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Troubleshooting
HPLC System Troubleshooting _____________________________________________________________

HPLC System Troubleshooting

This is a general guide to HPLC system troubleshooting. For system-
specific problems, consult the manufacturer’s manual. This section gives
advice on appropriate LC conditions and rectifying LC system problems.

Buffers and Additives

In many cases, buffers and/or other additives are necessary in the mobile
phase to modify chromatography. The concentration of buffer/additive
added is critical, as the MS performance can be affected. An example of this
is the addition of acid in negative ion mode. This will suppress ionization of
weakly acidic compounds. Refer to the chapter

LC/MS and the Cone

Wash

for information on specific solvents and additives.

Mobile Phase Reservoir

The mobile phase reservoir should be an inert container, usually glass, fitted
with a vented cap to keep particulate matter from entering. The white frit
serves as a gross filter only; always use a 0.45 µm filter in-line to prevent
solid particles from entering the MS detector.

Bubble Problems and Degassing

Bubble problems in LC systems result from mixing air-saturated solvents.
Air is generally less soluble in solvent mixtures than in pure solvents, and
the excess gas leaves the solution as bubbles. Bubbles in the LC system can
cause instability in UV and other detectors, and in API sources.
Thorough degassing can minimize bubble problems in the mobile phase.
Heating is the most efficient way of removing gas from reversed-phase
solvents, but this is inconvenient. The most common way of degassing
solvents is using a vacuum membrane degasser. Many LC systems have this
feature. Another efficient way to degas solvents is by helium sparging. Use
a flow of ~ 300 mL/min for 3 to 4 minutes and then reduce the flow to a
trickle (most LC systems allow constant helium sparging). One liter of
helium can degas one liter of solvent with ~99% efficiency. To minimize
evaporation of mobile phase and potential change in composition, only
sparge for a few minutes at high flow. Degassing in an ultrasonic bath is a
poor technique for removal of gas from solvents. Normal-phase solvents do
not need to be degassed.

6-4

___________________________ MSQ Hardware Manual ____________________________

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Содержание MSQ

Страница 1: ...Document No 031871 Revision 02 October 2003 Hardware MSQ...

Страница 2: ...HE USE OR THE RESULTS OF THE USE OF THIS PUBLICATION IN TERMS OF CORRECTNESS ACCURACY RELIABILITY CURRENTNESS OR OTHERWISE FURTHER DIONEX CORPORATION RESERVES THE RIGHT TO REVISE THIS PUBLICATION AND...

Страница 3: ...gmentation 1 16 Cone Voltage Ramping 1 18 Polarity Switching 1 19 Application of API Techniques 1 20 The Self Cleaning Source Cone Wash 1 23 Introduction 1 23 Functional Description 1 24 The Reference...

Страница 4: ...Introducing the MSQ Introduction ____________________________________________________________________________ 1 ii____________________________ MSQ Hardware Manual ____________________________...

Страница 5: ...ve detection using conventional to capillary LC flow rates on bench top MS detector systems LC MS works with typical solvent compositions whether the separation is achieved by isocratic or gradient el...

Страница 6: ...I ionization occurs in the gas phase In both cases efficient desolvation is needed to remove the solvents from the sample Ions now in the gas phase are passed through the mass analyzer and are collect...

Страница 7: ...re quadrupole RF lens Rotary pump Split flow turbomolecular pump Entrance cone From HPLC Orthogonal sample introduction probe Cone wash Exit cone Figure 1 2 Schematic diagram of the MSQ API inlet anal...

Страница 8: ...e atom of carbon 12 This follows the accepted convention that an atom of carbon 12 has exactly 12 atomic mass units amu The MS detector does not directly measure molecular mass but the mass to charge...

Страница 9: ...hts the exterior features of the MSQ The parts labeled here may be referred to in later chapters of this manual or other manuals supplied with the MSQ Status light Figure 1 3 Front view of the MSQ Fig...

Страница 10: ...When the instrument is functioning normally the status light will go from flashing yellow to solid yellow and Operate can be switched On If the pressure in the instrument rises above the operating pr...

Страница 11: ...OURCE EXHAUST BACKING PUMP RELAY USB USER I O RESET MAINS ON OFF MAINS IN GAS IN 6 BAR MAX To rotary pump To rotary pump Exhaust from API source Rotary pump power To PC Contact closure and analog inpu...

