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Troubleshooting

157

Problem

Probable Cause

Solution

Poor sensitivity (correct
amount of sample is reaching
the mass spectrometer).

Column is improperly
positioned in the ion
source.

Reinstall the column and
check the cut at the end
that fits in the source.

Improper tuning, or a
dirty or defective ion
source.

Check the tuning. Increase
the multiplier voltage.

Shut down the system,
remove the inner source,
clean or replace lenses in
the outer source, and
install a new filament.

Loss of resolution (especially
at high mass).

Dirty prequadrupole rods.

Clean the prequadrupole
rods.

Mass assignment drifts.

Large temperature
fluctuations in the
laboratory.

Stabilize the lab
temperature, or isolate the
GC/MS system from large
temperature fluctuations.

Mass assignment incorrect.

Run mass calibration.

Skewed spectra.

Improper scan speed (too
slow for the narrow peaks
produced by capillary
columns).

Increase the scan speed.

Unusually high repeller
voltage.

Repeller dirty.

Clean repeller.

Содержание Clarus SQ 8 MS Series

Страница 1: ...CLARUS SQ 8 MS Hardware Guide GAS CHROMATOGRAPHY ...

Страница 2: ......

Страница 3: ...Clarus SQ 8 MS Hardware Guide ...

Страница 4: ...in connection with furnishing performance or use of this material Copyright Information This document contains proprietary information that is protected by copyright All rights are reserved No part of this publication may be reproduced in any form whatsoever or translated into any language without the prior written permission of PerkinElmer Inc Copyright 2017 PerkinElmer Inc Trademarks Registered ...

Страница 5: ...nation 25 Cleaning the Instrument 25 General Laboratory Safety 26 Compressed Gases 26 Ventilation 27 Heated Zones 28 Using Hydrogen Methane or Isobutane 28 Using Ammonia Gas 29 Hazardous Chemicals 30 Definitions in Warning for Hazardous Chemicals 32 Temperature Humidity and Environment 33 Operating Conditions 33 Storage Conditions 35 General Laboratory Safety 35 Cleaning Requirements 35 WEEE Instr...

Страница 6: ...m System 58 Rotary Pump 58 Vacuum Pump Options 59 TurboMass Software 61 Top Level Screen 61 Tune Page 61 Analytical Column 63 Pre Operational Checklist 64 Maintenance 65 Overview 68 Typical Overall Maintenance Schedule 71 Daily 71 Weekly 71 Monthly 72 Every Six Months 72 Yearly 72 Leak Checking 73 Tuning the Clarus MS 76 Preparing Clarus MS for Hardware Maintenance 78 Removing and Returning the So...

Страница 7: ...ervice Representative Only 112 Items and Tools Required 112 Cleaning Materials 113 Removing and Returning the Ion Optics Assembly 114 Replacing the Electron Multiplier 124 Cleaning the Prequads 125 Changing to CI 135 Leak Checking 136 Setting Up CI 138 Troubleshooting 145 Overview 147 Spare Components 148 Logical Troubleshooting Steps 148 Troubleshooting Chart 150 Chromatography Related 161 Spectr...

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Страница 9: ...Warnings and Safety Information 1 ...

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Страница 11: ...l text is used to provide information and instructions Bold text refers to text that is displayed on the touch screen All eight digit numbers are PerkinElmer part numbers unless stated otherwise Notes warnings and cautions Three terms in the following standard formats are also used to highlight special circumstances and warnings NOTE A note indicates additional significant information that is prov...

Страница 12: ... como éste se proporciona información sobre este tipo de circunstancias F Warning Danger Nous utilisons la formule WARNING DANGER pour avertir des situations pouvant occasionner des dommages corporels à l utilisateur ou à d autres personnes Les détails sur ces circonstances sont données dans un encadré semblable à celui ci I Warning Pericolo Con il termine WARNING PERICOLO vengono segnalate situaz...

Страница 13: ...s En recuadros éste se proporciona información sobre este tipo de circunstancias F Caution Attention Nous utilisons le terme CAUTION ATTENTION pour signaler les situations susceptibles de provoquer de graves détériorations de l instrument ou d autre matériel Les détails sur ces circonstances figurent dans un encadré semblable à celui ci I Caution Attenzione Con il termine CAUTION ATTENZIONE vengon...

Страница 14: ...Customer Service Company Name and Address PerkinElmer 710 Bridgeport Avenue Shelton Connecticut 06484 4794 USA Tel 800 762 4000 or 203 762 4000 ...

Страница 15: ...ed does not exceed the level above which radio and telecommunications equipment or other equipment cannot operate as intended it has a level of immunity to the electromagnetic disturbance to be expected in its intended use which allows it to operate without unacceptable degradation of its intended use South Korea This device complies with MSIP Ministry 0f Science ICT and Future Planning EMC Regist...

Страница 16: ... communications Operation of this equipment in a residential may cause harmful interference in which user will be required to correct the interference at their own expense NOTE Changes or modifications not expressly approved by PerkinElmer could cause the instrument to violate FCC U S Federal Communications Commission emission regulations and because of this violation could void the user s authori...

Страница 17: ...ctor terminal Ground Off position of the main power switch On position of the main power switch Warning Risk of electric shock Avertissement Risque de choc électrique Warning Hot surface Avertissement Surface chaude Warning Refer to accompanying documents Avertissement Se référer aux documents d accompagnement Vacuum ...

Страница 18: ...Label Location and Content Figure 1 Front View of Clarus SQ 8 T ...

Страница 19: ...ervice qualifié de PerkinElmer avant d exécuter n importe quelle ligne essais à C A Avertissement La continuité du circuit de mise à la terre est indispensable au fonctionnement en toute sécurité de l équipement Ne faites jamais fonctionner l équipement lorsque le conducteur de mise à la terre est déconnecté Avertissement Démontez la corde de courant alternatif du débouché avant d enlever toute la...

Страница 20: ...cune couverture ou pièces enlevées Avertissement RETIRER LE CAPUCHON EN BLANCHE DE VENT LINE À L INSTALLATION Attention Cette unité contient les circuits protecteurs Contactez le personnel de service qualifié de PerkinElmer avant d exécuter n importe quelle ligne essais à C A Avertissement La continuité du circuit de mise à la terre est indispensable au fonctionnement en toute sécurité de l équipe...

Страница 21: ...tices for the laboratory and safety practices for the mass spectrometer Get advice from your safety engineer industrial hygienist environmental engineer or safety manager before you install or use this instrument Moving the Clarus SQ 8 MS WARNING The Clarus SQ 8 MS is 48 kg 105 lb in weight The mass spectrometer requires two people to safely lift it and should be lifted from the bottom Use the fol...

Страница 22: ...s can still be present Capacitors inside the instrument may still be charged even if the instrument has been disconnected from all voltage sources WARNING High voltage The Clarus SQ 8 MS contains high voltage To prevent the risk of shock unplug the line cord from the AC outlet and wait at least one minute before opening or removing any instrument panel AVERTISSEMENT Haute tension Le MS Clarus SQ 8...

Страница 23: ...sure satisfactory and safe operation of the mass spectrometer it is essential that the protective ground conductor the green yellow lead of the line power cord is connected to a true electrical ground Any interruption of the protective ground conductor inside or outside the mass spectrometer or disconnection of the protective ground terminal may impair the protection provided by the mass spectrome...

