布鲁克质谱说明书

来源：爱go旅游网

Hardware Operation Manual

Quadrupole Mass Spectrometer

300-MS and 320-MS

Legal and Regulatory Notices

Reproduction, adaptation, or translation without prior written permission is prohibited, except as allowed under the copyright laws.

Warranty

The information contained in this document is subject to change without notice. Bruker makes no warranty of any kind with regard to this material, including, but not limited to, the implied warranties of merchantability and fitness for a particular purpose. Bruker is not liable for errors contained herein or for incidental or consequential damages in connection with the furnishing, performance or use of this material. Bruker assumes no responsibility for the use or reliability of its software on equipment that is not furnished by Bruker.

Use of Trademarks

The names of actual companies and products mentioned herein may be the trademarks of their respective owners.

Safety Information

Operating Instructions

Use this manual to establish conditions for safe and efficient instrument operation. Special considerations and precautions are also included as NOTES, CAUTIONS, and WARNINGS. You must operate the instrument as specified by this manual and any additional information Bruker provides. Address questions about the safe and proper use of the instrument to your local Bruker office.

The safety information presented is for the MS, refer to the manuals of the GC or autosampler to ensure their safe and efficient operation.

NOTE

Use this information to obtain optimal performance from your instrument.

CAUTION Alerts you to situations that may cause moderate injury or instrument damage, and provides methods to avoid these situations.

WARNING Alerts you to potentially hazardous situations that could result in serious injury, and provides

methods to avoid these situations

Warning Description

Hazardous voltages are present inside instrument. Disconnect from main power before removing screw-attached panels.

Hazardous chemicals may be present. Avoid contact, especially when replenishing reservoirs. Use proper eye and skin protection.

WARNING: SHOCK HAZARD WARNING: CHEMICAL HAZARD WARINING: BURN HAZARD WARNING: EYE HAZARD WARNING: FIRE HAZARD WARNING: EXPLOSION HAZARD WARNING: RADIATION SOURCE WARNING: MOVING PARTS Very hot or cryogenically cold surfaces may be exposed. Use proper skin protection.

Eye damage could occur from flying particles, chemicals, or UV radiation. Use proper eye and face protection. The potential for fire may be present. Follow manual instructions for safe operation.

The potential for explosion may exist because of type of gas or liquid used.

Ionizing radiation source is present. Follow manual instructions for safe operation. Keep hands and fingers away.

General Safety Precautions

Follow these safety practices to ensure safe instrument operation.

• • • •

Perform periodic leak checks on all supply lines and pneumatic plumbing.

Do not let gas lines become kinked or punctured. Place lines away from foot traffic and extreme heat or cold.

Store organic solvents in fireproof, vented, and clearly labeled cabinets so they are easily identified as toxic and/or flammable materials.

Do not accumulate waste solvents. Dispose of such materials through a regulated disposal program and not through municipal sewage lines.

The following is a Federal Communications Commission advisory: This instrument has been tested and found to comply with the limits of a Class A computing device, pursuant to part 15 of the FCC Rules. These limits are designed to provide reasonable protection against harmful interference when the instrument is operated in a commercial environment. This instrument generates, uses, and can radiate radio frequency energy and, if not installed and used in accordance with the instruction manual, may cause harmful interference to radio communications. Operation of this instrument in a residential area is likely to cause harmful interference in which case the user will be required to correct the interference at his own expense. NOTICE:

This instrument has been tested per applicable requirements of EMC Directive as required to carry the European Union CE Mark. As such, this instrument may be susceptible to radiation/interference levels or frequencies not within the tested limits.

This instrument is designed for MS analysis of appropriately prepared samples. It must be operated using appropriate gases and/or solvents and within specified ranges for pressure, flows, and temperatures as described in this manual. The protection provided by the instrument may be impaired if the instrument is not used as specified by Bruker.

It is the responsibility of the Customer to inform Bruker if the instrument has been used for the analysis of hazardous biological, radioactive, or toxic samples, prior to any instrument service being performed or when an instrument is being returned to Bruker.

WARNING WARNING Electrical Hazards

• Disconnect the instrument from all power sources before removing protective panels to avoid exposure to dangerous voltages. • When it is necessary to use a non-original power cord plug, the replacement cord must adhere to the color coding and polarity described in the manual and all local building safety codes.

• Replacement fuses must have the size and rating stipulated on the fuse panel or in the manual.

• Replace faulty or frayed power cords

immediately with the same type and rating. • Voltage sources and line voltage must

match the value for which the instrument is wired.

Compressed Gas Cylinders

• Store and handle compressed gases in strict adherence to safety codes.

• Secure cylinders to an immovable structure or wall.

• Store and move cylinders in an upright, vertical position. Before transport, remove regulators and install the cylinder cap.

• Store cylinders in a well-ventilated area away from heat, direct sunshine, freezing temperatures, and ignition sources.

• Mark cylinders clearly, so they are easily identified • Use only approved regulators and connections. • Use only connector tubing that is

chromatographically clean ( Bruker part number 391832600) and has a pressure rating greater

than the highest outlet pressure from the regulator.

General MS Safety Practices

Shock Hazard

Many internal parts carry dangerous voltages. Even if the power switch is off potentially dangerous voltages can exist. The covers shield the operator. Unless specifically instructed, do not remove a cover.

Electrostatic Discharge

Do not touch printed circuit boards unless instructed. Wear a grounded wrist strap to prevent electrostatic discharge to the board, which may damage the board.

Burn Hazard

Heated parts of the mass spectrometers remain hot or cold for a long time after the instrument power is turned off. To prevent painful burns, ensure that all heated or cooled areas have returned to room temperature or wear adequate hand protection before you touch potentially hot surfaces.

Fire Hazard

Combustible materials put under, over, or around the foreline pump are fire hazards. Keep the foreline oil pan clean, but do not leave absorbent materials such as paper towels or rags in it.

Spare Parts

Bruker provides operational spare parts for any instrument and major accessory for a period of seven (7) years after shipment of the final production run of that instrument. Spare parts will be available after this seven (7) year period but on an as available basis. Operational spare parts are defined as those individual electrical or

mechanical parts that are susceptible to failure during their normal operation. Examples include relays, lamps, temperature probes, detector elements, motors, etc. Sheet metal parts, structural members or assemblies and castings, printed circuit boards, and functional modules are normally capable of being rebuilt to like-new condition throughout their useful life and therefore will be supplied only on an as available basis after the final production run of the instrument.

Service

Bruker provides service support to customers after warranty expiration. Repair service can be provided by service contracts or on a time and material basis. Technical support and training can be provided by qualified personnel on both a contractual or as-needed basis.

To contact Sales or Service, and to order Parts and Supplies, contact your local Bruker office.

Contents

Overview .................................................................................................................................... 3

Manual Description ..................................................................................................................................................... 3 300 Series Quadrupole Instruments ........................................................................................................................... 3 300 Series Quadrupole Systems ................................................................................................................................ 4

Controls and Connections ....................................................................................................... 6

300-MS or 320-MS ..................................................................................................................................................... 6 Back Panel Electrical and Gas Connections .............................................................................................................. 7

Principles of Operation ............................................................................................................ 8

Ion Sources ................................................................................................................................................................. 8 Mass Analyzer ............................................................................................................................................................ 9 MS and MS/MS ......................................................................................................................................................... 10

General Procedures ............................................................................................................... 13

Venting the MS ......................................................................................................................................................... 13 Pumping Down the MS ............................................................................................................................................. 14 Removing/Replacing the Glass Top ......................................................................................................................... 15

Routine Operation .................................................................................................................. 16

Routine Procedures .................................................................................................................................................. 16 Installing a GC Capillary Column .............................................................................................................................. 20 MS/MS Procedures ................................................................................................................................................... 21 Maintenance ............................................................................................................................................................. 23 Troubleshooting ........................................................................................................................................................ 32 Leak Troubleshooting ............................................................................................................................................... 37 GC/MS Spare Parts .................................................................................................................................................. 42

Foreline Pump Maintenance .................................................................................................. 43

Checking Foreline Pump Oil Level and Condition .................................................................................................... 43 Foreline Pump Oil and Cartridge .............................................................................................................................. 43 Flushing the Pump Oil .............................................................................................................................................. 45

Appendix Synchronization Signals for External Modules ................................................. 48

Hardware Setup ........................................................................................................................................................ 49 Software Setup ......................................................................................................................................................... 52

This page intentionally blank.