Страница 12: ...direct any involatile components present in the LC eluent such as those from buffers ion pairing agents or matrices away from the entrance orifice Under operating conditions however both the sample i...

Страница 13: ...roviding a sensitive means of analyzing a wide range of polar molecules Since the first combined ESI LC MS results were announced in 1984 and its first application to protein analysis four years later...

Страница 14: ...pumped through a stainless steel insert capillary that carries a high potential typically 3 to 5 kV see Figure 1 9 The strong electric field generated by this potential causes the solvent to be spraye...

Страница 15: ...n process close to the entrance cone enables the routine use of high LC flow rates up to 2 0 mL min in ESI mode The newly formed ions then enter the focusing region through the entrance cone This is d...

Страница 16: ...or instead of the quasi molecular ion Common adducts are ammonium ions NH4 M 18 sodium ions Na M 23 and potassium ions K M 39 60 80 100 120 140 160 180 200 220 240 260 280 300 320 340 360 m z 0 100 3...

Страница 17: ...ed region The combination of nebulizing gas and heat form an aerosol that evaporates quickly to yield desolvated neutral molecules see Figure 1 12 At the end of the probe is a corona pin held at a hig...

Страница 18: ...ted between the heated region and the entrance cone ionizes the sample molecules with a discharge voltage of approximately 3 0 to 3 5 kV in positive ion mode and 2 0 to 3 0 kV in negative ion mode Atm...

Страница 19: ...roduce multiply charged ions and so is unsuitable for the analysis of high molecular weight compounds such as proteins or peptides Although a high temperature is applied to the probe most of the heat...

Страница 20: ...data at source voltages of 20 40 and 60 V on an alternating scan basis within a single acquisition The benefits of setting up acquisitions in this way are The optimum source voltage for a particular...

Страница 21: ...Bu Protonated molecule at m z 240 Fragment ion at m z 222 Fragment ion at m z 166 Figure 1 14 Source fragmentation of salbutamol in electrospray ionization Optimum Response for Confirmatory Ions When...

Страница 22: ...ure 1 15 Electrospray spectrum of horse heart myoglobin This envelope is represented in diagrammatic form in Figure 1 16 The first diagram shows the envelope at a source voltage of 30 V Next the envel...

Страница 23: ...o the same m z value each time Polarity Switching Switching between positive and negative ionization modes in a single analytical run is supported by the MSQ Rapid polarity switching is a technique th...

Страница 24: ...210 220 230 240 m z 0 100 214 156 173 231 m z 130 140 150 160 170 180 190 200 210 220 230 240 0 100 231 Figure 1 17 Thermal fragmentation of the herbicide asulam in APCI APCI does not yield multiply c...

Страница 25: ...there are many applications common to both Compounds suitable for analysis by electrospray are polar and of molecular weight less than 100 000 amu The higher molecular weight compounds such as protein...

Страница 26: ...and steroids Sensitivity fg to pg compound dependent fg to pg compound dependent Type of spectra M H for ve ion mode M H for ve ion mode fragmentation via source voltage M H for ve ion mode M H for v...

Страница 27: ...ons and the charged liquid droplets containing involatile components are deflected by the electric field towards the inlet orifice This effect leads to a gradual buildup of involatile components and a...

Страница 28: ...ary is attached to PEEK tubing internal to the instrument which when connected to an LC pump delivers the solvent typically HPLC grade water or organic solvents such as methanol at a controlled flow r...

Страница 29: ...e the reference inlet system Functional Description As shown in Figure 1 20 the reference inlet system consists of a pressurized reservoir containing the reference sample and a PEEK delivery tube One...

Страница 30: ...owed to pass through at any one time The ions then reach the detector whose main component is a channeltron electron multiplier In positive ion mode the ions exit the analyzer and strike a conversion...

Страница 31: ...avel as ions through the mass analyzer It is important to remember that an MS detector must be under high vacuum in order to operate In the case of the MSQ system not all of the MS detector is under h...

Страница 32: ...soft Windows platform Software Xcalibur software controls the MSQ MS detector When Xcalibur is run the Home page is displayed see Figure 1 22 Xcalibur also runs the MSQ server see Figure 1 23 The Home...