Страница 24: ...lors de leur entretien WARNING Do not make adjustments replacements or repairs to the Clarus SQ 8 MS except as described in the supplied user manuals Only a PerkinElmer Service Engineer or similarly trained and authorized person should be permitted to service the Clarus SQ 8 MS AVERTISSEMENT Ne faites pas d ajustements de remplacements ou de réparations dans le MS de Clarus SQ 8 à l exception de c...

Страница 25: ...to the descriptions in the Clarus GC Installation Guide P N 09936590 or 09936779 Servicing of electrical components within the mass spectrometer should be performed only by a PerkinElmer Service Representative Servicing of the incoming AC power line components in your laboratory should be performed only by a licensed electrician WARNING Electrical shock hazard To prevent electrical shock disconnec...

Страница 26: ... 8 MS porter toujours des gants de nitrile de nylon ou de PVC sans pelu sans peluches sans poudre avant de toucher d enlever ou de remplacer les pièces sur ou dans l ensemble de collecteur sous vide Ces éléments comprennent la source le filament les pré quads les quads analytiques et le multiplicateur d électrons Conservez toujours la source EI ou CI par son handle Ne touchez jamais ces pièces ave...

Страница 27: ...ation Procedure and complete the Certificate of Decontamination These documents are available on the PerkinElmer public website http www perkinelmer com Content technicalinfo dts_instrumentdeconprocedure pdf If you do not have access to the internet contact Customer Care Customer Care USA 8 30 a m 7 p m EST 1 800 762 4000 inside the USA 1 203 925 4602 outside the USA Customer Care Canada 800 561 4...

Страница 28: ...ec un soin extrême Les bouteilles de gaz peuvent être dangereuses si elles sont mal manipulées Avoid banging the valves and ensure that the correct valves and gauges are installed Gas cylinders should be stored and placed outside the laboratory and connected to the instrument through specially cleaned copper tubing Use care to prevent kinking or stressing the gas tubing For safety cylinders should...

Страница 29: ...rs de l analyse de composés dangereux tels que les pesticides il est nécessaire d organiser l évacuation de l effluent du spectromètre de masse à partir de l échappement de la pompe avant dans une hotte ou un piège à charbon In addition adequate ventilation must be provided particularly if a liquid nitrogen or carbon dioxide sub ambient accessory is in constant use The area underneath the bench ar...

Страница 30: ...to work in the GC oven on the transfer line on an injector around the detector areas or inside the Clarus SQ 8 manifold Proper cooling of the transfer line may take from 1 2 to 1 hour Using Hydrogen Methane or Isobutane WARNING Explosive Hazard If the hydrogen is turned on without a column attached to the injector and or detector fittings inside the oven the gas could diffuse into the oven creatin...

Страница 31: ...olonne est fixée tous les joints ont été éprouvés et le spectromètre de masse est sous vide avec l évacuation des gaz d échappement correctement évacué vers une hotte aspirante Using Ammonia Gas WARNING Hazardous gas vapors When using ammonia gas while running in the chemical ionization CI mode it is necessary to vent the mass spectrometer effluent from the forepump exhaust into a fume hood or cha...

Страница 32: ...ompage Be aware that the chemicals that you use in conjunction with the Clarus SQ 8 may be hazardous DO NOT store handle or work with any chemicals or hazardous materials unless you have received appropriate safety training and have read and understood all related Material Safety Data Sheets MSDS MSDSs give information on physical characteristics precautions first aid spill clean up and disposal p...

Страница 33: ... hazardous after completion of an analysis The responsible person for example the Lab Manager must take the necessary precautions to ensure that operators and people in the surrounding workplace are not exposed to hazardous levels of toxic substances chemical or biological as defined in the applicable Material Safety Data Sheets MSDS or OSHA ACGIH or COSHH documents Venting for fumes and disposal ...

Страница 34: ... applicables MSDS ou OSHA ACGIH ou documents COSHH L évacuation des fumées et l élimination des déchets doivent être conformes à toutes les réglementations et lois nationales nationales et locales en matière de santé et de sécurité Definitions in Warning for Hazardous Chemicals Responsible body Individual or group responsible for the use and maintenance of equipment and for ensuring that operators...

Страница 35: ...old Room or a refrigerated area Clarus SQ 8 MS operates under the following conditions Ambient temperature is 10 C to 35 C 50 F and 95 F with a variability of less than 4 C 7 F The Clarus SQ 8 MS will operate safely between 5 C and 40 C 41 F and 104 F If operating at ambient temperatures 10 C and 35 C you will need the water cooling option for the turbopump Ambient relative humidity is 20 to 80 no...

Страница 36: ...ondensation L altitude de fonctionnement est comprise entre 400 et 2000 m 1 312 à 6 562 pieds WARNING The mass spectrometer is not designed for operation in an explosive environment The laboratory should be free of flammable explosive toxic caustic or corrosive vapors or gases and should be relatively free of dust AVERTISSEMENT Le spectromètre de masse n est pas conçu pour fonctionner dans un envi...

Страница 37: ...quipment ordinarily required for the safety of individuals working with chemicals fire extinguishers first aid equipment safety shower and eyewash fountain spill cleanup equipment etc Cleaning Requirements Exterior surfaces of the MS may be cleaned with a soft cloth dampened with a mild detergent and water solution Do not use abrasive cleaners or solvents Before using any cleaning or decontaminati...

Страница 38: ... most effective means of protecting the customer s environment Requirements for waste collection reuse recycling and recovery programs vary by regulatory authority at your location Contact your local responsible body e g your laboratory manager or authorized representative for information regarding applicable disposal regulations Contact PerkinElmer at the web site listed below for information spe...

Страница 39: ...m 12 in wide x 44 cm 17 3 in high x 72 cm 28 4 in deep 25 9 kg 57 lb Clarus 680 GC 99 cm 39 in wide x 53 cm 21 in high x 82 cm 32 in deep 49 kg 108 lb Autosampler Tower 13 cm 5 in wide x 36 cm 14 in high x 24 cm 9 5 in deep 4 5 kg 10 lb Physical Configuration Single unit for use on standard laboratory bench that can be interfaced to a computer and printer Peripherals Printers etc Allow at least 94...

Страница 40: ...ase of a malfunction of the instrument For the Clarus SQ 8 S the AC power on off switch is on the back of the instrument Environmental Requirements Pollution Degree This instrument will operate safely in environments that contain non conductive foreign matter up to Pollution Degree 2 as defined in EN IEC 61010 1 Laboratory Environment Install the GC MS in an indoor laboratory environment that is c...

Страница 41: ...nd remain within the following tolerances Clarus MS 120 VAC 10 50 60 Hz 1 1000 VA maximum 230 VAC 10 50 60 Hz 1 1000 VA maximum Clarus GC For GC with slow heating rate as standard 120 VAC 10 50 60 Hz 1 20 Amps 2400 VA maximum 230 VAC 10 50 60 Hz 1 10 Amps 2400 VA maximum For GC with optional oven heater for fast heating rate 220 VAC 5 50 60 Hz 1 15 Amps 3120 VA maximum 230 VAC 5 50 60 Hz 1 16 Amps...

Страница 42: ...ass spectrometer always use copper tubing that is free of grease oil and organic material If in doubt about the condition of your tubing clean it before use Pour tous les gaz livrés au spectromètre de masse utilisez toujours des tubes en cuivre exempts de graisse d huile et de matière organique En cas de doute sur l état de votre tube nettoyez le avant utilisation Carrier Gases GC MS Carrier Gases...

