5975 Series Mass Selective Detectors Hardware Installation Agilent Technologies
Notices © Agilent Technologies, Inc. 2010 No part of this manual may be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from Agilent Technologies, Inc. as governed by United States and international copyright laws. Manual Part Number G3170-90038 Edition Second edition, February 2010 Printed in USA Agilent Technologies, Inc.
Contents 1 General Information Introduction 8 Important Safety Warnings 11 Many internal parts of the MSD carry dangerous voltages 11 Electrostatic discharge is a threat to MSD electronics 11 Many parts are dangerously hot 12 Hydrogen 12 Safety and Regulatory Certifications 14 Information 14 Symbols 15 Electromagnetic compatibility 16 Sound emission declaration for Germany Cleaning 17 Recycling the Product 17 Customer Responsibilities Before You Start 18 19 Other Documentation 2 16 20 Installat
Conditioning the Column 29 Preparing the MSD for Installation Preparing the Vacuum System 30 31 Plumbing the Methane Line to the CI MSD Flow Module Connecting the MSD and the GC Installing the ChemStation PC 34 36 39 Verifying EI System Performance 40 Verify the tune performance 40 Verify the sensitivity performance 40 Switching from EI to CI Operating Mode Verifying CI System Performance Verify PCI performance 42 Verify NCI performance 42 42 Verifying High Mass System Performance Familiarizing th
MSD ChemStation software overview 54 MSD ChemStation software autotune descriptions Methods 55 Data acquisition 55 Data analysis 55 Sequence 56 MSD ChemStation maintenance 56 EI instrument user maintenance 56 Troubleshooting (Diagnostics) 57 Tune charts 57 Additional support information 57 Hardware Installation 54 5
Hardware Installation
5975 Series Mass Selective Detectors Hardware Installation 1 General Information Introduction 8 Important Safety Warnings 11 Safety and Regulatory Certifications 14 Cleaning 17 Recycling the Product 17 Customer Responsibilities 18 Before You Start 19 Other Documentation 20 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.
1 General Information Introduction This document provides installation instructions for the Agilent Technologies 5975 Series Mass Selective Detector (MSD). Installation must be performed by an Agilent Technologies service representative. The Agilent Technologies 5975 Series Mass Selective Detectors (MSDs) are diffusion and turbo pump MSDs. The 5975 Series MSD system consists of: NOTE Mix and match of the combinations below may not be supported.
General Information Table 1 1 Available high vacuum pumps Model name Product number Description Ionization modes 5975C TAD VL MSD G3170A Diffusion Pump MSD Electron impact (EI) 5975C TAD inert MSD G3171A Standard Turbo MSD Electron impact (EI) G3172A Performance Turbo MSD Electron impact (EI) 5975C TAD inert XL MSD G3174A CI High Mass Performance Turbo Pump Electron impact (EI) Negative chemical ionization (NCI) Positive chemical ionization (PCI) 7820 VL MSD G3175A Diffusion Pump MS
1 General Information ALS 7890A GC CI gas flow module Local control panel 5975 Series MSD MSD power switch GC power switch Figure 1 10 5975 Series MSD system Hardware Installation
1 General Information Important Safety Warnings Before moving on, there are several important safety notices that you should always keep in mind when using the 5975 Series MSD. Many internal parts of the MSD carry dangerous voltages If the MSD is connected to a power source, even if the power switch is off, potentially dangerous voltages exist on the wiring between the MSD power cord and the AC power supply, the AC power supply itself, and the wiring from the AC power supply to the power switch.
1 General Information Many parts are dangerously hot Many parts of the MSD operate at temperatures high enough to cause serious burns. These parts include but are not limited to: • The inlets • The oven and its contents • The detectors • The column nuts attaching the column to an inlet or detector • The valve box You should always cool these areas of the MSD to room temperature before working on them. They will cool faster if you first set the temperature of the heated zone to room temperature.
1 General Information WA R N I N G When using hydrogen (H2) as the carrier gas or fuel gas, be aware that hydrogen gas can flow into the oven and create an explosion hazard. Therefore, be sure that 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.
1 General Information Safety and Regulatory Certifications The 5975 Series Mass Selective Detector conforms to the following safety standards: • Canadian Standards Association (CSA): CAN/CSA—C22.2 No.