Страница 33: ...matograms and spectra in order to obtain more information about the compounds in the sample Quan Browser Use Quan Browser to examine acquired data in order to obtain an accurate determination of the a...

Страница 34: ...lowed and an error message will be displayed Raw Data Xcalibur acquires data in a raw file Raw data can be viewed as chromatograms and mass spectra see Figure 1 25 The term mass spectrum refers to a p...

Страница 35: ...00 450 500 m z 0 20 40 60 80 100 Relative Abundance 281 2 459 1 240 3 282 5 454 1 461 0 256 2 229 4 346 8 403 2 181 5 387 0 482 1 Figure 1 25 A mass spectrum taken at retention time 2 66 minutes lower...

Страница 36: ...ibur automatically determines and saves the mass center of the acquired profile peak returned from the detector Hence the previously large number of points that described the mass spectral peak are re...

Страница 37: ...d ions can be seen and measured if necessary This is most useful in the case of protein and peptide analysis where multiply charged ions are formed As data is being written to disk at all times even w...

Страница 38: ...noise A further advantage of MCA is that data is written to disk only at the end of an experiment therefore significantly less storage space is required MCA cannot be used for time resolved data becau...

Страница 39: ...ically greater than a factor of ten than full scan techniques However this sensitivity does depend on the number of masses being monitored simultaneously SIM is also a highly selective technique Impur...

Страница 40: ...Introducing the MSQ The Data System ________________________________________________________________________ 1 36 __________________________ MSQ Hardware Manual ____________________________...

Страница 41: ...ging Ionization Modes 2 Changing Ionization Modes 2 i Introduction 2 1 Switching from ESI to APCI 2 2 Switching from APCI to ESI 2 4 ____________________________MSQ Hardware Manual ___________________...

Страница 42: ...Changing Ionization Modes Introduction ____________________________________________________________________________ 2 ii____________________________ MSQ Hardware Manual ____________________________...

Страница 43: ...ion Introduction Use the information in this chapter in conjunction with the animations on the MSQ CD shipped with your system The chapter is divided into the following sections Switching from ESI to...

Страница 44: ...the locking plate clockwise to the open position and remove the ESI probe assembly P N FM102595 Locking plate PEEK fitting Figure 2 5 ESI probe assembly Swap the ESI probe assembly P N FM102595 with t...

Страница 45: ..._______________Switching from ESI to APCI Figure 2 6 APCI corona pin and APCI blank plug 6 Insert the PEEK finger tight fitting into the APCI probe assembly P N FM102587 and screw it into place ______...

Страница 46: ...heater assembly to cool before changing ionization modes 1 2 Unscrew and remove the PEEK finger tight fitting from the APCI probe assembly P N FM102587 Change the APCI blank plug P N FM101437 with th...

Страница 47: ...obe assembly P N FM102595 located in the holder in the door Turn the locking plate on the ESI probe assembly clockwise into the open position insert the ESI probe assembly P N FM102595 and turn the lo...

Страница 48: ...Changing Ionization Modes Switching from APCI to ESI ________________________________________________________________ 2 6 ___________________________ MSQ Hardware Manual ____________________________...

Страница 49: ...he Cone Wash 3 i Introduction 3 1 LC MS Considerations 3 2 Flow Rates 3 2 HPLC Solvents and Mobile Phase Additives 3 3 Setting Up the Cone Wash 3 7 Flow Splitting 3 9 ___________________________MSQ Ha...

Страница 50: ...LC MS and the Cone Wash Introduction ____________________________________________________________________________ 3 ii____________________________ MSQ Hardware Manual ____________________________...

Страница 51: ...ling region caused by the deposition of involatile phosphate salts The self cleaning API source allows routine LC MS with chromatographic buffers such as phosphates or ion pairing agents and samples i...

Страница 52: ...he guidelines in Table 3 1 apply Table 3 1 LC columns and flow rates Column ID Flow Rate 4 6 mm 1 0 mL min 3 9 mm 0 5 mL min 2 1 mm 0 2 mL min 1 0 mm 40 50 L min Capillary 10 L min The different ioniz...

Страница 53: ...are Water Acetonitrile Methanol These common reverse phase LC solvents are ideal for LC MS When using high percentages of water the probe temperature usually needs to be raised to aid desolvation in t...