Страница 43: ... purifiers for reagent gas is recommended Safety Requirements Gas Delivery Lines Copper tubing that is free of grease oil and organic material must always be used with the Clarus MS on all gas lines except ammonia reagent gas Ammonia reagent gas requires stainless steel Solvent washed copper tubing must be used to avoid contamination of the Gas Chromatograph Suitable solvents are acetone or dichlo...

Страница 44: ...ds such as pesticides it may be necessary to arrange to vent the mass spectrometer effluent from the forepump into a fume hood To prevent contamination if a fume hood is unavailable an oil separation filter should be installed at the outlet of the forepump vented to a fume hood or an oil mist separator Alcatel 68316 with a charcoal trap Koby KA1 An acceptable alternative is to attach a inch Tygon ...

Страница 45: ...______________________________ SPO __________________________________ Requirements OK Needs Prior To Installation Customer Responsibility Lab Space Requirements Power Requirements Gas Requirements Environmental Requirements Safety Requirements Preparation of Samples Customer Responsibility Computer Configuration Customer Experience ...

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Страница 47: ...Introduction 2 ...

Страница 48: ......

Страница 49: ... small profile of combination Gas Chromatograph and Mass Spectrometer GC MS allows it to fit on a standard six foot long laboratory bench Sophisticated software controls the GC MS from a Windows 7 computer System Overview The system consists of Clarus GC Clarus MS Computer TurboMass Software Foreline Pump ...

Страница 50: ...o check before using the instrument Chapter 4 Maintenance Contains preventive and routine maintenance procedures that typical users can perform Chapter 5 Troubleshooting Provides helpful troubleshooting tips and a table to help you identify and solve typical problems Related Documentation The Clarus ST8 family of manuals includes the following Clarus GC MS Tutorial part number 09931018 The tutoria...

Страница 51: ...s supplies training and service helps you meet both routine and demanding measurement challenges We invest heavily in testing and validating our products to ensure you receive guaranteed compatibility and performance on time every time for every instrument in your laboratory Supplies replacement parts and accessories can be ordered directly from PerkinElmer using the part numbers quoted in the gui...

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Страница 53: ...About the Clarus GC MS System 3 ...

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Страница 55: ...l as chemical ionization CI The Clarus SQ 8 S and SQ 8 T MS are electron impact EI only Figure 4 Clarus SQ 8 MS with Clarus 680 GC The Clarus MS system is controlled by a PC using TurboMass Software The application runs in a Microsoft Windows 7 Professional operating environment The software user interface contains color graphics and provides full user interaction with either the keyboard or the m...

Страница 56: ...nalyzer with a quadrupole prefilter assembly transmits only those ions having your selected mass to charge ratio The prefilter rod set improves sensitivity and protects the analytical quadrupole rods from contaminating ion deposits Ions emerging from the quadrupole mass analyzer are detected by the electron multiplier detector system ...

Страница 57: ... and view the prompting text and monitor instrument functions on a large full color touch screen display Figure 6 Clarus 680 GC The Programmed Pneumatic Control PPC Version of the Clarus 580 680 Series GC is used where the carrier gas and detector gases are monitored and controlled by the microprocessor thereby producing a fully automated system that is capable of managing all pneumatic functions ...

Страница 58: ...at the column end is flush with the inner wall of the EI or CI ion source The transfer line is temperature controlled by Clarus MS and has a 350 C upper limit If the Clarus GC detects improper operation for example no carrier gas and goes into an alarm condition it will turn off the temperature to the transfer line Figure 7 The transfer line Reference Gas Inlet The MS reference gas inlet system co...

Страница 59: ...s spectrometer is fitted with a quadrupole prefilter assembly that is designed to protect the main analyzer by intercepting the majority of any contamination As a consequence the main analyzer should never require cleaning On occasion it may be necessary to remove the prefilter rods for cleaning The need to clean these rods is usually indicated by poor peak shape or loss of resolution although oth...

Страница 60: ...e positioned beneath the instrument Care should be taken to avoid mechanically coupling vibrations from this pump to the mass spectrometer Operation and maintenance details about these pumps can be found in the manuals provided with the pump 0 l ll 0 Mass Spectrometer Connection Port Exhaust Port Oil Filler Plug Drain Plug Oil Level Indicator Gas Ballast Switch On Off Switch Mode Selection Switch ...

Страница 61: ...vèrement le MS de Clarus Instrument Power Rotary Pump Outlet 120 VAC 120 VAC 50 60 Hz MAX POWER 828 VA 230 VAC 230 VAC 50 60 Hz MAX POWER 690 VA Vacuum Pump Options The Clarus SQ 8 MS offers two different vacuum pump capacities Turbomolecular pumps are high speed turbines which transport the sample and carrier gas molecules away from the mass spectrometer Clarus SQ 8 S The 75 L sec turbomolecular ...

Страница 62: ...uum System 1 Cool the source and inlet to below 100 C 2 Select Vent Vacuum System Off from the Options menu on the Tune page and confirm that you want to vent the system Vacuum Gauge The single wide range vacuum gauge monitors the system pressure from atmosphere down to 10 9 Torr using a combined Pirani Inverted Magnetron ionization sensor Normal operating pressure with 1 mL min helium for the 255...

Страница 63: ...ng menu driven commands Printing file management and other routine procedures are performed using the appropriate Microsoft Windows modules Top Level Screen This screen contains the GC MS status sample list sequence queue and provides you with access to all other functions Tune Page The Tune Page allows you to tune the mass spectrometer control the gases set the GC interface temperature and monito...

Страница 64: ......

Страница 65: ... concentration range In general the larger the inside diameter of the column the larger the sample capacity However the larger the inside diameter the higher the flow necessary to achieve good performance 4 The next parameter is the phase or film thickness Film thickness will primarily affect the retentive character and the capacity of the column Increasing the film thickness will cause an increas...

Страница 66: ... prepared Is there a GC method Is the GC split vent open Is the proper mass spectrometer vacuum achieved Is the system leak free Is there a mass spectrometer method Are the autosampler wash vials filled with solvent Are you using the proper column flow or pressure Did you check the air water spectrum on the TurboMass Tune screen Is the injector hot and set to the proper temperature Is the transfer...

Страница 67: ...Maintenance 65 Maintenance 4 ...

Страница 68: ......

Страница 69: ...Maintenance 67 ...

Страница 70: ...omètre de masse Pour éviter tout risque de choc électrique ou de blessures causées par une tension élevée débranchez le cordon de ligne AC de la prise secteur et attendez au moins une minute avant d ouvrir ou de retirer un tableau de bord WARNING AVERTISSEMENT Disconnect AC power cord from outlet before removing any cover or parts Do not operate the instrument with any covers or parts removed Débr...

Страница 71: ...e instrument Always prepare a clear clean work area Make sure that any required tools or spare parts are close at hand Obtain small containers to store screws washers spacers etc Never touch any internal source parts with your bare fingers Use tweezers and pliers whenever possible If nylon or cotton gloves are used prevent leaving fibers in sensitive areas NEVER use rubber gloves Before reassembli...

Страница 72: ...ming these operations should be aware of the inherent risks and should take the necessary precautions Bon nombre des procédures décrites dans ce chapitre impliquent l élimination des dépôts de contamination potentiellement toxiques à l aide d agents inflammables ou caustiques Toute personne effectuant ces opérations devrait être consciente des risques inhérents et devrait prendre les précautions n...

