Agilent Technologies 5973N Скачать руководство пользователя

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Checklists

Hardware Installation

MSD ChemStation software autotune descriptions

❏

Various autotunes described

❏

Importance of retaining tuning records emphasized

❏

Ion source contamination, diagnosis of contamination, and
use of control charts discussed

❏

EI autotune demonstrated and tune report explained

❏

Manual tune explained

❏

View Tunes utility demonstrated and its importance
explained

❏

PCI Autotune performed (if applicable)

❏

NCI Autotune performed (if applicable)

❏

Optimization of reagent gas and application dependency on
gas flow, source temperature, and emission current
discussed

❏

Importance of retaining tuning and maintenance records
discussed

Methods

❏

Edit entire method demonstrated with OFN_SN.M,
explaining the GC and MS Scan Parameters.

❏

Method save demonstrated

Data Acquisition

❏

Analytical method developed to run both scan and SIM

❏

Steps involved in acquiring data and editing an entire
method described

❏

File designated to store the data; data file naming
demonstrated

❏

Acquisition parameters saved as part of a method

Содержание 5973N

Страница 1: ...Agilent Technologies 5973N and 5973 inert Mass Selective Detector Hardware Installation ...

Страница 2: ...all not be liable for errors or for incidental or consequential damages in connec tion with the furnishing use or per formance of this document or of any information contained herein Should Agilent and the user have a separate written agreement with warranty terms covering the material in this document that conflict with these terms the warranty terms in the sep arate agreement shall control Safet...

Страница 3: ...dangerously hot 11 Hydrogen 11 Safety and Regulatory Certifications 13 Information 13 Symbols 14 Electromagnetic compatibility 15 Sound emission certification for Federal Republic of Germany 15 Cleaning 16 Recycling the Product 16 Customer Responsibilities 17 Before You Start 18 Other Documentation 19 2 Installation Overview 22 Unpacking and Inspecting the Materials 23 Installing the GC 24 Connect...

Страница 4: ...rmance 41 Switching from EI to CI Operating Mode 42 Verifying CI System Performance 43 Verify PCI performance 43 Verify NCI performance 43 Familiarizing the Customer 44 3 Checklists Installation Checklist 46 Verifying that site preparation is complete 46 Unpacking and inspecting the shipped materials 46 GC installation 47 MSD installation 48 MSD ChemStation PC installation 50 Performance verificat...

Страница 5: ...tware autotune descriptions 55 Methods 55 Data Acquisition 55 Data analysis 56 Sequence 56 MSD ChemStation maintenance 56 EI Instrument user maintenance 56 Troubleshooting Diagnostics 57 Remote operation modem setup if applicable 57 Tune charts 58 Additional support information 58 ...

Страница 6: ...6 Hardware Installation ...

Страница 7: ...13 Cleaning 16 Recycling the Product 16 Customer Responsibilities 17 Before You Start 18 Other Documentation 19 This section provides information on how to identify specifically what type of MSD you are working with as well as how to properly clean and dispose of the instrument Also included in this section are the Important Safety Warnings which list critical safety precautions for all users ...

Страница 8: ...ective Detectors MSDs are turbo pump MSDs This document will refer to the 5973N MSD or 5973 inert MSD as 5973 Series MSD unless otherwise noted The 5973 Series MSD system consists of 5973N or 5973 inert MSD Optional 59864B vacuum gauge controller required for CI operation Gas Chromatograph 6890 Series GC with options for MSD use 7683 Automatic Liquid Sampler optional PC and MSD ChemStation softwar...

Страница 9: ...ump Performance turbo pump CI No No No PCI NCI 59864B gauge controller Recommended Recommended Recommended Required DIP compatible 3rd party Yes Yes Yes No Figure 1 5973 Series MSD system 6890 Series Gas Chromatograph 5973 Series MSD 6890 Series ALS tower CI gas flow module EI PCI NCI MSDs only 6890 Series ALS tray 59864B high vacuum Gauge Controller 5973 Series MSD LCP ...