Страница 54: ...electrospray ionization Least Suitable Additives Least suitable additives are surface active agents detergents These can suppress the ionization of other compounds Detergents by their very nature are...

Страница 55: ...e it is basic This is a particularly useful additive for the analysis of nucleic acids Tetrahydrofuran THF In ESI use of THF can reduce sensitivity This effect can be counteracted by post column addit...

Страница 56: ...rifluoroacetic acid TFA 0 1 v v surfactants Avoid Negative ion Surfactants organic acids for example acetic acid formic acid trifluoroacetic acid TFA Positive ion Acetic acid formic acid ammonium acet...

Страница 57: ...expected contaminants A pump such as the optional AXP MS pump delivers solvent to the cone wash The PEEK tubing green stripe is recommended is fed through the door and attached to a PEEK fitting whic...

Страница 58: ...____________________ Figure 3 2 Cone wash nozzle in the on position Caution Do not leave the cone wash running when the source heater is turned off this could lead to cone wash solvents condensing on...

Страница 59: ...to the source enclosure using narrow bore PEEK tubing or as shown in the diagram fused silica Use a PTFE or orange stripe PEEK tubing sleeve to secure the fused silica into the T piece Connect a leng...

Страница 60: ...bing connected to the waste or UV detector stream If there are fewer drops in Step 6 then a longer length of tubing is required Continue this until the number of drops in Step 6 is the same as that re...

Страница 61: ...4 Reference Inlet System 4 Reference Inlet System 4 i Introduction 4 1 Overview 4 2 Setting Up the Reference Inlet System 4 3 ____________________________MSQ Hardware Manual __________________________...

Страница 62: ...Reference Inlet System Introduction ____________________________________________________________________________ 4 ii____________________________ MSQ Hardware Manual ____________________________...

Страница 63: ...__________________ Introduction Introduction The MSQ s built in reference inlet system allows easy calibration and tuning This chapter provides instructions on how to set up the reference inlet system...

Страница 64: ...introduce a sample for tuning and mass calibration is to use the reference inlet system This method provides a steady flow of sample directly into the source typically at flow rates of 50 L min Note...

Страница 65: ...t in the calibration reference bottle If not unscrew the calibration reference bottle P N FM102771 fill it with calibrant and screw it back into place Figure 4 2 Calibration reference bottle 2 Check t...

Страница 66: ...ext button A complete system tune will be performed followed by a mass scale calibration A series of messages will be displayed informing you of the progress To print a report click the Print Report b...

Страница 67: ...gure 4 2 Calibration reference bottle 2 Check the waste bottle P N FM102770 If it is full unscrew it empty it and then screw it back into place Figure 4 2 Waste bottle 3 4 5 Check that liquid is emerg...

Страница 68: ...___________ Figure 4 2 Instrument Tuning and Calibration dialog box 6 Select Standard Mass Scale Calibration and click the Next button A series of messages will be displayed informing you of the progr...

Страница 69: ...the ESI Probe 5 6 Replacing the Capillary 5 6 ESI Probe Assembly 5 7 APCI Probe Removal 5 8 APCI Probe Disassembly 5 9 Cleaning the APCI Probe 5 9 Replacing the Capillary 5 10 APCI Probe Assembly 5 1...

Страница 70: ...tine and Preventive Maintenance Introduction ____________________________________________________________________________ 5 ii____________________________ MSQ Hardware Manual _________________________...

Страница 71: ...of how to perform all the user maintenance tasks on the MSQ both routine and as required Use this information in conjunction with the setup and maintenance animations on the MSQ CD shipped with the i...

Страница 72: ...nce schedule Frequency Action Weekly Clean the source if a drop in sensitivity is seen during analysis or if there is a drop in sensitivity when performing the sensitivity verification test refer to t...

Страница 73: ...e blocked Flushing the Capillaries To prevent blockage flush the capillaries with 50 50 acetonitrile water or methanol water after use with phosphates ion pairing agents acids or other additives The p...

Страница 74: ...ater assembly to cool before changing ionization modes 1 2 Unscrew and remove the PEEK finger tight fitting from the ESI probe assembly P N FM102595 Turn the locking plate clockwise to the open positi...