Overview

Manual Description

This manual contains the following sections:

• • •

Description of the instrument Principles of Operation GC/MS Operation

300 Series Quadrupole Instruments

300-MS

The 300-MS, a GC/MS single or triple quadrupole, offers excellent performance for an economical price.

The 300-MS offers the user excellent performance and features:

• • • •

Mass Range maximum of 800 amu.

Electron Ionization (EI) and Chemical Ionization (CI) are standard. Direct Insertion Probe and Direct Exposure Probes (DIP/DEP) are optional.

A Single Quadrupole can be upgraded to a Triple Quadrupole system.

320-MS

The 320-MS is available as a single or a triple quadrupole instrument. The variety of ionization sources makes this a very versatile instrument for quadrupole applications.

The 320-MS offers the user excellent performance and features:

• • • •

Mass range maximum of 2000 amu.

Electron Ionization (EI) and Chemical Ionization (CI) are standard. Optional Direct Insertion Probe and Direct Exposure Probes (DIP/DEP). A single quadrupole instrument can be upgraded to a triple quadrupole instrument.

300 Series Quadrupole Systems

Vacuum System

The MS Workstation software controls the vacuum system composed of foreline and turbo molecular pumps. One DS-42 vacuum pump is the foreline pump in all countries except for Japan in which one DS102 pump is used.

The Status View in the Instrument Control window displays the speed of the turbo pumps, expressed as percentage of the total.

In case of a power outage, the mechanical and turbo molecular pump turn off. The system maintains vacuum for 20 minutes before the system begins to vent. If power comes back within this time, the unit registers vacuum and automatically turns both pumps back on.

Do not initiate pump-down if any chipped edges or scratches are present on the glass top. Chipped edges or scratches can facilitate cracking of the glass resulting in a serious implosion and consequently a serious personal injury. Replace the glass top prior to using the instrument.

Data System

MS Workstation controls the MS and chromatography systems, GC systems, auto samplers and most accessories.

MS Workstation works within Windows® 2000, XP, and 7 operating systems (pre-installed on the PC), and can be configured to run under networks.

MS Workstation controls the MS system including setup, tuning, data acquisition, data handling, and report generation. For further information, refer to the following:

300-MS and 320-MS MS Workstation Software Operation Manual, part number BCA94200600.

MS Workstation Software Reference Manual, part number BCA94200400.

Electronics

HIGH VOLTAGES. There are no user serviceable parts under screw-attached covers. Contact your local Bruker service representative for instrument repair and service.

The electronic functions are distributed among nine main printed circuit boards. See the block diagram and descriptions that follow. ` Power Board RF Board Source Feedthru Board Ion Gauge Electrometer DIP Opt DEP Opt Inlet Control Board Manifold Assy : Quads , Collision Cell , Source , Detector Detector Board Foreline pumps Transfer Line Heater EFC

Power Board: Controls spectrometer operations and acquires data. It contains the valve drivers and vent control circuit, Manifold and Source heater circuit, Source Pressure circuit, Collision Cell Pressure circuit, Rear Panel Auxiliary Pressure circuit, and User I/O Interface circuit.

RF Generator Board: Generates and controls the Quad RF and DC electronics, Lens and Guide electronics, Source and Manifold temperature sensor circuits, Ion Gauge and Filament electronics, and Capillary electronics.

Detector Board: Detects the signal from the Multiplier. An A/D converter converts the analog signal to a digital signal.

Ion Gauge Electrometer Board: Contains the ion gauge electronics and links the RF board to the Ion Gauge on the manifold.

Electronic Flow Controller: Controls the flow of CI gas (methane, isobutane, ammonia, and helium) and CID gas.

API HV Board: Generates the Needle and Shield voltages.

Inlet Control Board: Controls the EFC electronics, the transfer line heater control, and the foreline pump control. The capillary voltage goes through this board through a protection relay before exiting to the API Source.

Ion Source Feedthru: The interface board between the RF board (lenses and source temp sensor) and the Power Board (source heaters).

Controls and Connections

300-MS or 320-MS

300-MS or 320-MS Front Panel

DIP/DEP Probe Probe Inlet EI/CI Source Calibration Gas Connects to the 7-pin round plug from the DIP/DEP probe. Connects the 10-pin round plug with the DIP/DEP Probe and controls inlet interlock switch. Connects the 14 -pin round plug from the GC source and controls the GC Plug and Play Source. Refill with PFTBA (FC-43) part number 392035300. 300-MS or 320-MS Status Display

On the left side of the instrument is a display panel with three lights that display the instrument status.

Back Panel Electrical and Gas Connections

CID He CI N2

Pump switch Data system User I/O, digital, analog input, valves, relays Foreline pump Power In Helium CI gas CID gas Manual power switch for foreline pumps. Serial connection to workstation. Sync Start cable 300-MS or 320-MS: 1 DS-42 Main Line power input. Connects to helium source for solvent flush

Connects to CI gas source, usually methane, isobutane, or ammonia. Connects to Collision gas source, usually argon. Bulkhead fittings for the gasses are on the right side of the back panel. The fittings require a 1/8-inch Swagelok® nut and ferrule.

Principles of Operation

The 300-MS and 320-MS GC/MS systems can analyze solid, liquid, and gas samples. Solid samples can be inserted directly into the MS using either the Direct Insertion Probe or the Direct Exposure Probe (purchase of an optional kit required) in EI or CI mode with the 320-MS or a 300-MS.

Ion Sources

In the ion source, the components are exposed to conditions that generate ions. These conditions may be gentle or harsh enough to fragment molecules.

• •

Electron Ionization (EI) Chemical Ionization (CI)

Electron Ionization (EI)

• • • •

Creates positive ions.

Analyzes any gas-phase compounds.

Causes significant and reproducible fragmentation.

Creates spectra that can be search against standard libraries, such as National Institute of Standards and Technology, NIST.

Electron ionization is the traditional GC/MS ionization technique and is suitable for all gas-phase compounds. It yields reproducible molecular fragmentation patterns independent of the make and model of the MS. This allows the creation of standard libraries containing searchable spectra.

The EI source consists of an ion volume, a filament assembly, electron collimating magnets, and ion focusing lenses, all supported by a heated ion

block. The ion volume is an open cylinder with two side holes. Vaporized sample and carrier gas from the GC enters the ion volume through the transfer line in one of the holes. An electron beam, generated at the heated filament, enters the ion volume through the other hole. The accelerated electrons collide with the sample molecules inside the ion volume and generate molecular ions. The resulting ions fragment into differently charged or neutral fragments. The ions enter the mass analyzer.

Chemical Ionization (CI)

• • •

Creates either positive or negative ions.

Ionizes in a selective manner, different compound classes. Generates fewer molecular fragments than EI, making CI a softer technique that EI.

CI is recommended when no molecular ion is observed in EI and to confirm the mass-to-charge ratio of the molecular ion. CI mass spectra depend on CI reagent gas type, pressure, and ion volume temperature. Methane, ammonia, and isobutane are the CI reagent gases supported by the 300 Series GC/MS Quadrupole Instruments.

The CI reagent gas enters the ion volume with the vaporized sample and carrier gas from the GC. An electron beam, generated at the heated filament, enters the ion volume through the other opening. The accelerated electrons preferentially ionize the reagent gas molecules. Reagent ions undergo collisions with other reagent molecules and with sample molecules to create ions. These reagent ions are of very low molecular weight and rarely enter the mass analyzer.