Страница 73: ... may be cleaned with a soft cloth dampened with a mild detergent and water solution Do not use abrasive cleaners or solvents All tasks should be logged into a logbook to keep a record of any problems or trends Daily Make sure all system components are in working order Check and ensure that there are gas supplies to the GC and to the mass spectrometer Check the air water spectrum Perform leak check...

Страница 74: ...eference gas vial Refill if necessary Every Six Months Replace the forepump oil Check the analyzer prequadrupole Clean if necessary Yearly Check lens 1 lens 2 and analyzer prequadrupole Clean if dirty Check and clean the forepump inlet filter gas ballast control and the motor fan cover and enclosure ...

Страница 75: ...row or keypad buttons to set the split flow to 50mL For example if the capillary injector is in position 1 and you selected split flow in the PPC configuration software the following screen is displayed The total flow split vent septum purge column is displayed in the lower left of the screen The split vent flow setpoint is displayed in the setpoint box in the lower right 3 Start the TurboMass sof...

Страница 76: ... by clicking The TunePage dialog is displayed 5 Make sure the Tune parameters are similar to the values displayed NOTE The inlet and source temperatures should be less than 100 C only when venting the system 6 Click Press for Operate next to the red indicator box ...

Страница 77: ...4 x 10 5 Torr 8 Observe the displayed masses Mass 4 helium should be much larger than mass 18 water which should be larger than mass 28 nitrogen which should be about 4 times larger than mass 32 oxygen 9 If the nitrogen and oxygen are larger it indicates an air leak which could damage the filament Immediately click Press for Standby to turn off the filament 10 If a leak exists locate and fix it Ty...

Страница 78: ...ing one of the buttons on the bottom left of the Tune page The panel displayed in the top right center of the Tune page displays the tune peak information and instrument pressure information The tune peak display is located on the right side of the screen and allows you to view up to four masses The corresponding check boxes located above the peaks allow you to control each peak display Any one of...

Страница 79: ... window The indicator box turns green to indicate that it is on 3 Select UltraTune Custom AutoTune from the Options menu then click Start You will hear a click when the reference gas solenoid valve opens and AutoTune begins Upon completion the message AutoTune completed successfully is displayed 4 Click OK 5 Select Reference Gas On from the Gas menu to remove the check mark or click to set it in t...

Страница 80: ...e Your mass spectrometer is now Tuned To ensure proper operation check the mass calibration Preparing Clarus MS for Hardware Maintenance To prepare Clarus MS for hardware maintenance there are several steps that are common and precursory to all maintenance procedures They are as follows Turn off the Operate Mode 1 Display the Tune window 2 If the Press for Standby button is green indicating an ope...

Страница 81: ...le four et la ligne de transfert atteignent la température de consigne inférieure avant de les toucher Ne saisissez et maintenez la source que par sa poignée 1 On the left side of the Tune page enter 20 in the Inlet Line Temperature to cool the GC Interface transfer line CAUTION ATTENTION If the Clarus GC is off then the PPC control is off and no gas is flowing through the system Si le Clarus GC e...

Страница 82: ...ifold venting kit Part No N6470045 Évitez d évacuer l air autant que possible Ceci élimine l introduction d oxygène et de vapeur d eau dans le spectromètre de masse Le Clarus MS doit être ventilé avec de l azote UHP 99 9995 L hélium ne doit pas être utilisé Pour connecter correctement une source d azote sec à l ordre des instruments le kit d évacuation du collecteur N de pièce N6470045 Vent the Sy...

Страница 83: ...ng on the helium flow and or vent gas flow into the manifold 6 The system is now vented to atmosphere or optional dry gas Turn off the GC Carrier Gas Set all temperatures to ambient Once the GC column oven source and transfer line are cool you may then turn off the GC carrier gas ...

Страница 84: ...ter toujours des gants de nitrile de nylon ou de PVC sans pelu sans peluches sans poudre avant de toucher d enlever ou de remplacer les pièces Tenez la source uniquement par son manche Ne touchez jamais ces pièces avec des doigts non agglomérés car cela introduira des contaminants dans le système Removing the Source To remove the source follow this procedure 1 Prepare the mass spectrometer for mai...

Страница 85: ... fingers Risque de brûlures Ne touchez jamais une ligne de transfert de spectromètre de masse chauffée ou un capuchon d injecteur GC avec des doigts non protégé 4 Pull the inner transfer line tube back 25 mm 1 inch 1 4 inch Nut Column Inner Transfer Tube Pull Back Figure 9 Pulling back the inner transfer tube 5 Open the Clarus SQ 8 MS access door ...

Страница 86: ...arus SQ 8 MS Hardware Guide 84 6 Hold the source by the edge and rotate it counter clockwise Figure 10 Rotating the source 7 Carefully pull out the source Figure 11 Removing the source Access Door Source ...

Страница 87: ...Maintenance 85 8 Place the source on a clean surface Preferably place the handle end on a flat surface so that the source stands in an upright position Figure 12 The source placed in an upright position ...

Страница 88: ...on du spectromètre de masse porter toujours des gants de nitrile de nylon ou de PVC sans pelu sans peluches sans poudre avant de toucher d enlever ou de remplacer les pièces Tenez la source uniquement par son manche Ne touchez jamais ces pièces avec des doigts non agglomérés car cela introduira des contaminants dans le système 1 Carefully hold the source by its edges 2 Align the red dot on the sou...

Страница 89: ...Maintenance 87 4 Using a 9 16 inch wrench tighten the inch nut on the transfer line 5 Close the Clarus SQ 8 MS access door ...

Страница 90: ...e de transfert MS Ne touchez jamais ces pièces avec des doigts non agglomérés car cela introduira des contaminants dans le système Tools and Items Required NOTE Do not use a 100 Graphite ferrule to connect the column since it is a porous material that will allow air to diffuse into the MS system and prevent a high vacuum from being attained inside the system 9 16 inch wrench 1 4 inch wrench 5 mm w...

Страница 91: ...mbly is not pulled back first Avant de retirer la source de l instrument Clarus SQ 8 MS par exemple pour changer un filament ou nettoyer la source la colonne doit être retirée de son emplacement à l intérieur de la source Ceci est réalisé de manière pratique en desserrant le gros écrou sur l ensemble du tube de la ligne de transfert afin que l ensemble du tube de la ligne de transfert puisse être ...

Страница 92: ...nts de nitrile de nylon ou de PVC propres exempts de peluches et sans poudre lors de la manipulation de la partie de la colonne capillaire qui sera insérée dans la ligne de transfert MS Ne touchez jamais ces pièces avec des doigts non agglomérés car cela introduira des contaminants dans le système 1 Slide an injector septum over the outlet end of the capillary column to use it as a positioning ind...

Страница 93: ...remove surface contamination 6 Place the column onto a clean lint free surface on the bench top Measure exactly 34 4 cm from the outlet end of the column to the front side of the septum 7 Confirm that the Source is fully installed in the instrument If it is not install the source into the instrument See Removing and Returning the Source on page 82Error Bookmark not defined 8 Insert the column into...

Страница 94: ...e Figure 16 Figure 16 Measuring from the outlet of the column to the front of the septum 11 Using the 5 mm and 1 4 inch crescent wrenches tighten the column nut until the ferrule is crimped onto the column See Figure 17 Figure 17 Tightening the column nut metric 10 20 30 40 50 60 70 8 Slide the column back until the septum is 10 mm from nut 1 16 inch Column Nut Septum Column ...