Страница 75: ...Using the 10 mm spanner unscrew the capillary retaining nut Remove the graphite ferrule P N 6070119 PEEK insert P N FM102591 and ESI probe capillary P N FM102698 Caution Exercise care when handling t...

Страница 76: ...for 5 to 10 minutes WARNING Exercise extreme caution when using concentrated nitric acid Always wear protective clothing and use only in a fume hood Observe appropriate disposal requirements when dis...

Страница 77: ...n key Insert the ESI probe capillary P N FM102698 graphite ferrule P N 6070119 and PEEK insert P N FM102591 Caution Exercise care when handling the ESI probe capillary because it is fragile and may be...

Страница 78: ...ter assembly to cool before changing ionization modes 1 2 Unscrew and remove the PEEK finger tight fitting from the APCI probe assembly P N FM102587 Turn the locking plate clockwise to the open positi...

Страница 79: ...Remove the graphite ferrule P N 6070119 PEEK insert P N FM102591 and APCI capillary tube P N FM102594 Caution Exercise care when handling the APCI probe capillary because it is fragile and may be dam...

Страница 80: ...PCI probe mount Screw in the two M3 x 8 cap head stainless steel screws P N 5313020 and tighten using the 2 5 mm Allen key Insert the APCI capillary tube P N FM102594 graphite ferrule P N 6070119 and...

Страница 81: ...ool before carrying out any maintenance Cleaning the Entrance Cone APCI corona pin Cone wash nozzle Probe Figure 5 4 Exposing the entrance cone 1 2 3 4 Vent the instrument if it is currently under vac...

Страница 82: ...trance cone 7 Sonicate the cone first in a 10 v v solution of formic acid and then in methanol Caution Do not sonicate the O ring as the solvent and acid may damage them 8 9 10 Replace the O ring For...

Страница 83: ...ource block assembly and then the procedure for disassembling and cleaning the source block if the source has become completely blocked From the animations main menu choose RF Lens Disassembly Cleanin...

Страница 84: ...1437 located in the holder in the source enclosure door If the cone wash is in use switch off the cone wash pump and turn the cone wash nozzle until it is clear of the entrance cone Turn the entrance...

Страница 85: ...t the base of the RF lens and remove the RF lens Remove the hexapole screw insulator P N FM102248 extraction cone P N FM102263 and extraction cone insulator P N FM102264 Remove the three O rings top l...

Страница 86: ...n particular ensure that the cones are face up at all times Caution Do not sonicate the O rings as the solvent and acid may damage them Cleaning the RF Lens Under normal working conditions this proced...

Страница 87: ...from touching the bottom of the vessel and hence becoming damaged either suspend it on a wire or place a tissue at the bottom of the vessel 2 3 If necessary clean the differential aperture plate with...

Страница 88: ...ngs and screw in the two sealing plugs P N FM102277 using the 6 mm screwdriver There is one plug and O ring at each side of the source block Replace the three O rings top left O ring 7 x 3 Viton degas...

Страница 89: ...in the source block enclosure and tighten the thumbscrews on the source block Replace the cone wash nozzle P N FM102521 Replace the entrance cone assembly P N FM103412 and turn counterclockwise Turn t...

Страница 90: ...this procedure is the source block assembly removed from the MSQ and disassembled Caution Exercise great care when handling the extraction cone Always store with the cone facing upward Note To preven...

Страница 91: ...ESI or APCI probe See ESI Probe Removal or APCI Probe Removal Remove the source block cover Disconnect the heater connectors Using the 2 5 mm Allen key unscrew the two M3 x 10 cap head stainless stee...

Страница 92: ...sert the heater assembly P N FM102576 Screw in the M3 x 10 cap head stainless steel screw P N FM103046 and tighten using the 2 5 mm Allen key Insert the screw insulators and the two M3 x 10 cap head s...

Страница 93: ...should be serviced at regular intervals The Edwards pump does not have filters that require routine maintenance The following maintenance procedures are covered here Checking the rotary pump oil leve...

Страница 94: ...add oil while the pump is running could result in serious personal injury from hot rotary pump oil NOTE Do not mix oil types The oil used in the Edwards Rotary Pump is type Ultragrade 19 P N 062746 o...

Страница 95: ...s Rotary Pump is type Ultragrade 19 P N 062746 or 062747 WARNING Wear gloves when changing the oil Avoid contact with the pump oil it may contain dissolved toxic residues from analyzed samples Observe...