Mass Analyzer

The ions leave the ion source and enter the mass analyzer. The first section, Quadrupole 1 (Q1) separates them according to their mass-to-charge ratio. The mass filter consists of a set of four parallel rods. Constant (dc) and radio

frequency (RF) electric fields are applied and cause the ions to move according to their mass-to-charge ratios. The field strength is varied so that only the selected ions go through the quadrupole.

Single Quadrupole Instruments

In a single quadrupole system, ions of the selected charge go through the curved Quadrupole 2 (Q2) and to the detector. Because neutral molecules are not led through the curve, they do not reach the detector. This reduces the background noise and increases the signal to noise ratio. The instrument is called a single quadrupole because only Q1 can be used as a mass filter; Q2 is an ion guide. The ions enter the on-axis dynode detector. Positive and negative ions can be detected with similar efficiency due to the on-axis geometry of the detector.

Extended Dynamic Range is an option that automatically adjusts the detector for the best signal to noise ratio and provides an “absolute” measure of ion counts.

Triple Quadrupole Instruments

In a triple quadrupole system, the mass analyzer consists of three quadrupole rod assemblies (Q1, Q2, and Q3).

Collision induced dissociation, (CID) or MSMS applications are done in the

curved Q2 of triple quadrupole systems. The ions are accelerated into Q2, which is filled with a collision gas, usually argon. The fast moving ions collide with the argon molecules and dissociate. The product ions, from these interactions, go to Q3 and neutral molecules do not reach the detector. This reduces the background noise and increase the signal to noise ratio.

Q3 can either guide the ions to the detector or act as a mass filter for the fragment ions produced by CID.

Triple quadrupole systems can be used for MS modes of operation (full scan or SIM) or for MS/MS modes of operation (SRM or MRM, product scan, precursor scan, neutral loss/gain scan).

•

During MS operation of a triple quadrupole system, the RF and DC

voltages are controlled so that Q1 acts as mass filter and Q2 and Q3 are ion guides that transmit all masses to the detector.

•

During MS/MS operations Q1 is a mass filter of the ions entering the system, Q2 is the collision cell, and Q3 is a mass filter for the product ion of the collisions.

The ions enter the on-axis detector. Positive and negative ions are detected with similar efficiency due to the on-axis geometry of the detector. Extended Dynamic Range is an option that automatically adjusts the detector for the best signal to noise ratio and provides an “absolute” measure of ion counts.

Q1 Q2 Detector Q3

MS and MS/MS

MS scans can be done with single quadrupole or triple quadrupole instruments:

• • • • • • •

Full Scans: Scan a selected mass range and record all ions. Selection Ion Monitoring (SIM): Scan for the selected ion(s) only. Product Ion Scan: A precursor ion is selected, fragmented and all fragments in the selected mass range are detected.

Selected Reaction Monitoring (SRM): A precursor ion is selected and one product ion is recorded.

Multiple Reaction Monitoring: Several SRMS can be done sequentially. Precursor Scan: A mass range is scanned for a specific ion.

Neutral Loss Scan: As a mass range is scanned in Q1, the scan of Q3 is synchronized so there is a constant mass reduction by the m/z value of the neutral fragment, such as -18 for the loss of water.

MS/MS scans are done with triple quadrupole instruments:

MS Scans

Full Scan

Scan from the Q1 First Mass to the Q1 Last Mass. These scans are rich in spectral information, excellent for screening assays, ideal for identifying unknowns and for library searches.

Selected Ion Monitoring

Scan selected ions only. Depending on the number of ions monitored and matrix interference, SIM sensitivity may be 5 to 50 times better than a full scan. SIM always give the maximum signal to noise ratio.

MS/MS Scans

Product Ion Scan

In Q1 select a precursor ion of interest and fragment it in Q2. In Q3, scan for

product ions in a selected mass range. This provides structural information about the precursor ion.

Neutral Scan Loss

In Q1 scan a mass range, in Q2 fragment the ions, and synchronize the Q3 scan for a constant mass loss. This represents the m/z of the neutral fragment and helps to identify compounds that contain the same functional groups.

Selected Reaction Monitoring

In Q1 scan for a precursor ion, in Q2 fragment the ions, and in Q3 scan for one specific product ion.

Multiple Reaction Monitoring

In Q1 scan several precursor ions, in Q2 fragment the ions, and in Q3 scan for a specific product ion from each.

Precursor Scan

In Q1 scan a mass range, in Q2 fragment the ions, and in Q3 check for a product ion of a particular mass. Identify common functional groups or moieties for several analytes.

General Procedures

Venting the MS

Cool the instrument down before venting. If you vent before the instrument is cool, the source will oxidize and must be cleaned before the system is pumped down.

1. In the Quad window, click Set Instrument Parameters.

2. Click the Analyzer tab and in the Pumps section, click Vent.

3. In the window that opens, click Cool Down.

4. Wait for the turbo pump blades to stop spinning and for the readbacks to

show no vacuum.

Pumping Down the MS

1. In the Quad window, click Set Instrument Parameters.

2. Click the Analyzer tab and in the Pumps section, click Pump down. 3. In the Quad window, click the Turbo pump, and monitor the speed of the

Turbo pump.

Removing/Replacing the Glass Top

Removing the Glass Top

1. Cool down and vent the instrument following “Venting the MS.”

2. Wait until the vacuum dissipates and the turbo pump blades stop spinning. 3. Place the suction tool on the glass top towards the front of the glass and

pump the piston until the red line is no longer visible.

4. Use the tool to lift the glass. If necessary, reposition the tool in the center of

the glass and try again. 5. Do not let dust or debris fall into the manifold.

6. Minimize dust accumulation by covering as much of the manifold as possible

with the glass top.

Replacing the Glass Top

1. If dust is on the O-ring, use a lint-free tissue to remove it.

2. Use the suction tool to lift the glass top and carefully place it on the manifold. 3. Pump the system down following “Pumping Down the MS.”

Do not initiate pump-down if the glass top has any chipped edges or scratches. Chipped edges or scratches can make it easy for the glass to crack. This would result in a serious implosion and consequently serious personal injury. Replace the glass top before using the instrument.

Routine Operation

Routine Procedures

Starting the GC/MS

Do not pump the instrument down if the glass top has chipped edges or scratches. Chipped edges or scratches can cause the glass to shatter and cause a serious implosion and possible serious personal injury. Replace the glass top before using the instrument.

NOTE: Although the examples use a 320-MS, the 300-MS is similar. 1. To start the GC/MS:

2. Turn on the computer, GC, and MS. The main power switch is on the left

front side of the instrument and the power switch for the turbo pump and foreline pump are on the back right panel.

3. From the Instrument menu, select the name of your system. The GC/MS

should connect to System Control in less than a minute. The instrument front panel shows that the instrument is connected to the Data System.

4. Turn the vacuum pump on. The switch is on the back of the chassis. 5. Click the Set Instrument Parameters icon in the Quad toolbar.

6. In the Analyzer view, click Pump down.

7. After the detector is calibrated, the date the Detector gain was computed last

is displayed.

Information about configuring other hardware modules is in the 300-MS and 320-MS MS Workstation Software Operation Manual, part number BCA94200600.

Replacing an Ion Volume

Before starting this procedure, put on a lab coat and gloves.

Removing the Ion Volume

The Ion Volume is HOT! Handle it carefully and use protective gloves.

1. Undo the flanges on the chamber and remove the cover of the vacuum

interlock chamber. 2. Connect the I/R tool to the vacuum interlock chamber by snapping the

flanges on the I/R tool. Check that the I/R tool handle is pulled back so that the handle does not hit the ball valve as you connect the I/R tool. 3. Slowly pull the vacuum interlock valve down.