Страница 95: ... la manipulation de la partie de la colonne capillaire qui sera insérée dans la ligne de transfert MS Ne touchez jamais ces pièces avec des doigts non agglomérés car cela introduira des contaminants dans le système NOTE The 10 mm positioning gauge tool is supplied with the instrument 1 Slide an injector septum over the outlet end of the capillary column to use it as a positioning indicator aid Sli...

Страница 96: ...olumn resulting in poor chromatography 10 With the column positioned as described in Step 9 slide the septum toward the column nut until it touches the nut 11 Pull the column back 10 mm Then use the 10 mm positioning tool Gauge to set the column nut at this position by placing the slot in the 10 mm Gauge over the column between the nut and the septum At this point be careful to avoid moving the se...

Страница 97: ...on du spectromètre de masse porter toujours des gants de nitrile de nylon ou de PVC propres exempts de peluches et sans poudre lors de la manipulation de la partie de la colonne capillaire qui sera insérée dans la ligne de transfert MS Ne touchez jamais ces pièces avec des doigts non agglomérés car cela introduira des contaminants dans le système 1 Loosen the large nut on the Transfer Line tube as...

Страница 98: ...Clarus SQ 8 MS Hardware Guide 96 Figure 19 Inserting the Plug Handle and Sight ...

Страница 99: ...ce of the column approximately 2 inches from the end and carefully break it off and discard the cut off piece of column 9 Use a lint free wipe pre soaked with a small amount of methanol to wipe the outside of the column a few times to remove surface contamination 10 Insert the column into the MS Transfer Line tube and carefully slide it toward the source Figure 20 Inserting the transfer line 11 Wi...

Страница 100: ...osition of the column is reached when it is aligned with the edge of the circle in other words at the 3 o clock position Figure 21 Viewing the Column through the Plug Handle and Sight 14 Using the 5 mm and 1 4 inch crescent wrenches tighten the column nut until the ferrule is crimped onto the column Be careful to avoid moving the column from the set position Confirm by gently tugging back the colu...

Страница 101: ...nstrument 17 Insert the source See Removing and Returning the Source on page Error Bookmark not defined 18 Re insert the Transfer Line tube assembly and tighten the large nut 19 The column is now installed and the MS is ready to be pumped down Confirm that the proper vacuum level is reached on the TurboMass software Tune Page 20 After initially heating the GC oven through one or two analysis cycle...

Страница 102: ...time you need to remove the mass spectrometer cover and vent the instrument Using a tool such as a dental mirror will help you observe the liquid level in the Reference Gas Vial Items Required Lint free powder free nitrile nylon or PVC gloves Pasteur Pipette or 50 µL syringe Heptacosa FC43 Part No N6212407 To refill the reference gas vial follow this procedure WARNING AVERTISSEMENT Make sure to ve...

Страница 103: ...brant is uncertain Take appropriate precautions to avoid getting the calibrant on your skin or in your eyes La toxicité de l étalonnage FC 43 est incertaine Prenez les précautions appropriées pour éviter d obtenir l étalon sur votre peau ou chez vos yeux 3 Loosen the knurled fitting by turn and pull out the vial A black O ring may remain in the fitting Knurled Fitting Reference Gas Vial ...

Страница 104: ...ting Make sure the O ring is still present and the tapered end of the ferrule faces the mass spectrometer 6 Tighten the knurled fitting with your fingers until fingertight 7 Replace the top cover and pump the system down to the proper vacuum 8 From the Gas Menu select the Reference Gas Option from the drop down menu Leave the Reference Gas Valve open for 60 minutes with Operate off to pump to pump...

Страница 105: ... peluche sans poudre et que vous essuyez chaque partie avec un Kimwipe humidifié au méthanol Items and Tools Required Filament assembly Part No E6470012 Methanol Lint free powder free nitrile nylon or PVC gloves Aluminum foil or lint free disposable cloth squares To replace a filament follow this procedure 1 Prepare a clean uncluttered work area and place a square of aluminum foil with the shiny s...

Страница 106: ...source so that the filament faces you then locate the filament retaining clip that holds it in place Figure 24 Moving the ceramic insulating connector assembly down Move the Ceramic Insulating Connector Assembly Down Filament Filament Retaining Clip ...

Страница 107: ...que le spectromètre de masse reste sans contamination assurez vous d utiliser des gants de nitrile de nylon ou de PVC sans peluches sans poudre et que tous les outils ont été nettoyés avec un chiffon de laboratoire humidifié 4 Using your thumb and forefinger push down the ceramic insulating connector assembly to release it from the filament leads trap lead and repeller lead 5 Press down on the ret...

Страница 108: ...7 Position the new filament assembly with the filament side up 8 Position the new filament assembly with the coiled filament wire facing and centered in the orifice in the ion volume and the white ceramic rests on the tab 9 Insert the Filament retaining clip into the slot in the block to hold it in place 10 Align the four male gold leads Trap Repeller and Filament with the four gold Filament ...

Страница 109: ...bly upwards to fully encapsulate the four gold leads You should be able to feel it click into position around the leads and close to the underside of the block 13 Install the source assembly back into the mass spectrometer by following the procedure Removing and Returning the Source on page 82Error Bookmark not defined ...

Страница 110: ...e masse reste exempt de contamination porter des gants de nitrile de nylon ou de PVC sans peluches sans poudre lors de cette procédure Disassembling Prepare a clean uncluttered work area and place a square of aluminum foil with the shiny side up Obtain some clean small containers for example small beakers to store the small parts as you remove them 1 Remove the source by following the Removing and...

Страница 111: ... can reassemble the source correctly There is only ONE way to replace the parts in the source The following illustrations should help you with the parts orientation and position Lorsque vous supprimez les pièces sources notez leur position et leur position dans la source afin de pouvoir rassembler correctement la source Il n y a qu une seule façon de remplacer les pièces dans la source Les illustr...

Страница 112: ...ving a residue 1 Mix together aluminum oxide and de ionized water and a few drops of methanol to make a watery paste 2 Dip a wooden stick cotton swab or a foam pad swab in the solution and clean the darkened areas on the source Work quickly to prevent the mixture from drying on the surface 3 Place the cleaned components in de ionized water prior to rinsing to prevent drying Rinsing 1 Add 50 mL of ...

Страница 113: ...and leaving a residue If you did not use acetone to rinse the parts wrap them in a clean lint free cloth and bake them in the GC oven at about 80 ºC for about fifteen minutes Reassembling 1 Replace the source parts into the source as shown below Remember to insert the parts into the source only as positioned below You may want to insert the trap insulator and trap before you insert the repeller Fi...

Страница 114: ... four male gold leads Trap Repeller and Filament with the four gold female connectors in the ceramic insulating connector assembly 6 Carefully move the connector assembly upwards to fully encapsulate the four gold leads You should be able to feel it click into position around the leads and close to the underside of the block 7 Install the source assembly back into the mass spectrometer by followin...

Страница 115: ... spectrometer is fitted with prequads that act as a prefilter assembly designed to protect the analytical quads by intercepting the majority of any contamination As a consequence the analytical quads should never under normal working conditions require cleaning Occasionally it may be necessary to remove the prefilter rods for cleaning The need to clean these rods is usually indicated by poor peak ...

Страница 116: ...ves to remove dirt from metal components Recommended abrasives are 6000 Grade Micro Mesh Part No N9303420 8000 Grade Micro Mesh Part No N9303421 600 grit aluminum oxide in DI Water with a few drops of methanol to make a paste After cleaning with abrasives it is necessary to wash all metal components in suitable solvents to remove all traces of grease oil and if micro mesh is used rubber The recomm...