1 General Information Refer servicing to qualified service personnel. Substituting parts or performing any unauthorized modification to the instrument may result in a safety hazard. Symbols Warnings in the manual 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.
1 General Information Electromagnetic 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.
General Information 1 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.
1 General Information Customer Responsibilities The following are not included in the standard installation. They are the responsibility of the customer, unless previous arrangements have been made between the customer and the Agilent Technologies Customer Service Organization. • Preparation of all site facilities including the provision of adequate space, supporting bench, and power to match the unit(s) purchased.
General Information 1 Before You Start Verify that all the conditions specified in the 5975 Series MSD Site Preparation Guide have been met: • Adequate space is available for the MSD system • Suitable supporting bench • Adequate electrical power is available at the correct voltages and frequencies • Environmental control systems are adequate • Adequate preparations for safe exhaust venting • Supplies necessary for instrument operation are available, including solvents, helium carrier gas, and methane reag
1 General Information Other Documentation Additional information is contained in the following documentation: • 5975 Series Mass Selective Detector Hardware Manuals, which are located on the 5975 Series Mass Selective Detector User Information CD-ROM • 5975 Series Mass Selective Detector Site Preparation Guide • GC Series manuals • GC automatic liquid sampler documentation • GC accessories documentation • Agilent MSD ChemStation software manuals and online help • The sensitivity specifications for your in
5975 Series Mass Selective Detectors Hardware Installation 2 Installation Overview 22 Unpacking and Inspecting the Materials 23 Installing the GC 24 Connecting the Helium Lines to the GC 26 Configuring the GC 28 Conditioning the Column 29 Preparing the MSD for Installation 30 Preparing the Vacuum System 31 Plumbing the Methane Line to the CI MSD Flow Module 34 Connecting the MSD and the GC 36 Installing the ChemStation PC 39 Verifying EI System Performance 40 Switching from EI to CI Operating Mode 41 Verif
2 Installation Overview Listed below are the steps performed for hardware installation. The actual order of the steps depends upon the type of MSD, GC, and accessory ordered.
Installation 2 Unpacking and Inspecting the Materials Shipping containers should not be opened until an Agilent Technologies representative is present to verify the contents of each container. Warranty claims for missing items will not be honored unless an Agilent Technologies representative verifies the contents of each shipping container as it is unpacked. 1 Unpack the GC, MSD, and PC boxes. See Figure 2. 2 Check each item off on the packing list, and verify serial numbers.
2 Installation Installing the GC Materials needed: Column cutter (5181-8836) Flat-blade screwdriver GC Series shipping kit Please refer to the GC/MS application note, “Optimizing splitless injections on your GC for high-performance MS analysis” (5988-9944EN) before installing the GC. 1 WA R N I N G NOTE 24 Place the GC on the bench. To prevent injury, get lifting assistance. 2 Remove the left side panel of the GC.
Installation 2 Metal knockouts GC/MSD interface heater cable (GC end) Figure 3 Removing the knockouts Hardware Installation 25
2 Installation Connecting the Helium Lines to the GC 1 Connect the 6-foot copper tubing (or a custom length) to the carrier gas supply line (Figure 4). Copper supply tubing On/Off valve Two-stage regulator Main supply On/Off valve Helium carrier gas supply Helium gas purifier (be sure the arrow points in the direction of gas flow) Copper supply tubing Figure 4 Connect helium CAUTION 26 2 Turn on the carrier gas flow at a low pressure, 35 to 55 kPa (5 to 8 psi).
2 Installation Purge the flow system for 20 minutes. You can continue with the next step while you wait.
2 Installation Configuring the GC 1 If there is an ALS, install it now. Follow the instructions provided with the ALS. 2 CAUTION Install the Merlin Microseal (optional). Follow the instructions provided with the Merlin Microseal. Do not use syringes with tapered needles with a Microseal. 3 Connect the GC power cord to the appropriate electrical outlet. 4 Turn on the GC and verify that the GC passes self-test. Keep the GC oven turned off.
Installation 2 Conditioning the Column 1 Remove the septum covering the free end of the GC column and cut about 1 cm off the end of the column. 2 Place the free end of the column into a beaker of solvent and check for bubbles to verify helium flow. Do not leave the beaker in the oven. 3 Set the inlet temperature to 300 °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.