4. Turn the I/R tool handle so that the pin on the handle slides through the

groove labeled EXTR. 5. Gently push the I/R tool towards the ion volume.

6. After the I/R tool is in the groove on the ion volume, gently rotate the I/R tool

clockwise and pull back so that the pin on the handle comes out through the groove labeled INSR. 7. Close the vacuum interlock valve. 8. Remove the I/R tool. 9. Replace the inlet cover.

Installing an Ion Volume

1. Remove the cover from the vacuum interlock chamber by undoing the

flanges on the chamber.

Use the I/R tool gently. Rotate the I/R tool only to couple or uncouple the ion volume holder, NOT to lock or unlock the ion volume from the source block. After the ion volume is aligned with the source block, it only moves straight into or out of the source block.

2. Place the desired ion volume on the Installation/Removal (I/R) tool.

3. Place the I/R tool on the vacuum interlock chamber and snap the flanges into

place on the I/R tool to connect it. Check that the I/R tool handle is pulled back to prevent the ion volume from hitting the ball valve as you connect the I/R tool.

4. Slowly pull the vacuum in handle interlock valve up.

5. Turn the I/R tool so that the pin slides through the groove labeled INSR. 6. Gently push the ion volume into the source. The I/R tool stops when the

volume is in place.

7. After the ion volume is in the source block, gently rotate the I/R tool

counterclockwise and pull back so that the pin on the handle comes out through the groove labeled EXTR.

Pin Groove

8. Push the handle down to close the vacuum interlock valve. 9. Remove the I/R tool. 10. Replace the inlet cover.

Installing a GC Capillary Column

Before starting this procedure, put on a lab coat and gloves.

Components become very hot and can present a burn hazard. Ensure that all parts are cool before beginning this procedure.

To install a GC capillary column: 1. Cool the transfer line.

2. Cool and vent the MS. See “Venting the MS.”

3. Move the ion volume about 2 mm away from the ion source block using the

I/R tool, this blocks the 1.0 mm ion volume hole and prevents the column from entering the ion volume. 4. Place the nut and graphite/Vespel® ferrule on the column.

5. Clip a few millimeters from the end of the column to remove any graphite

particles. 6. Position the nut and ferrule on the column. Insert the column through the

transfer line. Push it in a few times to check that it travels the full distance, and does not become caught. After the column stops, pull it back about 1 mm, and tighten the column nut and ferrule on the transfer line.

7. Check that the vacuum interlock valve is closed.

8. Start the MS and monitor the turbo pump speed until it reaches 90%. If 90%

is not reached in 10 minutes, there may be a leak. If so, stop the pump and fix the leak. See “Detecting Leaks Using Air Water Report.” 9. After the pumps run for 10-15 minutes, check the ion source pressure. The

pressure indicates the column placement. GC Ion Source Pressure and Column Placement GC Ion Source Pressures with GC flow 1-2 mL/min and Pressure Pulse not enabled Pressure mTorr 10 to 50 >50 Indication Typical operating pressure Column too far away from ion volume Corrective Action None Stop pumping down. Re-install the column. MS/MS Procedures

To do MS/MS procedures using Cal Gas: 1. Turn on Cal Gas.

2. Click the Define scan method icon.

3. In the Scan method, enter the Q1 mass and the mass range of the product

ions. In this example, 219 is the precursor mass and the product mass range is 50 to 300.

Optimizing MS/MS Parameters for Analytes

After selecting a precursor ion from the full scan spectrum of the analyte, determine the product ions as follows:

1. Set a mass range on Q3 that includes the Precursor Ion. 2. Run this reaction in increments of 5 eV steps.

The result is a chromatogram with several traces.

3. Click a peak to get a three-dimensional spectrum and see the product ion

distribution for each energy segment.

The following is an example of a single ion MS/MS experiment, which displays Signal to Noise (S/N) ratios.

1. Set Q1 to the Precursor Ion, and Q 3 to the Product Ion.

2. Enter several Collision Energies.

This creates a chromatogram with the traces of several ion pairs. 3. Click the Chro Display Options icon

Chro in the Mouse Clicks section.

and enable Display S/N Ratio in

The S/N ratio of the selected chromatogram is displayed on the top. The MSWS software denotes the selected chromatogram by using a different color for the axes.

Maintenance

Maintenance Procedure Intervals

Your MS may require maintenance more frequently than indicated depending on your sample load and composition.

Daily

• • • •

Check and if needed, refill the solvent wash vial on autosampler. Check the autosampler syringe and replace if necessary. Check for leaks. See “Checking for Leaks.”

Check the tightness of column nut on transfer line and injector.

Daily or Weekly

• • • • •

Replace or clean ion volume if needed. Replace the injector septum (50-200 injections). Replace insert and O-ring.

Clip column (8-30 cm, depending upon matrix).

If in use, check gas filters, carrier gas supply (>250 psi), and CI/CID gas supply.

Monthly

• • •

Autotune if needed. Clean the source if needed. Run Electronics Diagnostics.

2 to 3 Months

Check the level of the oil in the foreline pump. If the color is darker or if the oil is opaque, change the oil and the oil mist cartridge.

Variable

• • • •

Refill calibration gas bulb when empty.

Replace detector when optimum EDR calibration voltage = 2000V. Zero the collision cell after you vent the system.

Calibrate CI/CID pressures when you change the type of gas or if the pressure does not reach the setpoint.

Replace filament if broken, failing diagnostics or sensitivity is low. Replace column if necessary.

Drying Parts

Dry parts using one of the following methods:

• • •

Dry the parts with a stream of dry nitrogen or air. Air-dry the parts in a dust free environment.

Bake the parts in a GC oven set between 50 to 90 °C.

Dry the parts completely before installing them, to prevent contaminating the source.

Cleaning the Ion Volume

Before starting this procedure, put on a lab coat and gloves.

1. Use the ion volume insertion/removal tool to remove the ion volume from the

source block.

The ion volume may be hot. Rinse the ion volume with cool de-ionized water before handling.

2. Separate the assembly by untwisting the parts.

3. Clean all surfaces with a cotton swab and a fine abrasive such as size 15

WCA type aluminum oxide in a water or methanol based slurry. 4. After cleaning, rinse the parts by flushing them several times with water,

being sure to remove all visible aluminum oxide from the parts. 5. Sonicate the parts in water for three minutes. Change the water and repeat

the process two more times. 6. Remove the parts from the water and rinse several times with methanol. 7. Follow the “Drying Parts” procedure and check that the parts are completely

dry before reassembling the ion volume. 8. Reassemble the ion volume by holding the ion volume holder in one hand

and the ion volume in the other. 9. Line up the pins on the ion volume holder with the entrance slots on the ion

volume and push the two parts together. 10. Turn the ion volume holder clockwise to lock the two parts together. The

spring washer creates tension between the ion volume and ion volume holder to keep the pieces from coming apart.

Cleaning the Plug and Play Source

Overview

The parts of the Plug and Play Source that require regular cleaning are the ion volume and lenses 1, 2, and 3. Use these procedures to keep your Plug and Play GC Source in good working order, and to restore sensitivity. Sensitivity can degrade when GC effluent accumulates on these surfaces.

Required Materials

• • • • • •

Aluminum Oxide Cotton swabs Methanol rinse bottle De-ionized water rinse bottle Several glass beakers Sonicator

Removing the Plug and Play GC Source

Before starting this procedure, put on a lab coat and gloves.

1. Vent the MS, see “Venting the MS.”

2. Rotate the transfer line counterclockwise and gently pull the transfer line until

the column is outside of the source. 3. Unplug the GC/MS source cable and the inlet interlock cable. 4. Unscrew the two 5 mm socket screws that hold the source plug on the

manifold. 5. Remove the source plug from the MS by pulling it straight back. NOTE: Be careful not to break the GC column.

6. Disconnect the CI gas line, which is a Teflon® tube, from the source block. 7. Loosen the two finger screws holding the Ion Guide Assembly on the Probe

Inlet Assembly.