Страница 10: ...es and cables connected to these boards The wires for any heater oven detector inlet or valve box Electrostatic discharge is a threat to MSD electronics The printed circuit PC boards in the MSD can be damaged by electrostatic discharge Do not touch any of the boards unless it is absolutely necessary If you must handle them wear a grounded wrist strap and take other antistatic precautions Wear a gr...

Страница 11: ...ench and wear gloves Whenever possible cool the part of the instrument that you will be maintaining before you begin working on it Hydrogen Hydrogen gas may be used as carrier gas and or as fuel for the FID When mixed with air hydrogen can form explosive mixtures WARNING Be careful when working behind the instrument During cool down cycles the MSD emits hot exhaust which can cause burns WARNING Th...

Страница 12: ...t the supply is off until all connections are made and ensure that the inlet and detector column fittings are either connected to a column or capped at all times when hydrogen gas is supplied to the instrument Hydrogen is flammable Leaks when confined in an enclosed space may create a fire or explosion hazard In any application using hydrogen leak test all connections lines and valves before opera...

Страница 13: ...AUS NZ This ISM device complies with Canadian ICES 001 Cet appareil ISM est conforme a la norme NMB 001 du Canada The 5973 Series Mass Selective Detector is designed and manufactured under a quality system registered to ISO 9001 Information The Agilent Technologies 5973 inert Mass Selective Detector meets the following IEC International Electro technical Commission classifications Safety Class I T...

Страница 14: ...anual or on the instrument must be observed during all phases of operation service and repair of this instrument Failure to comply with these precautions violates safety standards of design and the intended use of the instrument Agilent Technologies assumes no liability for the customer s failure to comply with these requirements See accompanying instructions for more information Indicates a hot s...

Страница 15: ...or antenna 2 Move the device away from the radio or television 3 Plug the device into a different electrical outlet so that the device and the radio or television are on separate electrical circuits 4 Make sure that all peripheral devices are also certified 5 Make sure that appropriate cables are used to connect the device to peripheral equipment 6 Consult your equipment dealer Agilent Technologie...

Страница 16: ...ardware Installation General Information Cleaning To clean the unit disconnect the power and wipe down with a damp lint free cloth Recycling the Product For recycling contact your local Agilent sales office ...

Страница 17: ...tails Operating supplies high purity carrier and reagent gas es syringes pipettes vials and solvents See the 5973N and 5973 inert MSD Site Preparation Guide for details Installation and testing of additional detectors on the 6890 Series GC Training for programs not specifically listed in this document Tests of customer supplied samples equipment and or method development Any tasks not described in...

Страница 18: ...ng Supplies necessary for instrument operation are available including solvents helium carrier gas and methane reagent gas for CI MSDs Computer supplies including diskettes and printer paper Conveniently located telephone Lifting the GC and MSD will require the assistance of another person to prevent injury NOTE Installation and verification will only be performed using helium carrier gas Product ...

Страница 19: ...tive Detector User Information CD ROM 5973N and 5973 inert Mass Selective Detector Site Preparation Guide 6890 Series GC manuals GC accessories autosampler etc manuals G1701DA MSD Productivity ChemStations software manuals and online help The sensitivity specifications for your instrument Agilent publication 5988 9991EN Hydrogen Carrier Gas Safety Guide 5955 5398 For updated information see the Ag...

Страница 20: ...20 Hardware Installation General Information ...

Страница 21: ...GC 28 Conditioning the Column 29 Preparing the MSD for Installation 30 Preparing the Vacuum System 32 Plumbing the Methane Line to the CI MSD Flow Module 35 Connecting the MSD and the GC 37 Installing the ChemStation PC 40 Verifying EI System Performance 41 Switching from EI to CI Operating Mode 42 Verifying CI System Performance 43 Familiarizing the Customer 44 This chapter contains instructions ...

Страница 22: ... requires additional steps PFDTD calibrant added to calibration vial Methane isobutane gas purifier installation Methane reagent gas line and gas purifier purge Methane reagent gas line hookup After system performance has been verified in EI mode the MSD must be switched to CI mode and evaluated CI ion source and CI interface tip seal installation Bakeout and purge at least 2 hours CI setup PCI au...