2 Installation Preparing the MSD for Installation Materials needed: 5975 Series MSD Hardware Manual Tygon tubing or hose for pump exhaust (11-mm id) Wrench, 1/4-inch × 5/16-inch open end 5975 Series MSD Shipping Kit 5975 Series MSD CI Shipping Kit 1 WA R N I N G Unpack the MSD and foreline pump, and place them on the bench near the GC. To prevent injury, get lifting assistance. 2 Remove the analyzer cover of the MSD. See the 5975 Series MSD Hardware Manual for more information.
Installation 2 Preparing the Vacuum System Materials needed: 5975 Series MSD Hardware Manual Diagonal cutters Plastic gloves 1 Remove the plugs from the inlet and the outlet of the pump. 2 Verify that the available ac power matches the voltage rating of the foreline pump. 3 Attach the correct line voltage identification sticker to the MSD back panel. 4 Place the oil drip pan under the foreline pump as shown in Figure 5.
2 Installation 6 Remove the blank flange from the free end of the hose, and connect the hose to the inlet port of the pump. 7 If nontoxic and nonflammable 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 MSD power.
2 Installation Remote start cable Transmit (Tx) and receive Power cord LAN cable Foreline pump power Power (PWR) and heartbeat (heart) LEDs Figure 6 Foreline pump power plug WA R N I N G 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. 9 WA R N I N G Install the optional G3397A High vacuum gauge controller (required for CI MSDs).
2 Installation Plumbing the Methane Line to the CI MSD Flow Module Special procedure for CI MSD Refer to the 5975 Series MSD Hardware Manual. Materials needed: Methane supply with regulator Methane/Isobutane gas purifier (G1999-80410) Stainless-steel tubing, 1/8-inch Swagelok fittings and ferrules for 1/8-inch tubing Wrench, 7/16-inch open-end, two needed 34 CAUTION Only remove the caps in the gas stream, or the gas purifier will be contaminated by air. This will ruin the gas purifier.
Installation 7 Let the lines purge into a fume hood for 5 to 10 minutes. 8 Connect the other end of the tubing to the Gas A fitting on the flow module as shown in Figure 7. 9 If another reagent gas is to be used, use more stainless steel tubing to connect it to the Gas B fitting. 2 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.
2 Installation Connecting the MSD and the GC 1 Verify that the GC power is turned off. 2 Connect the two ends of the GC/MSD interface cable as shown in Figure 8. GC/MSD interface cable 5975 Series MSD 7890 Series GC Figure 8 Connecting the MSD and the GC 3 36 Carefully position the MSD close to the GC as shown in Figure 8.
Installation 2 When positioned properly, the end of the GC/MSD interface cover will touch the metal of the oven wall, and the end of the interface will protrude into the GC oven. The sides of the GC and MSD should be parallel. 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. 5 Connect the MSD power cord to an appropriate AC outlet.
2 Installation Press on the side plate of the MSD to achieve a good seal. Verify that the foreline pump and the front fan turn on, and that the foreline pump stops gurgling within 1 minute. 38 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.
2 Installation Installing the ChemStation PC 1 Unpack the PC, monitor, printer, and the modem (if present). 2 Position the PC components on the bench. 3 Install the PC. See the PC installation documentation. Please pay attention to the voltage requirements in the PC documentation. 4 Position the network switch on the bench, and plug in its power supply. See the switch installation documentation.
2 Installation Verifying EI System Performance Material needed: 1 pg/µL (0.001 ppm) OFN sample (5188-5348) Verify the tune performance 1 Verify that the system has been pumping down for at least 60 minutes. 2 Set the GC oven temperature to 150°C, and the column flow to 1.0 mL/min. 3 In the Instrument Control view, select Checkout Tune from the Checkout menu. The software will perform an autotune and print out the report.
Installation 2 Switching from EI to CI Operating Mode Special procedure for CI MSD Refer to the 5975 Series MSD Hardware Manual. CAUTION CAUTION 1 Vent the MSD. 2 Open the analyzer. 3 Remove the EI ion source. Electrostatic discharges to analyzer components are conducted to the side board where they can damage sensitive components. Wear a grounded antistatic wrist strap (see the 5975 Series MSD Hardware Manual) and take other antistatic precautions before you open the analyzer.
