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Routine and Preventive Maintenance

Maintaining the Source Block Assembly

Thermo Scientific

Surveyor MSQ Plus Hardware Manual

11. Lock the probe heater in place by turning its black knobs forward 90 degrees. See

Figure 55

page 74

12. Reinsert the API probe into the probe heater and reattach the PEEK fingertight fitting to

the probe. See

Figure 35

page 57

Removing the Source Block Assembly

You must clean the entire source block assembly on a regular basis if you inject complex
sample matrices or use highly buffered mobile phases. To clean the source block assembly, you
must remove it from the instrument and disassemble it.

To remove the source block assembly from the MS detector

1. If you have not already done so, do the following:

• Prepare your LC/MS system for maintenance as described in

“Preparing the LC/MS

System for Maintenance”

page 80

• Remove the probe and the probe heater as described in

“Clearing Access to the

Source Block Assembly”

page 81

• Remove the entrance cone and the cone wash nozzle as described in

“Removing the

Entrance Cone and the Cone Wash Nozzle”

page 81

2. Loosen the thumbscrews on the source block and pull the source block assembly out of

the MS detector. See

Figure 67

Figure 67.

View of the source block assembly being removed from the MS detector

CAUTION

Wait for the source block and probe heater assembly to cool before carrying out

any maintenance.

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Summary of Contents for Surveyor MSQ Plus

Page 1: ...Surveyor MSQ Plus Hardware Manual 60111 97043 Revision B November 2007 ...

Page 2: ...or any part of this document is strictly prohibited except with the written authorization of Thermo Fisher Scientific Inc The contents of this document are subject to change without notice All technical information in this document is for reference purposes only System configurations and specifications in this document supersede all previous information received by the purchaser Thermo Fisher Scie...

Page 3: ...andards Changes to your system include replacing a part or adding components options or peripherals not specifically authorized and qualified by Thermo Fisher Scientific To ensure continued compliance with EMC and safety standards replacement parts and additional components options and peripherals must be ordered from Thermo Fisher Scientific or one of its authorized representatives FCC Compliance...

Page 4: ...nal regulations Use of this instrument in a manner not specified by Thermo Fisher Scientific could impair any protection provided by the instrument Notice on the Susceptibility to Electromagnetic Transmissions Your instrument is designed to work in a controlled electromagnetic environment Do not use radio frequency transmitters such as mobile phones in close proximity to the instrument For manufac...

Page 5: ... Directives and the recyclers in your country WEEE Konformität Dieses Produkt muss die EU Waste Electrical Electronic Equipment WEEE Richtlinie 2002 96 EC erfüllen Das Produkt ist durch folgendes Symbol gekennzeichnet Thermo Fisher Scientific hat Vereinbarungen mit Verwertungs Entsorgungsfirmen in allen EU Mitgliedsstaaten getroffen damit dieses Produkt durch diese Firmen wiederverwertet oder ents...

Page 6: ...ieurs compagnies de recyclage dans chaque état membre de l union européenne et ce produit devrait être collecté ou recyclé par celles ci Davantage d informations sur la conformité de Thermo Fisher Scientific à ces directives les recycleurs dans votre pays et les informations sur les produits Thermo Fisher Scientific qui peuvent aider la détection des substances sujettes à la directive RoHS sont di...

Page 7: ...dati si raffreddino prima di effetturare l intervento di manutenzione Fire Use care when operating the system in the presence of flammable gases Feuer Beachten Sie die einschlägigen VorsichtsmaBnahmen wenn Sie das System in Gegenwart von entzündbaren Gasen betreiben Incendie Agir avec précaution lors de l utilisation du système en présence de gaz inflammables Fuego Tenga cuidado al operar el siste...

Page 8: ...s and proper procedures to dispose waste oil Heat Before servicing the instrument allow any heated components to cool Fire Use care when operating the system in the presence of flammable gases Eye Hazard Eye damage could occur from splattered chemicals or flying particles Wear safety glasses when handling chemicals or servicing the instrument General Hazard A hazard is present that is not included...

Page 9: ... ESI 3 Atmospheric Pressure Chemical Ionization APCI 6 Scan Types 8 Full Scan 8 Selected Ion Monitoring SIM 8 Data Types 8 Profile Data Type 9 Centroid Data Type 10 MCA Data Type 10 Chapter 2 Functional Description 13 Liquid Chromatograph 15 Reference Inlet System 16 MS Detector 19 Front Panel Status Indicator 19 Rear Panel Controls and Connections 21 Connection Between LC and MS Detector 23 API S...