Страница 23: ...tative verifies the contents of each shipping container as it is unpacked 1 Unpack the GC MSD and PC boxes 2 Check each item off on the packing list and verify serial numbers 3 Record the serial numbers in the installation documentation 4 Retain shipping containers and material until contents are checked for completeness and instrument performance is verified 5 If there are any discrepancies conta...

Страница 24: ...lace the GC on the bench 2 Remove the left side panel of the GC 3 Remove the metal upper front knockout from the interior oven wall using a flat blade screwdriver see Figure 3 4 Do not remove the insulation between the exterior and interior oven walls but move it aside Use the screwdriver not your fingers 5 Pop out the two large plastic knockouts from the GC left side panel 6 Reinstall the GC left...

Страница 25: ...Installation Hardware Installation 25 Figure 3 Removing the knockouts Plastic knockouts Metal knockout GC MSD interface heater cable GC end ...

Страница 26: ...he input of the gas purifier 5 Connect one end of the another length of copper tubing to the output of the gas purifier 6 Let the line and gas purifier purge for 5 to 10 minutes Figure 4 Connect helium Copper supply tubing Main supply On Off valve Helium carrier gas supply Two stage regulator On Off valve Helium gas purifier be sure the arrow points in the direction of gas flow Copper supply tubin...

Страница 27: ...Installation Hardware Installation 27 7 Connect the other end of the tubing to the input of the EPC controller Purge the flow system for 20 minutes You can continue with the next step while you wait ...

Страница 28: ...et 4 Turn on the GC and verify that the GC passes self test Keep the GC oven turned off 5 Configure the column parameters for the MSD column that is installed in the GC On the GC keypad select Config Col 1 and set the following column parameters 6 Increase the supply pressure of the carrier gas to 60 to 80 psi 7 Set the column flow rate to 5 mL min and split flow to 200 mL min CAUTION Do not use s...

Страница 29: ...0 C 4 Turn on the oven and ramp the oven temperature from 40 C to 300 C or 10 C above the maximum temperature used for your analysis at 15 C per minute Hold for 10 minutes then reset to 35 C While the oven is heating proceed with the next steps 5 Once the oven temperature exceeds 80 C inject 5 µL methanol into GC repeat two more times at 5 minute intervals This will help remove any contamination f...

Страница 30: ...er cover of the MSD See the 5973N or 5973 inert MSD Hardware Manual for more information 3 Equalize the pressure in the MSD by turning the vent valve knob counterclockwise 1 2 turn The MSD is not under vacuum It has been backfilled with clean dry nitrogen for shipping 4 Add PFTBA 05971 60571 to the EI calibration vial at the front of the MSD See the 5973N or 5973 inert MSD Hardware Manual for more...

Страница 31: ...Installation Hardware Installation 31 Special procedure for CI MSD 5 Add PFDTD 8500 8130 to the vial on the CI calibration valve See the 5973N or 5973 inert MSD Hardware Manual for more information ...

Страница 32: ...nnect the hose to the inlet port of the pump 7 If non toxic and non flammable carrier gas solvents and analytes will be used install the pump exhaust oil trap on the outlet of the pump Otherwise install a hose 11 mm id to take the foreline pump exhaust outside or to a fume exhaust hood Do not use the trap on a CI MSD CAUTION Remove the red plug from the outlet of the pump before switching on the M...

Страница 33: ...led will result in serious damage to the instrument See the instructions taped to the MSD WARNING The foreline pump must be plugged into the receptacle provided in the back of the MSD in order to have adequate overcurrent protection Plugging the pump into a wall outlet will void the warranty on the pump Figure 5 Preparing the vacuum system Foreline hose from high vacuum pump outlet Exhaust outlet ...

Страница 34: ...0 Install the optional 59864B gauge controller required for CI MSDs Be sure not to stress the cable or the tube may crack WARNING The gauge controller must be properly grounded See the manufacturer s manual supplied with the gauge controller ...

Страница 35: ...methane regulator to 20 psig do not exceed 30 psig 3 Connect one piece of the 1 8 inch stainless steel tubing to the methane supply regulator 4 Turn on the gas flow slightly 5 Connect the other end of the tubing to the inlet of the gas purifier CAUTION Only remove the caps in the gas stream or the gas purifier will be contaminated by air This will ruin the gas purifier WARNING Methane is flammable...