2 Installation Verifying CI System Performance Special procedure for CI MSD Refer to the 5975 Series MSD Hardware Manual. Verify PCI performance 1 Perform a positive CI autotune. See the 5975 Series MSD Hardware Manual. 2 Verify positive CI performance. See the 5975 Series MSD Hardware Manual. 3 Verify that rms signal-to-noise ratio meets the published specification. Verify NCI performance NOTE 42 1 Perform a negative CI autotune. 2 Verify negative CI performance.
Installation 2 Verifying High Mass System Performance Refer to the 5975 Series MSD Hardware Manual. To check high mass performance, the system makes 1 injection of the high mass checkout sample and analyzes the results. For high mass systems, verify high mass system performance as follows: 1 Load the high mass checkout method, PFHT.M, and resolve any configuration conflicts. 2 Load the high mass checkout sample into vial 2.
2 Installation Familiarizing the Customer Follow the “Customer Familiarization Checklist” on page 53. Important points about the CI MSD to cover include: Cleanliness is the most important factor for success in CI, especially negative mode. This includes air leaks, water, and residual PFDTD calibrant. NCI reagent gas setup: There are no negative reagent ions formed.
5975 Series Mass Selective Detectors Hardware Installation 3 Checklists 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.
3 Checklists Installation Checklist Verifying that site preparation is complete Adequate space is available for the MSD system. Suitable supporting bench. Adequate electrical power is available at the correct voltages and frequencies. Environmental control systems are adequate to maintain a correct, stable operating environment. Safe exhaust venting preparations are adequate.
Checklists 3 Shipment damaged or incomplete: Distribution center notified (date): Person contacted: DM notified (date): Damaged or missing material: GC installation The following steps are general, and may differ slightly depending upon the series of GC used.
3 Checklists GC plumbed Configuring the GC ALS installed (optional) Merlin Microseal installed (optional) GC plugged in and turned on GC passes self-test Column parameters configured Carrier gas line pressure set to approximately 414 kPa (60 psi) Column flow rate set to 5 mL/min (split flow to 200 mL/min) Conditioning the column Free end of column trimmed Helium flow through column verified Inlet temperature set to 300 °C Oven temperature ramped from 40 °C to 300°C at 15 °C per m
Checklists 3 PFDTD vial for CI cal valve filled Preparing the vacuum system Plugs removed from the foreline pump Foreline pump line voltage verified to match available AC power Line voltage identification sticker installed on MSD Oil drip pan under the foreline pump Foreline hose connected to the pump Pump exhaust vented to a fume hood or the oil trap installed Foreline pump power cord plugged into MSD G3397A High Vacuum Gauge Controller installed (required for CI MSDs) Plumbing the me
3 Checklists Foreline pump and the front fan operation verified Foreline pump stops gurgling within 60 seconds verified MSD turned off after 10 minutes of pumping down GC heated zones turned off GC carrier gas flow set to 1.
Checklists 3 EI ion source removed CI ion source installed CI 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 High Mass performance verifi
3 Checklists Instrument Log Book updated MSD serial number recorded on S/N report S/N Report(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 5975 Series MSD serial number/product number: EI serial number (rms): PCI serial number (rms): NCI serial number (rms): 52 Hardware Installation
Checklists 3 Customer Familiarization Checklist The purpose of customer familiarization is to demonstrate the steps required to: • Perform a basic analysis using an Agilent standard sample or an internal data file • Evaluate the acquired data • Perform routine maintenance Much of the familiarization is accomplished while the hardware is being installed and checked out. For this reason, at least one operator must be present throughout installation and familiarization.
3 Checklists Hardware overview MSD CI MSD (if applicable) Gas Chromatograph ALS (if applicable) Bar code reader (if applicable) PC 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 confi
Checklists 3 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 Importance of backing up data, including tune files Methods Edit entire method demonstrated with OFN_SN.
3 Checklists Library search (searching 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 DEFRAG and SCANDISK utilities discussed EI instru
Checklists 3 Differences between the EI and CI source parts described Differences in installation and removal of the EI versus 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 Troubleshooting (Diagnostics) Tune charts under Qualify menu demonstrated Online help for troubleshooting demonstrated Tune charts Displaying results exp
3 Checklists Company name: Customer signature/date: Engineer signature/date: Sales order number: 58 Hardware Installation
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