Page 10: ... the Solvent Waste Bottles 49 Chapter 4 Switching Probes 51 Switching From ESI to APCI 51 Switching From APCI to ESI 53 Chapter 5 Routine and Preventive Maintenance 55 Maintenance Schedule 55 Maintaining the ESI Probe 56 Removing the ESI Probe 57 Removing the ESI Capillary 58 Cleaning or Replacing the ESI Capillary 60 Replacing the Ceramic Sleeve of the ESI Probe 61 Installing the ESI Capillary 63...

Page 11: ...ogen Gas 96 Placing the System in the Off Mode 97 Turning the MS Detector Off from Xcalibur 98 Turning the MS Detector Off from the Tune Window 99 Shutting the System down for Non Routine Maintenance 100 Restarting the System Following a Complete Shutdown 101 Checking the System Connections 102 Restarting the Surveyor MSQ Plus System 103 Resetting the MS Detector 104 Chapter 7 Replaceable Parts 10...

Page 12: ...Contents xii Surveyor MSQ Plus Hardware Manual Thermo Scientific Cone Wash System 123 Flow Splitting 124 PEEK Tubing 124 Index 127 ...

Page 13: ...ion of the MS detector once you have configured it choose Help About Home Page from the Xcalibur Roadmap Home Page Related Documentation In addition to this guide Thermo Fisher Scientific provides the following documents for the Surveyor MSQ Plus MS detector Surveyor MSQ Plus Preinstallation Requirements Guide Surveyor MSQ Plus Getting Connected Surveyor MSQ Plus Getting Started Safety and Special...

Page 14: ... if touched Allow heated components to cool before you service them Place the MS detector in Standby or Off before you open the atmospheric pressure ionization API source The presence of atmospheric oxygen in the API source when the MS detector is On could be unsafe The MS detector automatically goes into Standby when you open the API source however it is best to take this added precaution Take ca...

Page 15: ...om the waste container connected to the Exhaust port on the back of the MS detector to a second dedicated fume exhaust system Consult local regulations for the proper method of exhausting the fumes from your system Do not vent the PVC drain tube or any vent tubing connected to the waste container to the same fume exhaust system to which you have connected the forepump The forepump exhaust contains...

Page 16: ... To contact Customer Service for ordering information Y To suggest changes to documentation or to Help Fill out a reader survey online at www thermo com lcms techpubs Send an e mail message to the Technical Publications Editor at techpubs finnigan lcms thermofisher com Phone 800 685 9535 Fax 561 688 8736 E mail TechSupport C MS thermofisher com Knowledge base www thermokb com Phone 800 532 4752 Fa...

Page 17: ...nalytical instrument that includes an MS detector forepump data system and an optional cone wash pump Integrated with an LC system the Surveyor MSQ Plus MS detector provides you with the separation capability of an HPLC and the detection capability of a single quadrupole MS detector See Figure 1 Figure 1 View of the Surveyor MSQ Plus MS detector and the Surveyor LC system Contents Overview Ion Pol...

Page 18: ...e either a positive or negative charge on the capillary of the API probe at any point in time During a chromatographic run the MS detector can switch the charge applied to the capillary By repelling ions of like charge towards the entrance of the MS detector the charged capillary acts as a charge filter The vacuum produced by the forepump draws both neutral molecules and ionized molecules through ...

Page 19: ...d best in the negative ion polarity mode Rapid screening of unknown analytes Some compounds with functional groups such as carboxylic acids respond only in the negative mode Some compounds with functional groups such as amines alcohols and ketones respond better or only in the positive mode If you do not know the identity of your analyte screen in both modes Ionization Techniques You can operate t...

Page 20: ...els gas phase ions of the same charge The low vacuum of 1 Torr produced by the forepump draws both ionized molecules repelled by the charge on the capillary and neutral molecules in the gaseous phase into the MS detector through the entrance cone Figure 2 shows the steps in the formation of gas phase ions from highly charged droplets Figure 2 Positive ion electrospray mechanism Spectral Characteri...

Page 21: ...st typically of a series of peaks corresponding to a distribution of multiply charged analyte ions You can run ESI in three ion polarity modes positive negative or positive negative switching Because like charges repel each other select the ion polarity mode that matches the polarity of your analytes For acidic compounds which form negative ions in solution select the negative ion polarity mode Fo...