8. Lift the Ion Guide Assembly off the Probe Inlet Assembly. 9. Lift the Lens Stack Assembly off the Ion Guide Assembly.

Disassembling the Source Components

1. Remove the two lens stack screws.

2. Remove the lenses from the PCB heater rods.

Lens stack screws, 2 each Lens 2 PCB screws, 3 each Lens 1 Lens 3

Cleaning the Ion Source

Do not clean the ion source Printed Circuit Board or expose it to solvents.

Never expose the black anodized surfaces to abrasives or allow them to be scratched. If they are scratched they lose their insulation properties, electrical breakdown may occur, and they may fail electronic diagnosis. Replace any lens if the black anodized material is scratched completely through to the base metal.

Before starting this procedure, put on a lab coat and gloves.

1. Prepare a clean and dust-free-work area.

2. Clean all stainless steel surfaces thoroughly with a cotton swab and a fine

abrasive such as size 15 WCA type aluminum oxide in a water based slurry. 3. After cleaning, rinse the parts by flushing them several times with water, to

remove all visible aluminum oxide from the parts. 4. Place all cleaned parts in a sonicator and sonicate in water for 3 minutes. 5. Change the water and repeat the process two more times.

6. Remove the parts from the water. 7. Rinse the parts thoroughly with methanol.

8. Dry the parts completely, refer to \"Drying Parts,” before reassembling the ion

source.

Assembling the Ion Source

1. Place lens 1 over the PCB heater rods on the ionization block. The pin on

lens 1 must be adjacent to the CI gas line connector. 2. Place lens 2 over the heater rods so that its pin is in the opposite direction of

the lens 1 pin. 3. Place lens 3 over lens 2 with the screw holes aligned with the PCB screw

holes. 4. Install the 2 screws that hold the lens on the PCB.

Installing the Ion Source

Before starting this procedure, put on a lab coat and gloves.

1. Place the source assembly on the lower source frame with the source block

facing away from the lower source frame. 2. Place the upper source frame on the lower source frame and tighten the

finger screws. 3. Attach the CI gas line, which is a Teflon® tube.

4. Gently insert the plug and play source into the MS system so that the lens 4

pins contact their respective pin receptacles. NOTE: Do not break the lens 4 connector board pins.

5. Tighten the two 5 mm socket screws that hold the source plug on the

manifold. 6. Attach the GC/MS source cable and the inlet interlock cable. 7. Re-install the transfer line.

Install the Ion Volume

1. Follow \"Installing an Ion Volume\" procedure.

2. Turn the pump on and let the instrument pump down overnight before tuning.

Cleaning the Hexapole Pre-quad Assembly

To clean the hexapole pre-quad assembly:

1. Cool down and vent the instrument following “Venting the MS.” 2. Remove the plug and play source from the MS. 3. Remove the hexapole from the plug and play frame.

4. Disconnect the 2 red wire leads that connect the ion guide to the frame.

5. Unscrew the 2 small screws that hold the beige, plastic top of the hexapole to

the frame. 6. Pull the hexapole out of the frame.

7. Cleaning does not require disassembly. The leading edge of the Hexapole

blades (the ends closest to the source block and lenses 1-3), and the inner faces of the blades are the areas that most often need cleaning. Scrub the dirty surfaces with a clean swab and slurry of aluminum oxide and de-ionized water. 8. Completely rinse all aluminum powder from the rod surfaces using de-ionized

water then clean methanol. 9. Wipe the surfaces of the Hexapole dry with a lint-free cloth, or blow the

surfaces dry with clean gas. 10. Re-attach the hexapole to the plug and play source, and reinstall the source

into the MS.

Refilling the Calibration Gas

To refill the calibration gas:

1. Remove the Cal Gas glass bulb.

2. Add some PFTBA (FC-43), but do not fill it higher than the glass, tapered

neck. NOTE: Do NOT fill the bulb above the glass, tapered neck. The bulb holds about 0.5 mL of solution.

3. Re-install the glass bulb.

Changing the Filament

1. Cool down and vent the instrument, using the “Venting the MS” procedure. 2. Remove the glass top, following “Removing the Glass Top.” 3. Use forceps to remove the filament ceramic block from the source.

The following picture shows a filament that has excessive carbon deposits on the ceramic body. The deposits can form a leakage path to the grounded source body and mimic emission current. This decreases the emission current.

Ceramic Body

4. Insert the new filament ceramic block. Verify that the pins are in the sockets

and not above, below, or on the sides of the socket. 5. Replace the glass top, being careful to prevent any dust or debris from falling

into the manifold area. 6. Pump the system down.

7. Verify that vacuum is established in about 10 minutes, if not check for leaks. 8. Re-tune the instrument.

9. Reset the MSWS filament statistics by following “Resetting the Filament

Statistics.\"

Resetting the Filament Statistics

To reset the filament statistics:

1. On the Quads toolbar, click the Tools menu. 2. Click Troubleshooting.

3. Click EI/CI Filament statistics in the Others section. 4. Click Execute.

Troubleshooting

The key to successful troubleshooting is isolating the problem. Determine which module is the source of the problem. It is good practice to start with the last known working configuration of your system. User Bruker test samples to verify correct operation.

Find the description of your problem in the Observation column and follow the suggestions in the Solution column. If you cannot resolve the problem, call your Bruker service representative. Troubleshooting Observation MS not communicating with the PC. MS not communicating with the GC. Ion Gauge does not turn on. Solution Check that the MS and GC are plugged in and turned on. Check that the serial cable is connected from the PC to the MS. Shutdown and restart System Control. Check that the cable is connected from the PC to the GC. Check that the pump is turned on in System Control by clicking the Set Instrument Parameters icon and choosing the Analyzer tab. Check that the serial cable is connected from the MS to the PC. Check that the foreline pump is plugged into the MS. Check that the pump switch on the back of the MS is in the on position. Check that the turbo pump blades are spinning. Check that the foreline pump is functioning by listening for noise or feeling vibration. Check that the hose connections are secure on the foreline pump and the MS. Check that the interlock valve for the ion volume is closed. Check that the transfer line is tightly connected to the MS. Check that the column is installed and not broken. Check that the glass top is sealing onto the manifold O-ring. Press the glass top to verify the glass is not warped and is sealing properly. If no problems with the above checks are detected, install the MS plug, pump down, and check again for leaks. If the MS does not leak when plugged, refer to this manual to find large leaks. If the MS still has a large leak when plugged, check the valve block for leaks using Dust-Off type spray with Freon. See “Ion Gauge does not turn on’, which is above. Check that the carrier gas flow is 1-2 mL/min. If pressure pulse is enabled on the GC, the column flow increases, causing the source pressure to be higher than normal while the pulse is enabled. Check that the correct (EI) ion volume is installed. Check that the column is correctly installed into the transfer line. If the column is too far away from the ion volume, the source pressure is high. NOTE: If solvent flush is enabled, the source pressure will rise significantly (up to 10Torr) during the beginning of an EI analytical run, but should start dropping before the filament turns on. This is normal functioning in solvent flush mode when using EI ionization. To check the solvent flush setting, open System Control and click on Configuration> Options > Advanced MS Options. This window displays the EI Solvent Flush as either ‘enabled’ or ‘disabled’. Enable solvent flush to minimize the solvent baseline caused by solvent accumulation in the CI line when running in EI mode. Check that the GC carrier gas flow is 1-2 mL/min. Foreline Pump gurgles continuously. Large leak. Turbo Pump is not spinning. Source Pressure is too high (>50mTorr in EI mode). Source Pressure is too high (>50mTorr in EI mode). (cont.) Source pressure is too low 32

