

Страница 224: ...ll the CI EI XTR Source Radiator 224 7000 7010 Series TQ GC MS Operating Manual 2 Connect the green ground wire to the radiator See Figure 75 Figure 75 CI Source radiator Green ground wire Radiator Radiator screw Radiator screw ...

Страница 225: ...9 Cut the column on the tapered side of the ferrule to remove the ferrule 10 Install the column into the GC MS interface extending 4 to 5 mm past the analyzer end of the transferline See To Install a Capillary Column in the GC MS Interface Using the Self Tightening Column Nut on page 37 or To Install a Capillary Column in the GC MS Interface Using a Standard Column Nut on page 42 11 Remove the EI ...

Страница 226: ...Remove the old filament See To Remove the CI Source Filament on page 238 2 Place the new filament into its position on the ion source body See Figure 80 on page 239 3 Secure the filament to the ion source body with the screw 4 After installing the filament verify that it is not grounded to source body 5 Reinstall the CI source See To Install the 7010 Series CI Source on page 211 or see To Remove t...

Страница 227: ...ng the 7010 side plate 1 Remove the CI source See To Remove the 7010 Series CI Source on page 221 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 contamination when working in the analyzer chamber CAUTION Make sure you use an antistati...

Страница 228: ...nual 2 Disconnect the green ground wire from the radiator See Figure 76 3 Use a T 10 Torx screwdriver to loosen the two retained screws that secure the radiator to the analyzer and place the radiator in its storage container Figure 76 CI EI XTR Source radiator Green ground wire Radiator Radiator screw Radiator screw ...

Страница 229: ...age 230 1 Remove the CI source See To Remove the 7000 Series CI Source on page 220 2 Remove the filaments See To Remove the CI Source Filament on page 238 3 Separate the source heater assembly from the source body The source heater assembly includes the source heater repeller and related parts See Figure 77 and Table 19 on page 230 4 Disassemble the repeller assembly by removing the ceramic insula...

Страница 230: ...9 11 10 2 15 14 15 14 Table 19 Parts list for CI source Figure 77 Item Description Part number 1 Set screw G1999 20022 2 Filament screw G1999 20021 3 CI repeller insulator G1999 20433 4 CI lens insulator G3170 20540 5 CI drawout cylinder G1999 20444 6 CI drawout plate G1999 20446 7 CI source heater block assembly G3870 60415 8 Entrance lens G7000 20026 ...

Страница 231: ...0072 13 Dummy filament G1999 60454 14 Washer spring curved 2 2 mm ID 4 5 mm OD Qty 2 3050 1374 15 Flat washer 3050 9082 Not shown Package GC MS source Clamshell G7002 80008 Not shown Bracket GC MS source Clamshell G7002 00008 Not shown CI source assembly G7002 67404 Not shown CI source assembly without tip seal G7077 67404 Table 19 Parts list for CI source Figure 77 continued Item Description Part...

Страница 232: ...free Large 8650 0030 Small 8650 0029 Solvents Acetone reagent grade Methanol reagent grade Methylene chloride reagent grade Ultrasonic bath Preparation 1 Disassemble the CI source See To Disassemble the CI Source on page 229 2 Collect the following parts to be cleaned for a CI source See Figure 78 on page 233 Repeller Source body Drawout plate Drawout cylinder Ion focus lens Entrance lens These ar...

Страница 233: ...e electrons from the filaments enter the source body 3 Rinse away all abrasive residue with reagent grade methanol Make sure all abrasive residue is rinsed before ultrasonic cleaning If the methanol becomes cloudy or contains visible particles rinse again three times 4 Separate the parts that were abrasively cleaned from the parts that were not abrasively cleaned CAUTION If the CI lens insulator i...

Страница 234: ...ing cleaning with methanol is sufficient 6 Place the parts in a clean beaker Loosely cover the beaker with clean aluminum foil dull side down 7 Dry the cleaned parts in an oven at 100 C for five to six minutes WARNING Al All of these solvents are hazardous Work in a fume hood and take all appropriate precautions WARNING Let Let the parts cool before you handle them NOTE Take care to avoid contamin...

Страница 235: ...6 1 Assemble the ion focus lens entrance lens and lens insulator See Figure 79 and Table 20 on page 236 2 Slide the drawout plate and the drawout cylinder into the source body See Figure 79 on page 236 3 Slide the parts assembled in step 1 into the source body 4 Install the setscrew that holds the lenses in place 5 Attach the ceramic disk to the repeller and place on top of the source body 6 Place...

Страница 236: ...1 10 2 15 14 15 14 Table 20 Parts list for CI source Figure 79 Item Description Part number 1 Set screw G1999 20022 2 Filament screw G1999 20021 3 CI repeller insulator G1999 20433 4 CI lens insulator G3170 20540 5 CI drawout cylinder G1999 20444 6 CI drawout plate G1999 20446 7 CI source heater block assembly G3870 60415 8 Entrance lens G7000 20026 ...

Страница 237: ...72 13 Dummy filament G1999 60454 14 Washer spring curved 2 2 mm ID 4 5 mm OD Qty 2 3050 1374 15 Flat washer 3050 9082 Not shown Package GC MS source Clamshell G7002 80008 Not shown Bracket GC MS source Clamshell G7002 00008 Not shown CI source assembly G7002 67404 Not shown CI source assembly without tip seal G7077 67404 Table 20 Parts list for CI source Figure 79 continued Item Description Part n...

Страница 238: ... To Open the Front Analyzer Chamber on page 156 3 Remove the CI source See To Remove the 7000 Series CI Source on page 220 4 Remove the screw holding the filament to the CI source body See Figure 80 on page 239 5 Slide the filament off the CI source assembly See Figure 80 on page 239 CAUTION Always wear clean gloves to prevent contamination when working in the analyzer chamber WARNING The analyzer...

Страница 239: ...8 CI Maintenance To Remove the CI Source Filament 7000 7010 Series TQ GC MS Operating Manual 239 Figure 80 Changing the CI source filament Screw Filament CI source body ...

Страница 240: ...cedure 1 Remove the old filament See To Remove the CI Source Filament on page 238 2 Place the new filament into its position on the ion source body See Figure 80 on page 239 3 Secure the filament to the ion source body with the screw 4 After installing the filament verify that it is not grounded to source body 5 Reinstall the CI source See To Install the 7010 Series CI Source on page 211 6 Pumpdow...

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Страница 242: ...www agilent com Agilent Technologies Inc 2019 First edition January 2019 G7003 90050 G7003 90050 ...

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