Страница 96: ...15 16 Remove the drain plug from the pump and allow the old oil to drain out until it reaches a trickle If the oil filter is to be replaced Busch pump only remove the old one using the type of tool u...

Страница 97: ...6 3 Restarting the PC 6 3 HPLC System Troubleshooting 6 4 Buffers and Additives 6 4 Mobile Phase Reservoir 6 4 Bubble Problems and Degassing 6 4 Contamination in the LC System 6 5 Tubing and Fittings...

Страница 98: ...Troubleshooting Introduction ____________________________________________________________________________ 6 ii____________________________ MSQ Hardware Manual ____________________________...

Страница 99: ...ionex Service Representative for assistance This chapter is divided into the following sections Troubleshooting Help An introduction to the troubleshooting help system that assists in identifying the...

Страница 100: ...ms relating to liquid chromatography and the HPLC system Spectral problems Problems relating to mass spectral data Calibration Problems relating to calibration Tuning Problems relating to tuning Commu...

Страница 101: ...acturer s specifications Restarting the PC Most communication problems that occur with Xcalibur are transient and can be resolved by restarting the PC To restart the PC do the following 1 2 3 4 5 Try...

Страница 102: ...articles from entering the MS detector Bubble Problems and Degassing Bubble problems in LC systems result from mixing air saturated solvents Air is generally less soluble in solvent mixtures than in p...

Страница 103: ...d if necessary to minimize the solid particles that may be transferred to the pumping system Change the pump seals at least once a year When seals are replaced rinse the piston s to remove any foreign...

Страница 104: ...0 010 6000 psig Yellow 1 16 0 007 8000 psig Red 1 16 0 005 8000 psig The choice of ID depends mainly on the LC flow In general avoid the red 0 005 ID tubing as it is prone to blockage It is mostly use...

Страница 105: ...e manufacturer s manual Injectors are prone to blockage if dirty samples are injected or if particles from the mobile phase or a worn pump seal block the passages Strip and clean the injector regularl...

Страница 106: ...nd Deuterium lamps should last for 1000 hours Noise spikes in the detector can arise from lamp filament flicker Detector cells are prone to trapping air bubbles from the mobile phase or micro particul...

Страница 107: ...nt air from entering the pump to minimize problems associated with bubbles and to improve check valve operation Flushing Flush the system regularly to remove unwanted contaminants and to prevent build...

Страница 108: ...Troubleshooting HPLC System Troubleshooting _____________________________________________________________ 6 10 __________________________ MSQ Hardware Manual ____________________________...

Страница 109: ...on 7 1 Instrument Standby and Shutdown 7 2 In Between Analytical Runs 7 2 Up to Two Weeks 7 3 Two Weeks or More 7 4 Restarting the System 7 6 Pre Switch on Checklist 7 6 System Start up Procedure 7 7...

Страница 110: ...ng Down and Restarting the System Introduction ____________________________________________________________________________ 7 ii____________________________ MSQ Hardware Manual _______________________...

Страница 111: ..._______ Introduction Introduction This chapter provides details of how to shut down the MSQ system for a short period up to 2 weeks or for a longer period It also describes how to restart your system...

Страница 112: ...as been turned off Open the MSQ Tune window in one of the following ways a Double click on the MSQ Tune shortcut icon shown on the Windows desktop b Click on the Start button and choose Programs Xcali...

Страница 113: ...Tune window click on the Toggle Operate button The button will turn from green to gray and the text will change from On to Off Switch off the PC monitor Leave the remainder of the system running with...

Страница 114: ...d Parameters are not visible click on the Show Per Method Parameters slide bar to display them Click on the Toggle Nitrogen Gas button to switch the nitrogen gas flow Off The button will turn from gre...

Страница 115: ...e text will change from On to Off Right click on the MSQ server on the Windows taskbar and choose Vent to vent the system The server is displayed as an icon on the Windows taskbar just to the left of...

Страница 116: ...uning and calibration see the MSQ Getting Started manual for details Pre Switch on Checklist Before you switch on the system after an extended shutdown period a major overhaul or instrument relocation...