Troubleshooting Observation (<10mTorr in EI mode). No peaks or small peaks. Solution Check that the column is correctly installed into the transfer line. If the column is too far into the source, the source pressure will be low. Check that the standard was prepared correctly. Scan with cal gas on to check MS sensitivity. If no or low cal gas (FC-43) peaks: Check/refill cal gas bulb. Check that the scan range includes cal gas ions (60-550). Check for leaks. Replace or clean the ion volume. Raise the detector voltage. Clean the source and hexapole and retune the instrument. Retune the instrument. Replace the filament. Replace the Electron Multiplier (detector). Check the sample preparation. Check the transfer line nut for leaks; tighten if necessary. Check that the transfer line is installed correctly in the GC oven so there is not a cold spot (make sure the GC is not too far away from the MS). Manually (do not use autosampler) inject standard into the GC, if still no or low peaks: Check/correct the column parameters in the GC Configuration page. (Press the status button in the instrument section of the GC front panel, then choose Setup>View Instrument setup>View column parameters). Replace the septum on the GC injector. Replace the injector insert and O-ring. Clip 8-30 cm off the column at the injector end and replace the column ferrule. Check for leaks at the injection port; refer to \"Leak Troubleshooting.\" If still no or low peaks with manual GC injection: Vent the MS and clip a few cm off the MS end of the column. Re-install column and pump down. If still low, replace the column. Check/replace autosampler syringe. Verify autosampler or purge and trap are functioning. If using fixed voltage detector setting: • Optimize the detector or lower the detector voltage. • Switch to EDR mode. • Check/set GC split flow. • Check concentration of the standard; dilute if necessary. If using the EDR detector setting: • Check set GC split flow. • Check standard concentration; dilute if necessary. NOTE: EDR extends the dynamic range of the MS, but the GC may be overloaded at very high concentrations, causing carryover or other contamination problems. If cal gas peaks are present and not too low, and GC injection of a standard has no or low peaks: Excessive signal (Saturated detector). 33

Troubleshooting Observation Tuning problems Solution Low Sensitivity • Follow steps for “no/small peaks”, in this table. • Poor sensitivity in Positive CI Mode: • Replace/clean the ion volume. • Clean the source. NOTE: PCI sensitivity will degrade significantly with water in the ion volume and source. Noisy baseline in AutoTune: • Possible moisture in system; pump down longer at a high source temperature (300 °C) and try again. • Poor peak shape or resolution: • Retune. • Replace the ion volume. • Clean the source. • Clean the hexapole. • Poor Quad #1 vs. Quad #3 sensitivity or the other way around: • Possible particulate contamination of the Quadrupole. Contact the Bruker Service Representative. The source may be oxidized due to leaks, or dust on the quadrupole(s). • Clean the ion volume and source then perform a leak check (you may not find leaks before you clean the volume and source if low mass ions are suppressed due to source oxidation). • Schedule a visit from your Bruker Service Representative to clean the Quadrupole(s). Replace the filament. Check that the filament rods were inserted correctly into the ceramic source printed circuit board (PCB). If error still occurs, inspect the PCB source for cracks. Check/replace the source ceramic printed circuit board (PCB). Confirm that the Sync Start Cable (part number 393717901) is connected to the User I/O connector on the MS and to the J6 connector on the GC. Confirm that the Sync Start cable is enabled in the software: Low mass ions are absent or have low intensity. Broken filament error. Source temperature fluctuating. Poor retention time stability. Poor retention time stability. (cont.) Check for leaks in the GC. Confirm that the actual oven temperature follows the GC program, or the oven temperature is stable if an isothermal program is running. Replace the column. Baseline is too low. If the baseline is low, the problem may be due to GC injector contamination. See Contamination in this table. 34

Troubleshooting Observation Baseline is too high. Solution Retune the MS. If the problem persists, try to eliminate possible sources by starting a GC run with no sample injection (press the start switch manually). If the baseline remains high, check the spectra when running EI full scan and determine if it matches common contaminants listed in the Contamination section that follows. If there is a high solvent baseline in EI mode, check that the solvent flush is enabled in the software and helium is plumbed to the MS. Check the solvent flush setting, by opening System Control and clicking Configuration > Options > Advanced MS Options. If the baseline is high at the beginning of the run and drops off at the end, the problem is probably solvent related. If the baseline increases at the end of the run and never comes down, the problem is usually column bleed. Isolate the MS from the GC using the MS plug and scan the MS. If contamination ions remain, clean the ion volume, source, and hexapole. Swab manifold with solvent using lint -free tissue. If isolating the MS removes contamination, contamination is coming from the GC or the carrier gas. See the following possible sources of contamination. Check the injection technique for your application. Tailing chromatographic peaks are usually caused by GC problems. Check the GC for leaks. Check that the transfer line is installed correctly in the GC oven so there is not a cold spot (make sure the GC is not too far away from the MS). Check that the transfer line temperature is at or slightly higher than the highest temperature in the GC ramp (do not exceed the maximum allowable temperature for the column). Replace the insert, O-ring, and septum. Clip 8-30 cm off the injector end of the column. Replace the column. Usually due to overloading the column. Dilute the sample or increase the split ratio. If problem persists, replace the column. The stationary phase may have degraded. If the method is being developed: • Optimize the GC oven program. • Optimize the GC flow. • Try a column with a different stationary phase. If the method has worked before: • Replace the column because it may have degraded. Contamination. Peak Tailing Peak Fronting Poor resolution of chromatographic peaks 35

Troubleshooting Observation Poor Peak Area Reproducibility * Reproducibility can be sample dependant. Compare current performance to previous performance or to expectations for an unknown or new sample/method. Solution Visually check that the autosampler syringe is pulling up the sample. Check that the GC injector nut is tight. Flush the autosampler syringe with solvent. Replace the autosampler syringe if necessary. Replace the septum regularly and ensure that the septum nut is tight. Check the installation of the column in the injector. Tighten the capillary column nut. Change the injector insert and O-ring. Clip 8-30 cm of column off the injector end. Check the transfer line nut for leaks; tighten if necessary. Replace the column. Check the following injector parameters: Injector is hot enough to vaporize the sample completely. Injector is not operating at too high of a temperature Split is optimized. Sample size does not exceed insert capacity. Autosampler parameters are compatible with sample viscosity. Tighten the transfer line column nut (If there was a leak, clean the ion volume and source in case the surfaces were oxidized. Check for leaks in the MS and the GC. Retune the MS. Clean the ion volume, source, and hexapole, and then retune. Sources Of Contamination Ion(s) 18, 28, 32 40 44 149 207, 281 Groups of peaks14 amu apart Contamination Sources Air and water, possible leak. Argon, possible carrier gas contamination. Carbon dioxide, possible carrier gas contamination or purge and trap by-product. Phthalates (found in plastics/gloves). Column/septum bleed. Hydrocarbons (possibly pump oil or fingerprints). Ion(s) 31, 32 57 91, 92 49, 84 43, 58 Solvent Contamination Sources Methanol Hexane, isooctane Toluene (in paint, nail polish and other products) Methylene Chloride (Dichloromethane) Acetone

Leak Troubleshooting

Overview

Air leaks and water leaks are common problems. Leaks may reduce sensitivity, tuning problems, and decreased resolution. They may reduce the lifetime of the capillary column, filaments, turbomolecular pump, and the electron multiplier. Check your system daily for air and water leaks before running samples.

Checking for Leaks

Determine if the leak is coming from the MS or the GC by doing the following: 1. In System Control, select Plot, tics, readbacks from the Tools menu. 2. Open the TIC view.

3. Increase the carrier gas flow from 1 mL/min to 2 mL/min.

4. If the signal of the 28 m/z ion increases or decreases and the plot in the TIC

changes then the leak is probably in the GC. Do maintenance on the injector. 5. If the trace remains stable then the leak is probably in the MS. 6. Check that the column nut is tight on the transfer line.