Страница 36: ...e as shown in Figure 6 9 If another reagent gas is to be used use more stainless steel tubing to connect it to the Gas B fitting If you are going to connect isobutane you will need another gas purifier for the Gas B line Observe the manufacturer s suggested pressure settings CAUTION Do not connect isobutane without a gas purifier Do not use the gas purifier with ammonia Figure 6 Connecting the met...

Страница 37: ...nterface cover will touch the metal of the oven wall and the end of the interface will protrude into the GC oven Note that the end of the interface on a CI MSD will not protrude quite as far into the GC oven as that on an EI MSD 4 Connect a remote cable between the MSD and one of the remote connectors on the back of the GC Figure 7 Connecting the MSD and the GC 6890 Series GC 5973 Series MSD GC MS...

Страница 38: ... nut and blank ferrule from the end of the GC MSD interface 8 Install the column in the GC MSD interface See the 5973N or 5973 inert MSD Hardware Manual for more information Figure 8 Loosen sideplate thumbscrews Rear sideplate thumbscrew loosen completely CAUTION Opening the analyzer with either sideplate thumbscrew tight will irreparably damage the baseplate Damage of this type is not covered by ...

Страница 39: ...nd the front fan turn on and that the foreline pump stops gurgling within one minute 12 After 10 minutes of pumping turn off the MSD 13 Turn off the GC temperature zones 14 Set column flow to 1 0 mL min with constant flow enabled 15 Reinstall the MSD analyzer cover Figure 9 Rear panel view Transmit Tx and receive Rx LEDs Foreline pump power cord Power cord receptacle LAN cable Remote start cable P...

Страница 40: ...nector on the MSD and connector 1 on the network hub 6 Connect a shielded LAN cable between the RJ 45 connector on the back of the GC to connector 2 on the network hub 7 Connect a shielded LAN cable between the RJ 45 connector on the back of the PC and connector 3 on the network hub 8 Install the printer See the printer installation documentation 9 Install the modem not all ChemStations have modem...

Страница 41: ...as completed save the method and then select Tune Evaluation from the Qualify menu The software will evaluate the last autotune and print a System Verification Tune report Verify the sensitivity performance 1 Set up to inject 1 µL of OFN either with the ALS or manually 2 In the Instrument Control view select Sensitivity Check from the Qualify menu 3 Click the appropriate icons in the Instrument Ed...

Страница 42: ...I operation Verify that PCICH4 U is loaded 11 Select Purge Cal Valve from the Vacuum menu in the Diagnostics Vacuum Control view 12 Set up the methane reagent gas flow 13 Verify that there is no visible peak at m z 32 and that the peak at m z 19 is less than 50 of that at m z 17 CAUTION Electrostatic discharges to analyzer components are conducted to the side board where they can damage sensitive ...

Страница 43: ...are Manual Verify that rms signal to noise ratio meets the published specification Verify NCI performance 1 Perform a negative CI autotune 2 Verify negative CI performance Verify that rms signal to noise ratio meets the published specification See Agilent publication 5988 9991EN NOTE There are no criteria for a passing CI autotune If the CI autotune completes it passes EMV at or above 2600 V howev...

Страница 44: ...en load NCI tune file to switch parameters set gas flow to 40 adjust if necessary for specific analyte NCI operation Reagent gas flow source temperature and emission current are the three most important parameters for optimizing NCI No PFDTD calibrant ions are formed in PCI with isobutane or ammonia Tune with methane and copy parameters to new file e g PCINH3 U The gas purifier can not be used wit...

Страница 45: ...ists Installation Checklist 46 Customer Familiarization Checklist 53 This section provides a series of checklists which will help you verify your completion of the various steps of the installation process Also included are checklists which are intended to aid you in becoming familiar with the system ...

Страница 46: ...instrument operation are available including solvents carrier and reagent gasses and printer paper Conveniently located telephone Unpacking and inspecting the shipped materials Shipping containers must be opened only with an Agilent Technologies representative present to verify the contents of each container Check each item off on the packing list and verify serial numbers Record the serial number...