Страница 117: ...ans le système WARNING AVERTISSEMENT Make sure to vent the instrument and turn the power off and unplug the mass spectrometer from the AC power source The mass spectrometer contains high voltage To prevent the risk of shock unplug the line cord from the AC outlet and wait at least one minute before opening or removing any instrument cover or panel Assurez vous d énerver l instrument et de mettre l...

Страница 118: ...rning the Source on page 82Error Bookmark not defined 3 Use the medium sized Philips screwdriver to remove the two screws on the left access panel See the following figure Figure 30 Removing the cover screws 4 Remove the left access panel and place in a secure location Screws ...

Страница 119: ...side of the cover off the metal tabs on the instrument See the following figure Figure 31 Removing the top cover 6 Place the top cover in a safe location 7 Loosen the two screws holding the plastic extensions in the front cover in place Top Cover Top Cover Slot 2 Metal Tab on Chassis 2 ...

Страница 120: ...ing the lid It is not necessary to remove the front cover completely from the instrument 9 Use a 5 mm Allen key to loosen the four hex screws that hold the optics assembly in place See the following figure Figure 32 Removing the screws on the lid and the front cover Screw Screw Screws Holding the Front Cover ...

Страница 121: ...at the rear of the optics assembly 11 Locate the Sliding Lock attachment on the RF Generator Cable connector then press down on the Sliding Lock attachment to release the lock on the connector See the following figures Cables RF Generator Connector Sliding Lock attachment RF Generator Connector Sliding Lock attachment ...

Страница 122: ...tor See the following figure Figure 35 Removing the RF Generator cable NOTE The metal tube attached to the reference gas vacuum hose has a ferrule on it that may slip off when the nut is removed from the reference gas valve fitting Be careful to avoid dropping the ferrule inside the instrument Press Down to Release the Lock ...

Страница 123: ... reference gas vacuum hose See the following figure Figure 36 Disconnecting the cables at the front of the optics assembly 14 Hold the ion optics assembly by its handles lift it up and place it on a clean surface 15 Cover the vacuum manifold with aluminum foil Reference Gas Valve Cable Connector Fan Cable Source Connector Nut and Ferrule for Reference Gas Vacuum Hose ...

Страница 124: ...uches sans poudre avant de toucher d enlever ou de remplacer les pièces Ne touchez jamais ces pièces avec des doigts non agglomérés car cela introduira des contaminants dans le système 1 Remove the aluminum foil covering the vacuum manifold 2 Ensure that the large O ring around the ion optics assembly tub is properly set into place 3 Hold the ion optics assembly by its handles and align the guide ...

Страница 125: ...or to connecting it to the receptacle on the RF Generator box as shown in the following figure Figure 37 RF Generator cable connector 7 Connect the RF Generator Cable connector to the receptacle on the RF Generator box See the following figure Figure 38 Reconnecting the RF Generator cable connector to the receptacle RF Generator Box ...

Страница 126: ...he four hex screws previously removed NOTE Do not tighten these hex head screws beyond finger tight The vacuum will pull the ion optics assembly top plate onto the large o ring to create the seal Over tightening these screws may cause the ion optics assembly top plate to warp which may cause a leak 11 Secure the top cover by securing the slots in the cover to the tabs on the instrument 12 Use the ...

Страница 127: ...ectron multiplier 1 Remove the ion optics assembly See Removing and Returning the Ion Optics Assembly on page 114Error Bookmark not defined 2 Release the electron multiplier by pressing the retainer clip then pull the electron multiplier from the assembly See the following figure Figure 40 Removing the electron multiplier Quadrupole Assembly Electron Multiplier Electron Multiplier Pulled from the ...

Страница 128: ...loved bare fingers as this will introduce contaminants into the system Pour éviter toute contamination du spectromètre de masse porter toujours des gants de nitrile de nylon ou de PVC sans pelu sans peluches sans poudre avant de toucher d enlever ou de remplacer les pièces Ne touchez jamais ces pièces avec des doigts non agglomérés car cela introduira des contaminants dans le système 1 When operat...

Страница 129: ...de clean the ion burns off the prefilters 3 Wipe the prequads with a methanol dampened laboratory wipe 4 Blow dry with helium or dry nitrogen 5 Return the ion optics assembly to the vacuum manifold See Removing and Returning the Ion Optics Assembly on page 114 ...

Страница 130: ...e pump Maintanenace of the Turbomolecular Pump You should never service the turbomolecular pump Call your PerkinElmer Service Representative for the maintenance and any problems you may have with the pump Checking the Forepump Oil Level 1 Locate the oil level indicator window on the forepump 0 l ll 0 Mass Spectrometer Connection Port Exhaust Port Oil Filler Plug Drain Plug Oil Level Indicator Gas ...

Страница 131: ... Unscrew and remove one of the filler plugs on the top of the pump 2 Locate the bottle of pump oil supplied with the pump and add oil until it reaches the MAX mark on the top of the oil level indicator Do not overfill 3 Replace the oil filler plug by tightening it until it is fingertight Do not overtighten the oil filler plug 4 After restarting the pump and allowing it to run for a few minutes rec...

Страница 132: ...il by running the pump for at least 10 minutes and then switch off the vacuum system 2 Unplug the pump from the AC outlet and disconnect it from your vacuum system 3 Remove one of the oil filler plugs Figure 43 Draining forepump oil Filler Plug Drain Plug 2 Liter Drain Container Max Oil Level Min Oil Level ...

Страница 133: ...e the drain plug and allow the oil to drain into the container If the pump oil was contaminated pour clean oil into the filler hole and allow it to drain until the oil appears clear 6 Replace the drain plug remove the block and reconnect the vacuum system 7 Add oil until it reaches the MAX mark on the top of the oil level indicator Do not overfill 8 Replace the oil filler plug by tightening it unt...

Страница 134: ...ck on connectors are installed into the gas line here is no need to loosen or tighten any fittings the new trap will just click in Replacement Traps Description Part No Indicating Glass Triple Gas specific He Oxygen Moisture Hydrocarbons N09306107 Indicating Glass Triple Gas specific He Oxygen Moisture Hydrocarbons with 1 8 Brass Connector 2 N09306114 Indicating Glass Triple Gas specific He Oxygen...

Страница 135: ...pors When using ammonia gas when running in the chemical ionization CI mode it is necessary to vent the mass spectrometer effluent from the forepump exhaust into a fume hood or charcoal trap Vapeurs de gaz dangereux Lors de l utilisation d ammoniac gazeux lors de l utilisation du mode ionisation chimique CI il est nécessaire d évacuer l effluent du spectromètre de masse à partir de l échappement d...

Страница 136: ...diffuser dans le four en créant la possibilité d une explosion Si le spectromètre de masse n est pas sous vide l hydrogène le méthane ou l iso butane peuvent remplir la chambre à vide en créant ainsi un risque explosif Pour éviter d éventuelles blessures ne pas allumer l hydrogène le méthane ou l iso butène sauf si une colonne est fixée tous les joints ont été éprouvés et le spectromètre de masse ...

Страница 137: ...or on the rear of the mass spectrometer 3 Ensure that the mass spectrometer is at the proper vacuum level 4 Turn on the CI gas and set the delivery pressure to 15 psi 104 kPa WARNING AVERTISSEMENT If ammonia is used for chemical ionization all fittings and tubing must be stainless steel to avoid corrosion Also the forepump must be vented to a fume hood or trap Si l ammoniac est utilisé pour l ioni...