7. If the column nut is secure, set the scan range from 10 to 100 and spray a

Freon based Dust-Off® type spray around the seals, column nut, transfer line O-ring, glass cover O-ring, and the interlock. If you do not have this product, use the argon supply for the CID gas. Spray the argon in short bursts at the seals and look for the 40 m/z ion. 8. If necessary, plug the MS at the transfer line and generate an air/water

report. 9. From the Tools menu in System Control, select Troubleshooting and run the

Air and water report. 10. If there are no leaks from the plugged MS, connect the GC and look for GC

leaks.

Detecting Leaks Using Air Water Report

NOTE: Do this step only if the MS was tuned successfully before.

The ratios for air/water are relative and depend on the way the unit is tuned. Minor changes in the tune file can strongly affect the ratio of air/water ratio. Therefore, make sure a recent tune file is used, or if a recent tune file does not exist, re-tune the instrument.

To detect leaks using the Air water report:

1. In the Quads window click Tools and select Troubleshooting.

2. Select Air and water report, and then click Execute.

3. The following is a report in which the air/water check failed.

Comparing the 18/28 ion ratio to the calgas 69 ion does not provide information about leaks or high water. The amount of calgas in each instrument differs because it enters the system through a long piece of PEEK™ tubing. The amount of calgas that enters the source can depend on the dimensions of the tubing, ambient temperature, and so on.

Fixing Large Air Leaks

Typical sources of large air leaks are:

• • • • • • •

Loose transfer line nut.

Particles on or damage to the manifold flange O-ring seal. Particles on or damage to the transfer line O-ring seal.

Poor O-ring seal between the turbomolecular pump and the manifold. Scratched Ball valve.

Improperly tightened interlock assembly.

Loose fitting Valve block for CI/CID and FC-43 gases or poor O-ring seals.

Do not over tighten the fittings. Doing so may cause an even larger leak. Attempt to identify and eliminate the source of the leak without venting the system. If you cannot, vent the system, and check the O-rings on the manifold and transfer line for particles. Wipe both O-rings with a lint-free cloth.

If there is a leak, the turbomolecular pump will probably fail to reach 100%

speed. Do not operate the system under these conditions. If the pump does not reach 90% in 10 minutes after pump down, vent the system, and fix the leak.

Fixing Small to Moderate Air Leaks

Small to moderate air leaks are often more difficult to locate than large ones. One way to diagnose this type of leak is that the peak at 28 m/z will be bigger and significantly larger that the peak at 18 m/z.

Checking GC Connections for Air Leaks

NOTE: Check the GC manual section on maintenance for more information about troubleshooting leaks.

Locating and repairing leaks at the connections between the capillary column and injector or transfer line. Most transfer line connections occur on the high vacuum side, such as around the transfer line nut or O-ring.

•

Check that the size of the ferrules is correct. Use 0.4 mm ferrules for 0.25 mm I.D. columns. Use 0.5 mm ferrules for 0.32 mm I.D. columns Check that the ferrules are tightened one-half turn beyond finger tight. Check that the ferrule on the transfer line is made of a mixture of

graphite and Vespel. Do not use ferrules only made with graphite at this location because graphite can be pulled into the MS and create active sites on the source. Check that the ferrules are tightened one-half turn beyond finger tight.

•

Check the septum. Change the septum regularly, every 50-200

injections. Use high quality, low bleed septa to reduce the air bleed and background ionization of the septum material.

Check the injector nut. It should fit snugly. If it is worn or misshapen, replace it.

Check the GC pneumatics. Because these leaks are very difficult to detect, tighten all fittings one-half turn beyond finger tight.

Check the moisture/oxygen filters. If the filter becomes saturated, there may be an increase in the air/water background. Replace them at regular intervals and whenever there is moisture or the GC background is high.

• • •

Using Leak Detection Gas to Troubleshoot Air Leaks

NOTE: Use the leak detection spray very deliberately. Allow about a 10-second delay between spraying different fittings or you may identify the source of the leak incorrectly.

If you are using a Dust-Off® Freon based type gas, determine the major ions. The compound(s) and the CAS numbers are listed on the canister. Typical components include the following:

Leak Detection Gases and Their Major Ions Compound Tetrafluoroethene Difluoroethene Argon Major Ion (m/z) 83, 69 65, 51 40 To detect leaks using leak detecting gas:

1. Do a NIST search on either the name or CAS number of the compound and

check the spectra. 2. On the Tools menu in System Control, click Plot tic, readbacks.

3. In the Plot in pict view dialog box, click In use. Check either one or two

Area of mass check boxes and enter the mass of the gas for each. A graph is generated that displays a baseline spike when the gas is detected.

4. Spray a fine stream of leak detection gas on the transfer line nut.

5. Watch the Pict graph for a response.

• •

If the baseline does not rise immediately, the leak is not at the transfer nut.

If the baseline rises immediately, the leak is at the transfer line. Tighten the transfer line nut. If the leak persists, cool and vent the system, and replace the nut and ferrule. Pump the system down and check for leaks again.

6. Spray the injector.

7. Watch the Pict graph for a response.

•

If the baseline rises in a minute or two, the injector has a leak.

8. Check the following gaskets and fittings for leaks. Tighten the connections as

needed. After spraying the gas, wait 2-3 minutes before spraying again.

• • • •

Manifold O-ring Transfer line O-ring Valve block connections Carrier gas EFC connections

9. If you have not found the source of the leak, vent the MS. 10. Install the transfer line plug and pump the MS down.

11. From the Tools menu in System Control, select Troubleshooting and run the

Air and water report.

•

If no leak is detected with only the MS connected, the leak is at either the transfer line or the GC. a. Vent the MS.

b. To determine if the leak is in the transfer line, place a ferrule without

a hole in the transfer line nut and do not attach the column. c. Reattach the transfer line and pump the system down. •

If the plugged MS has a leak, check the MS using the leak detection gas.

Fixing High Water Levels

The presence of excess water vapor may be caused by:

• • • • • •

Insufficient bake out time (after you vent the system, bake it out for at least 24 hours). Cleaning the source.

Replacing the capillary column. Water vapor in the carrier gas tank.

An atmospheric air leak in the system. This may occur when the relative humidity is high. Saturated GC filters.

To remove excess water vapor:

1. Bake the system out for 2 days to eliminate the water vapor from the vacuum

system surfaces. 2. If water is still present, the carrier gas tank may be contaminated, moisture

may be collecting in cold spots, or there may be an air leak.

GC/MS Spare Parts GC Injector 2869458001 CR298777 392534201 390842300 190015800 200003400 7200008400 CR298713 391866308 RT210462145 394955100 8850103100 190010906 0.4 mm Graphite / Poly Ferrules BTO Septa 11.5 mm, 50/pk Ferrule Insert Graphite Injector Nut Wrench Ceramic Scoring Wafer Carrier Gas Line Assembly Septa Extraction Tool 9 mm Septa Screw Captive Micro Seal Inlet Sleeve, Siltek, 4 mm w/Frit, 5/pk Capillary Injector Nut Viton O-rings, 25/pk Inlet Sleeve, SPI, 0.5 mm, 5/pk Transfer Line Tip Pin, Ion Volume Filament Transfer Line Assy, Ion Volume Holder Inert FC 43 Calibration Gas EI Ion Volume CI Ion Volume PCB Assembly, Ion Source M2x5 Screw Lens 1, Ion Source Lens 2, Ion Source Lens 3, Ion Source Electron Multiplier (Detector) Allen Wrench for EM Dynode Pogo Pin for EM Main O-ring, Manifold Center Support O-ring Glass Top Premium Foreline Pump Oil DS-42 Oil Mist Filter Foreline Pump Oil (1L) Oil Mist Cartridge, 2/pk Injector Type 1079/1177 1079 1079 1079/1177 1079/1177 1079/1177 1079/1177 1177 1177 1177 1079/1177 1079/1177 1079 Mass Spectrometer 393743001 CUB0200053 9300000400 393749401 9300020500 392035300 9300020300 9300020200 393853201 1216810200 393777301 CUB0300006 393826501 393705201 393776001 5145281600 CUB0200239 2740229500 393785501 8829953800 393847701 DS-102 Foreline Pump 8829951700 2710100200 DS-42 Foreline Pump 42

Foreline Pump Maintenance

Checking Foreline Pump Oil Level and Condition

The oil level must be between the maximum and minimum levels on the sight glass. If the oil level falls below the minimum level, use a funnel to add more oil gradually through the filler port until the oil level reaches midpoint.