Страница 47: ...ge plastic knockouts removed from the left side panel Left side panel reinstalled GC MSD interface cable routed through the rear hole Connecting helium lines to the GC Carrier gas supply plumbed with copper tubing Plumbing purged with helium at 5 to 8 psi 35 to 55 KPa for 5 to 10 minutes Distribution center notified date Damaged or missing material Person contacted DM notified date ...

Страница 48: ...n split flow to 200 mL min Conditioning the column Free end of column trimmed Helium flow through column verified Injection port temperature set to 300 C Oven temperature ramped from 40 C to 300 C at 15 C per minute and held for 10 minutes 5 µL of methanol injected into GC repeated two more times at 5 minute intervals Injection port set to 250 C GC power off MSD installation Preparing the MSD for ...

Страница 49: ...pump cap removed diffusion pump MSD only Foreline pump power cord plugged into MSD 59864B Gauge Controller installed required for CI MSDs Plumbing the methane line to the CI MSD Methane isobutane gas purifier installed Regulator pressure set to 20 psig do not exceed 30 psig Gas purifier and lines purged Methane reagent gas lines plumbed to flow module Connecting the MSD and the GC GC power turned ...

Страница 50: ...th constant flow enabled MSD ChemStation PC installation PC monitor and printer unpacked PC installed Network hub unpacked and plugged in LAN cable from the MSD connected to hub Port 1 LAN cable from the GC connected to hub Port 2 LAN cable from the PC connected to hub Port 3 Printer installed Modem installed if supplied Modem printer monitor and PC turned on in that order Software installed per G...

Страница 51: ... interface tip seal installed MSD pumped down and baked out for 2 hours Software set up for CI operation Purge Cal Valve performed Methane reagent gas flow set up Acceptable air and water background verified PCI performance verification if applicable PCI autotune performed PCI sensitivity verified NCI performance verification if applicable NCI autotune performed NCI sensitivity verified Instrument...

Страница 52: ...s and Tune Report s faxed to GCMS LSCA Technical Marketing at USA 408 553 3188 or your region s local Technical Marketing Support Provider 5973 Series MSD serial number product number NCI serial number rms EI serial number rms PCI serial number rms ...

Страница 53: ...asic overview of the operation and maintenance of new instruments systems and applications software It is not a substitute for a full operator training course Topics not included in familiarization Training on the PC the mouse Windows Operating System DOS Excel Access or any other Windows applications Advanced mass spectral processing Analysis of unknown samples Analysis of customer standards or s...

Страница 54: ... hardware and peripherals System operation Switching on instruments PC and peripherals Starting Windows Operating System and using online help Starting MSD ChemStation software Switching between EI and CI operation CI MSD only MSD ChemStation software overview Software configuration of the instruments MS Config demonstrated EI CI instrument configuration with MS Config demonstrated if applicable D...

Страница 55: ...if applicable NCI Autotune performed if applicable Optimization of reagent gas and application dependency on gas flow source temperature and emission current discussed Importance of retaining tuning and maintenance records discussed Methods Edit entire method demonstrated with OFN_SN M explaining the GC and MS Scan Parameters Method save demonstrated Data Acquisition Analytical method developed to...

Страница 56: ...g a spectrum demonstrated Difference between standalone and online data analysis explained Sequence Sequence loading demonstrated Sample Log Table editing demonstrated Sequence saving demonstrated Running halting and position and run demonstrated MSD ChemStation maintenance Directory structure and maintenance of MSDCHEM files discussed Data backup options discussed Use of Windows Operating System ...

Страница 57: ...d pumpdown procedures performed and described using the ChemStation software Differences between the EI and CI source parts described Differences in installation and removal of the EI vs CI source described Maintenance section of Hardware manual demonstrated Ion source cleaning demonstrated Vacuum system preventive maintenance demonstrated special precautions for certain reagent gases discussed Tr...

Страница 58: ...ained Additional support information Use of manuals and online help explained Warranty and warranty enhancements explained Agilent Technologies Support services and how to obtain help explained Hardware Software Assist Packages Additional Training Consulting Company name Sales order number Customer signature date Engineer signature date ...

Страница 59: ......

Страница 60: ...G2589 90073 Agilent Technologies Agilent Technologies Inc Printed in USA August 2003 ...

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