Страница 138: ...nd Returning the Source on page 82 2 Install the CI source by following the procedure Removing and Returning the Source on page 82 Properly cover and protect the EI source and put it in a safe place 3 Select CI from the Ion Mode menu The CI window appears Rotary Pump Power Power In Vacuum Line ROTARY PUMP POWER IN Warning Labels Warning WATER IN WATER OUT N VENT 2 NH C C H CI GAS 3 4 4 10 H 15 psi...

Страница 139: ...uge time line Wait about 5 minutes until the vacuum gauge achieves about 2 5 x 10 5 Leak Checking Before running in the CI mode confirm that the column is properly installed and the system is leak free The best way to check this is by running CI without the reagent gas To leak check a system 1 Display the Tune page 2 Select CI from the Ion Mode menu 3 Click Press for Operate and observe the air wa...

Страница 140: ...reagent gas to produce an EI emission similar to the EI mode but with reduced sensitivity You will leak check your system this way If mass 28 is larger than mass 18 you have a leak Determine the source of the leak and correct it For example leak check all fittings and connections ...

Страница 141: ... Setting Up CI After verifying that no leaks exist you can proceed to set up the CI mode for an analysis Setting the Parameter Values 1 Display the following CI window 2 Set the values as shown in the following table ...

Страница 142: ... z 35 should be optimized If using isobutane reagent gas the reagent ions at m z 43 C3H7 and 57 C4H9 should be tuned in the approximate ratio of 1 2 The following example uses methane reagent gas NOTE The CI reagent gas adjustment knob controls a delicate needle valve To avoid damaging the needle valve do not overtighten it Always use the CI gas button on the screen to turn off the CI gas Paramete...

Страница 143: ...ark appears next to the option NOTE Always turn on the CI gas before Operate to avoid a pressure surge hitting the filament 3 Click Press for Operate and monitor the Penning gauge as you adjust the CI gas Observe that mass 16 initially grows larger As pressure increases in the ion chamber of CI source the mass 29 peak will begin to grow Keep the pressure below 5 e 4 Torr CI Reagent Gas Adjustment ...

Страница 144: ... 5 Continue to turn the knob counterclockwise Observe that the pressure increases and mass 41 will start to grow Stop when mass 29 is at 100 6 Turn the knob to maximize the intensity of mass 29 Also verify that mass 16 is small 1 0 of the height of the peak at mass 17 If mass 16 does not appear as a small peak STOP You probably have a gas leak at the transfer line inner source connection Locate an...

Страница 145: ...s before clicking Press for Operate Parameter CI value and comments Electron Energy 30 to 70 eV This parameter should be optimized Emission 200 to 300 µA is acceptable Emission measures the real emission current i e the source current from the source block there is no separate measurement of source current in CI Lens 1 and 2 The tuning of these lenses may be different from the optimum values set f...

Страница 146: ...2 and 633 which usually produce relative intensities of 65 85 and 95 respectively Heptacosa can be used to calibrate the m z range for negative ion CI analyses 3 Maximize the peak intensities then slightly decrease the reagent gas by turning the knob clockwise 1 8 turn Optimize the tuning parameters for maximum intensity 4 Save the Tune page parameters by selecting Save As from the File menu 5 Sel...

Страница 147: ...t selected Assurez vous que la case à cocher Utiliser Air Refs n est pas sélectionnée 7 Click the Start button to display the following dialog box 8 Click Acquisition Parameters and enter the following values 9 Click OK to begin calibration You are now ready to run CI analysis ...

Страница 148: ...Troubleshooting 5 ...

Страница 149: ...Troubleshooting 147 ...

Страница 150: ...The more a column is used the greater the possibility of contamination loss of substrate etc Columns do not last forever and should be changed when results become suspect The gas flow system Gas leaks are a major concern in gas chromatography and can lead to many problems The vacuum system Vacuum leaks are a major concern in mass spectrometry and can lead to many problems Ion Optics Over time the ...

Страница 151: ...th age and can begin to leak You should have a thermal conductivity leak detector to help find and fix leaks Injector liners are made of glass or fused silica and can be easily broken when removed You should keep a supply of spare liners on hand Please remember that you cannot run satisfactory analyses without an injector liner Logical Troubleshooting Steps There are some simple steps that you sho...

Страница 152: ...m instead of replumbing the internal pneumatics Change only one parameter at a time and check for its effect If you change three items at once and your problem goes away you may not know which of the three moves or combination of moves corrected the problem This way if the problem happens again you will know exactly what corrective action to take ...

Страница 153: ...AC power to the outlet Check the outlet Fuse blown Call a PerkinElmer service engineer Mass Spectrometer is on but the forepump is not running Forepump is not plugged into the AC outlet on the rear of the mass spectrometer Plug the forepump line cord into the mass spectrometer Forepump is not operating correctly mass spectrometer does not pump down Make sure the forepump is switched on Blown fuse ...

Страница 154: ...ontact your PerkinElmer service representatives Is the backing pressure high Check for a leak in the backing pipeline and poor backing pump performance Correct as necessary The pump is very noisy or there is excessive vibration or both Is the noise irregular and getting progressively worse If so a bearing may be defective Contact your PerkinElmer service representative Is the pump making a constan...

Страница 155: ...or your site Vacuum light continues to blink Large leak Locate vacuum leak and correct Foreline trap has excessive moisture Replace filter Rotary pump set to gas ballast Switch the gas ballasting off Rotary pump requires oil change Change oil High mass spectra appears as a large blotch or loss of high mass spectra Bad tune Run AutoTune Drastic change in mass peak shape for no apparent reason Bad t...

Страница 156: ...oard Call a PerkinElmer service engineer Multiplier near the end of its lifetime Replace the multiplier No filament current Defective filament Replace the filament Wavering baseline by several hundred counts Defective outer source temperature sensor or a defective electrometer Replace the temperature sensor Call a PerkinElmer service engineer Increasingly setting higher multiplier voltage settings...

Страница 157: ...ector Peak splitting Prevent double injections Dry the outside of the injector needle Replace the injector septum Injector and column are more active toward acid base compounds Install a silanized injector liner or silanize the current injector liner Check or replace the injector packing material such as quartz wool Cut off the first 30 cm of the column and rerun the test mix If the results do not...

Страница 158: ...erature to allow the less volatile compounds of the sample to reach the mass spectrometer Peaks at masses 28 nitrogen and 32 AMU oxygen are in a ratio of 4 to 1 and the peak at mass 28 is larger than the peak at mass 18 Leaks in or around vacuum or column fittings Tighten the fittings and connection points to the high vacuum system Set the injector split flow to 50 1 Peaks at masses 14 and 16 are ...

Страница 159: ...e the inner source clean or replace lenses in the outer source and install a new filament Loss of resolution especially at high mass Dirty prequadrupole rods Clean the prequadrupole rods Mass assignment drifts Large temperature fluctuations in the laboratory Stabilize the lab temperature or isolate the GC MS system from large temperature fluctuations Mass assignment incorrect Run mass calibration ...

Страница 160: ... Dirty prefilter Clean prefilters Dirty source Clean source Particulates on analyzer rods Clean the particulates of the rods with a methanol dampened lab wipe Blow the particulates off the rods with helium or dry nitrogen Defective or damaged analyzer Call a PerkinElmer service engineer No reference peak Reference gas off Turn on the reference gas Empty reference vial Visually check and refill Fau...