Страница 117: ...acuum The server light will change from flashing amber to solid amber Open the MSQ Tune window see page 7 2 Turn on the gas flow If the Per Method Parameters are not visible click on the Show Per Meth...

Страница 118: ...e MSQ is pumping down the server light will be flashing amber When it is pumped down the light will remain amber but stop flashing Reaching high vacuum takes approximately 5 minutes If the MSQ has not...

Страница 119: ...Spares 8 i Introduction 8 1 Consumables 8 2 General Consumables Kit P N 060046 8 2 Probe Maintenance Kit P N 061495 8 4 Source Maintenance Kit P N 061494 8 5 Spares 8 6 ____________________________MS...

Страница 120: ...Consumables and Spares Introduction ____________________________________________________________________________ 8 ii____________________________ MSQ Hardware Manual ____________________________...

Страница 121: ...maintaining your MSQ The parts are categorized as follows Consumable Parts Keep a stock of each of these parts as they may need to be replaced frequently Consumables can be purchased in Kit form The...

Страница 122: ...Part Number FM Part Number Quantity in Kit Cone wash nozzle assembly 060749 FM102521 2 Entrance cone assembly 060746 FM103412 2 Exit cone 060767 FM102263 1 APCI corona pin 060781 FM101433 2 PEEK tube...

Страница 123: ...ton degas 060806 5711035 10 O ring 3 1 Viton degas 060807 5711933 10 O ring BS012 Viton degas 060808 FM100231 10 O ring BS207 Viton degas 060809 FM101417 10 O ring BS007 Viton degas 060810 FM101464 10...

Страница 124: ...ITE VESP GVF 16 MSQ 060769 FM6070119 6 FIXTURE PLATE DEPTH GAUGE MSQ 060772 FM102057 1 INSERT TUBE PEEK MSQ 060774 FM102591 6 PIN CORONA APCI MSQ 060781 FM101433 1 PLUG BLANK APCI MSQ 060783 FM101437...

Страница 125: ...1 EXIT CONE MSQ 060767 FM102263 1 INSULATOR EXIT CONE MSQ 060775 FM102264 1 KIT O RING AND SCREW MSQ 060777 FM104674 1 PLUG SEALING MSQ 060785 FM102277 2 SEAL VACUUM HOUSING MSQ 060789 FM101633 1 O R...

Страница 126: ...CONE WASH MSQ 060684 1 KIT PROBE MAINT MSQ 061495 1 KIT SOURCE MAINT MSQ 061494 1 KIT FILTER MAINT N2 GEN MS 061492 1 OIL MECH PUMP BUSCH QRT SYN 061024 Qt OIL MECH PUMP BUSCH GAL SYN 061025 Gal OIL M...

Страница 127: ...ESI PROBE MSQ 060747 FM102595 1 CAPILLARY ESI PROBE MSQ 060760 FM102598 1 PLUG DRAIN MSQ 060784 FM102604 1 O RING VITON BS258 MSQ 060812 FM102605 1 O RING VITON 7 X 3 MSQ 060813 FM102655 10 CONNECTOR...

Страница 128: ...13 ESI probe capillary 5 6 ion generation 1 13 flushing capillaries 5 3 probe removal 5 8 RF lens 5 16 source figure 1 14 source block assembly 5 13 source description 1 14 cleaning the entrance cone...

Страница 129: ...probe removal 5 4 inorganic acids 3 5 source figure 1 11 Instrument Setup 1 29 source description 1 11 ion evaporation 1 10 ESI probe assembly 5 7 ion generation ESI probe disassembly 5 5 APCI 1 13 E...

Страница 130: ...ne diagnostics 6 4 Rayleigh limit 1 10 sample infusion flow rate 4 2 rebooting the PC 6 3 sample infusion probe temperature 4 4 4 6 reference inlet system starting vacuum pumps 7 7 functional descript...

Страница 131: ...tion 1 8 schematic figure 1 9 self cleaning 1 3 UV detectors 6 7 source block cleaning 5 16 V cleaning Caution 5 16 replacing 5 19 vacuum source block assembly pumping down 7 8 cleaning Warning 5 11 s...

Страница 132: ...___________________________________________________ Index Home Page figure 1 28 introduction 1 28 rebooting the PC 6 3 server 1 29 server figure 1 29 ____________________________MSQ Hardware Manual __...

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