NOTE: Pump models are subject to change. If not using a DS-42 pump, refer to the pump manual for details.

The pump oil should be clear and light in color. If the oil becomes opaque, dark in color, or has a burnt smell, change it.

Foreline Pump Oil and Cartridge

Change the oil and the cartridge while the oil is warm but not immediately after stopping the pump.

Tools and Materials

Tools

• • Oil

• • • •

DS-42 Premium Foreline Pump Oil (part number 8829953800) DS-102 Pump Oil (part number 8829951700) DS-42 Oil Mist Filter (part number 393847701)

DS-102 Oil Mist Cartridge pack of 2 (part number 2710100200) 5/16 in. Allen Wrench

1 liter (1 US qt) or larger container

Filter or Cartridge

Changing the Pump Oil

Changing the pump oil involves the following procedures:

Preparing the Pump

1. Turn off and vent the MS. Refer to “Venting the MS.”

2. Disconnect the power cord of the pump from the rear of the MS.

Use proper eye and skin protection.

Hot Surface. Take appropriate precautions. Wait for the pump cool enough to handle before changing the oil.

3. Remove the clamping ring and disconnect the vacuum hose from the foreline

pump. 4. Pull the hose free, and place the seal on a clean lint-free surface for later

use.

The pump weighs about 22 kg (48 lb). Use proper lifting techniques to avoid injury.

Hazardous chemicals may be present in the used pump oil. Wear a lab coat and gloves to avoid contact with skin.

5. Carefully place the foreline pump on a raised surface. The surface should be

high enough to allow a 1.0-liter (1 US quart) or larger container to be placed under the drain port when the pump is tilted forward. Use a container with an opening diameter of at least six inches to make this task easier. 6. Place an oil pan beneath the drain port to catch spills.

Draining Pump Oil

1. Remove the filler plug on top of the pump.

2. Put the container in place to catch the oil, and then slowly remove the drain

plug using a 5/16 in. Allen wrench.

Toxic residues from MS samples build up in used pump oil. Dispose of all used pump oil in accordance with applicable regulations. Place a hazardous chemical warning label on the container.

3. Tilt the pump forward and hold until the flow stops. 4. Place the pump flat and refit the plug.

5. Run the pump for approximately ten seconds with the intake port open. This

removes residual oil from the pumping block.

Avoid breathing oil mist coming from the exhaust port.

6. Remove the plug, tilt the pump, and drain any remaining oil. Place the pump

flat. 7. Wipe the oil residue from the drainage port, and refit the drain plug.

Adding New Pump Oil

1. If the pump oil was particularly dirty, flush the pump oil. Use a funnel to fill the

pump with fresh oil through the filler port until the oil level reaches mid level in the sight glass. Replace the filler plug. 2. Run the pump for at least one hour with the gas ballast valve open to achieve

a good vacuum. 3. Change the oil mist filter when the oil is changed.

Flushing the Pump Oil

If the oil was very dirty, flush the pump after draining the pump.

Avoid breathing oil mist coming from the exhaust port.

1. Remove the inlet filter with a pair of tweezers or long nose pliers.

2. Clean the filter in warm soapy water. Rinse and blow-dry with air or nitrogen. 3. Reinsert the filter.

4. Pour about 100 mL of fresh pump oil in through the inlet port then run the

pump. 5. Stop the pump, drain the flushing oil, and then continue filling with fresh oil.

Changing the DS-42 Oil Mist Cartridge

To disassemble the oil mist eliminator: 1. Unscrew and remove Upper housing. 2. Remove Spring 2. 3. Remove Valve 3. 4. Remove Cartridge 4.

5. Clean the parts with a dry cloth.

6. Degrease the parts with a water soap solution. 7. Rinse with clean water and dry. To reassemble the oil mist eliminator: 1. Install a new cartridge.

2. Press gently to check that it is firmly seated.

3. Install Valve 3 so that the raised center fits inside the cartridge. 4. Center the Spring 2 over the Valve 3.

5. Cover the entire assembly with Upper housing 1, ensuring that the O-ring

gasket is flush against the housing. 6. Tighten Upper and Lower housings.

NOTE: After changing the cartridge several times, it may be necessary to replace the O-ring gasket.

Changing the DS-102 Oil Mist Cartridge

To disassemble the oil mist eliminator: 1. Remove assembly screws A. 2. Remove Upper housing B. 3. Remove Spring C. 4. Remove Valve D. 5. Remove Cartridge E. 6. Remove -ring F.

7. Clean the parts with a dry cloth.

8. Degrease the parts with a water soap solution. 9. Rinse with clean water and dry.

To reassemble the oil mist eliminator:

1. Install a new cartridge in Lower housing B. 2. Press gently to check that it is firmly seated. 3. Install Valve D with polished side toward cartridge. 4. Center Spring C over Valve D, fit gasket, F in the groove. 5. Cover entire assembly with Upper housing B.

6. Tighten Upper and Lower housings B, using screws A.

NOTE: After changing the cartridge several times, it may be necessary to replace the gasket and the centering O-ring gasket.

Appendix

Synchronization Signals for External Modules

Input and output signals can be used for external modules or devices. These modules include purge and trap concentrators, direct insertion probes, and

fraction collectors. Communication with these external devices requires the use of the I/O (Input/Output) Connector PWA (Printed Wire Assembly). Bruker part number CUB0600047. To obtain the I/O board part number CUB0600047, order the kit, part number, 0393847890, which has the I/O board and instructions. The following are pictures of the I/O connector PWA with the connections removed.

I/O Connector PWA with connectors removed (part number CUB0600047)

Hardware Setup

1. Connect the appropriate cable from the external device or module to the

connector on the I/O Connector PWA. Tighten the retaining screw on each wire. Gently pull the wire to ensure the connection is secure. 2. If an external device is to start the instrument, then a Start-In signal is

required. Connect the appropriate wire from the external device to #1 and #2, and the other wire to #3 and #4 on the 6-pin connector of the I/O Connector PWA. For this example, plug the connector into J5 (Row 1, Column A). The following is a picture of a Start-In Signal cable with jumper wires.

The following is a picture of a typical Start-In Signal cable connected to the I/O Connector PWA.

NOTE: Use the correct connector type (6-pin or 8-pin). Ensure that the connector is plugged into the correct jack on the I/O PWA. The wiring schematics in the software shown in step 2 specify the jack connector (J2, J4,J5, or J7) and the Row and Column position (Row 2 Column A, Row 2 Column C, Row 1 Column A, or Row 1 Column C, respectively).

3. The software has setups for Start and Ready configurations. From the Quad

Tool bar, click Configuration and then Sync signal. 4. The following are examples. The left side of the schematic is the instrument

and the right side is the connection to/from the external device. ‘In’ refers to ‘into the instrument’ and ‘out’ refers to ‘out of the instrument.’ For example, a ‘Start-In Signal’ sends a signal INTO the instrument to start it.

5. Before connecting the I/O Connector PWA to the instrument, remove the two

screws and two nuts, if present on the 37-pin DSUB connector on the I/O PWA to ensure a good connection.

6. Connect the I/O Connection PWA to the D37 connector on the back of the

instrument. Use the two screws from step #3.

Software Setup

1. Open System Control from the MS Workstation software.

2. In the Quad Module, click the Configuration, and then Sync signals.

3. Click Advanced in the Sync Signals window.

因篇幅问题不能全部显示，请点此查看更多更全内容

查看全文