Страница 161: ...er resolved tuning Retune Big peaks observed at m z 18 28 32 Air leak developed Check column connections Change carrier gas tank Fit oxygen scrubber Moisture from recent source clean column change Bake out source overnight No ion beam but the filament status OK Large air leak See procedure for leak checking Detector voltage too low Increase multiplier value Electronics failure Call a PerkinElmer s...

Страница 162: ...rkinElmer service engineer Total Ion Chromatogram too high Dirty source Clean the source Contamination from poor handling technique Set source and transfer line to 250 ºC and maintain this temperature overnight Stationary phase of column de polymerizing bleeding Change column Air leak Find the leak and fix it Poor quality carrier gas Replace the carrier gas tank Carrier gas filter is ineffective a...

Страница 163: ...uning and recalibrating Poor AutoTune Manual tune Retune Contaminated ion source Clean the ion source Set the source temperature to 250 ºC and maintain this temperature overnight Source too hot cool Set the correct source temperature Air leak Find the leak and fix it Wrong calibration reference file selected Select the correct file Incorrect calibration calculation parameters Set the calibration p...

Страница 164: ...r and condition the column Vacuum leak Locate and fix the leak Discreet high intensity contaminant peaks Column bleed Disconnect the column from the mass spectrometer and condition the column Injector septum bleed Replace the septum and or glass liner Tailing peaks sloping on RHS Improperly installed column Check the column and reinstall if necessary Injector too cool Raise the injector temperatur...

Страница 165: ...ram Enter a new oven program Discrimination of relative peak intensities Poor resolution or improper tuning Retune Unstable filament Replace filament Poor calibration Recalibrate Air leaks at detector Check He Air ratio Peaks are flat topped Signal strength exceeds dynamic range of detector Reduce multiplier voltage Sample is too strong Dilute or split High baseline Dirty sample Prepare and filter...

Страница 166: ... off for too long Reduce purge time Low sensitivity Dirty source Clean the source Poor column performance Replace column Dirty injector Replace injector liner Source temperature not optimized Set the proper source temperature Detector voltage set too low Increase multiplier voltage Tune not set correctly Run AutoTune Poor filament alignment Realign or replace filament Incorrect column position in ...

Страница 167: ...r tuning Retune Poor calibration Recalibrate Air leak Locate and fix Active sites in column liner Replace column liner Intermittent source heater failure Call a PerkinElmer service engineer Poor S N on test standards See low sensitivity causes above Incorrect GC MS method Use the correct method Accidental split injection Set the proper split Detector voltage set too low Increase multiplier voltage...

Страница 168: ...um distortion Scanning too fast or slow Reset the scan rate Incorrect Isotope ratios Poor calibration Recalibrate Incorrect tune Retune Defective filament Replace filament Air leak Find and fix Missing Isotopes in spectrum Bad calibration Recalibrate Poor tuning Retune Dirty source Clean source Sample too weak Use a higher sample concentration Peak detection thresholds set too high Lower the thres...

Страница 169: ... chromatography Incorrect column alignment Reinstall the column Section of a mass range missing from a spectrum Corruption of data file Reacquire data Scanning too fast Reduce the rate Hard disk has too much fragmentation Defrag the hard drive Hard disk full Remove unnecessary files Molecular Ion too weak Source temperature too high Reduce the source temperature ...

Страница 170: ... Will not control GC RS 232 communications cable loose connections Check and restart the mass spectrometer Power failure transient surge to GC or autosampler GC electronic malfunction Call a PerkinElmer service engineer Communication cable intermittent contact GC electronics malfunction Call a PerkinElmer service engineer Crashes when starting an acquisition Software corrupted Reload software Rota...

Страница 171: ...unblock Pump has failed to reach vacuum Pressure measurement or gauge head gives an incorrect indication of pressure A contaminated Pirani gauge can indicate a pressure several times higher than the actual Replace if necessary Pump contains the wrong type of oil Drain and refill with the correct oil Edwards Ultragrade 19 Oil Consult your Edwards Pump instruction manual Mode selector and or gas bal...

Страница 172: ...um fitting dirty or damaged Check and replace if necessary Noisy Pump Motor fan cover damaged Call a PerkinElmer service engineer Worn motor bearings Call a PerkinElmer service engineer Oil contaminated with solid particles Determine cause and replace oil Oil saturated from CI analysis Drain and refill with clean oil ...

Страница 173: ...erkinElmer service engineer Oil box gaskets deteriorated Call a PerkinElmer service engineer Oil leak from gas ballast control Call a PerkinElmer service engineer Oil leak from drain plug Tighten the drain plug or replace Oil leak from sight glass Tighten sight glass screws or call a PerkinElmer service engineer ...

Страница 174: ...con to get more details on the message Message Title Icon Message Action System not at pressure Caution The system has not reached the proper operating pressure The filament could be damaged by starting the system now Do you wish to continue Press Yes if you wish to continue Press No if you wish to stop See the Maintenance chapter in this Hardware Guide for the procedure to replace a filament Safe...

Страница 175: ...our PerkinElmer service representatives Vacuum Gauge Failure There is a problem with the vacuum gauge Press OK to close the message Restart the system if you still have this failure message contact your PerkinElmer service representatives Pump failure Safe to Vent The vacuum system is off and the system can now be vented The carrier gas should be turned off There is a problem with the turbo pump P...

Страница 176: ... the system can now be vented The carrier gas should be turned off There is a problem with the vacuum gauge Please look in the Hardware Guide for additional instruction Press OK to close the message To replace the vacuum gauge contact your PerkinElmer service representatives Exit TurboMass Vacuum System pumping down The vacuum system is in the process of the pumping down the spectrometer Exiting T...

Страница 177: ...urn off the backing pump If the transfer line or the source temperatures are above 100C please wait until they have cooled before pressing OK Pressing the OK button will turn off the backing pump Problem with Vacuum The backing pump could not reach the necessary vacuum level to start the turbo pump There could be a problem with a vacuum leak the backing pump or the vacuum gauge The backing pump wi...

Страница 178: ...TurboMass Software Installation 176 ...

Страница 179: ...Index ...

Страница 180: ......

Страница 181: ...ing 109 disassembling 107 reassembling 110 rinsing 109 EI to CI mode changing 132 Electricity safety practices 23 ElectroMagnetic Compatibility 13 F Filament replacing 102 G Gases 40 H Hardware maintenance 78 I Inline Gas Purifiers 131 Introduction to TurboMass 53 Ion source 57 L Labels WEEE Instructions 36 Leak checking 73 CI 136 M Maintenance 69 leak checking 73 mass analyzer 112 overview 69 pre...

Страница 182: ...ctricity 23 pollution degree 34 ventilation 27 Software 61 top level screen 61 Tune page 61 Source removing 82 Spare components 148 T Transfer line cooling 79 Traps click on connectors 131 replacement 131 Troubleshooting 147 chart 150 overview 147 spare components 148 Tune page 61 Tuning 76 TurboMass Software 61 Turbomolcular Pump venting 60 V Vacuum Gauge 60 Vacuum system 58 options 59 rotary pum...

Страница 183: ......

Страница 184: ...PerkinElmer 710 Bridgeport Avenue CT 06484 4794 U S A Shelton Internet http www perkinelmer com email info perkinelmer com PerkinElmer is a registered trademark of PerkinElmer Inc ...

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