Page 22: ...nts occurs 1 The APCI capillary sprays the sample solution into a fine mist of droplets 2 A high temperature tube the heated nebulizer vaporizes the droplets 3 A high voltage applied to a needle located near the exit end of the tube creates a corona discharge Energized electrons produced by the corona discharge ionize the nitrogen nebulizing gas The nitrogen ions react with the solvent molecules t...

Page 23: ...e no effect You can use APCI in the positive negative or positive negative switching ion polarity mode For most molecules the positive ion mode produces a stronger ion current This is especially true for molecules with one or more basic nitrogen or other basic atoms Exceptions to the general rule are molecules with acidic sites such as carboxylic acids and acid alcohols which produce more negative...

Page 24: ...un SIM can provide lower detection limits than a full scan analysis If you need to detect small quantities of a target compound use SIM if you know the mass spectrum of your target compounds and the mass spectrum of the sample matrix SIM can improve the detection limit for quantitative analyses but it can also reduce specificity In SIM only specific ions are monitored Therefore any compound that p...

Page 25: ...ampling intervals The intensity at each sampling interval is displayed with the intensities connected by a continuous line In general the profile data type is used when you tune and calibrate the MS detector so that you can easily see and measure mass resolution In general the profile data type is used when you tune and calibrate the MS detector so that you can easily see and measure mass resoluti...

Page 26: ...ee Figure 6 As Xcalibur acquires each scan it adds the intensity data to the accumulated summed data of previous scans An advantage of MCA is that although noise accumulates at the same rate as sample related data summing random noise over a number of scans reduces its effect increasing the signal to noise ratio A further advantage of MCA is that Xcalibur writes data to disk only at the end of an ...

Page 27: ...ypes Thermo Scientific Surveyor MSQ Plus Hardware Manual 11 Figure 6 Full scan MCA spectrum of horse heart myoglobin 700 800 900 1000 1100 1200 1300 m z 0 100 848 808 771 738 707 694 893 942 998 944 1060 999 1131 1212 1305 ...

Page 28: ......

Page 29: ...urveyor LC Surveyor MSQ Plus MS detector cone wash pump forepump and data system Contents Liquid Chromatograph Reference Inlet System MS Detector Cone Wash System Data System EDWARDS 30 Oil Mist Filter EMF 20 EDWARDS MSQ Surveyor LC system Autosampler Pump Solvent trap Forepump Surveyor MSQ Plus MS detector Reference inlet system inside front door Cone wash pump Monitor Data system computer User s...

Page 30: ...flow tee For instructions on connecting a split flow tee see Appendix A Optimizing the LC Conditions Upon entering the API source of the MS detector preformed sample ions are desolvated by electrospray ionization ESI or sample molecules are desolvated and ionized by atmospheric pressure chemical ionization APCI The vacuum system draws the vaporized molecules and ions into the ion optics The ion op...

Page 31: ... number of devices displayed in the Devices list box you can do one of the following Select All in the Device Type box to display all the available devices controlled by Xcalibur 1 4 Select LC in the Device Type box to display only LC pumps Select AS in the Device Type box to display only autosamplers and devices that include an autosampler Select Detector in the Device Type box to display only de...

Page 32: ...ale Calibration which is a subset procedure of the Full System Autotune procedure During an automated Full System Autotune procedure the Surveyor MSQ Plus MS detector and instrument control software perform these steps The MS detector infuses the calibrant solution and the software electronically adjusts the resolution of the peaks at low mid and high mass The resolution of the peaks is adjusted t...

Page 33: ...witching valve One end of the PEEK tubing is inserted into the reference reservoir and the other end of the tubing is attached to port 5 of the Rheodyne microinjection valve Pressuring the reference reservoir with nitrogen gas and switching the valve to the load position forces the calibrant solution through the tubing into a 500 μL sample loop as shown in Figure 10 After the sample loop is filled...

Page 34: ...tion Figure 11 Microinjection switching valve in the Inject position 1 2 3 4 5 6 500 uL sample loop To waste Nitrogen line Clip Reference inlet reservoir Waste reservoir Connection to LC Grounding union To API probe 1 2 3 4 5 6 500 uL sample loop To waste Nitrogen line Clip Reference inlet reservoir Waste reservoir Connection to LC Grounding union To API probe ...

Page 35: ...tatus Indicator One light emitting diode LED is located at the upper right corner of the front panel of the Surveyor MSQ Plus MS detector as shown in Figure 12 Table 2 lists the states of the Status LED Initially when a Thermo Fisher Scientific service engineer installs the Surveyor MSQ Plus MS detector turns on the forepump the status LED is red As the system pumps down the LED flashes yellow Aft...

Page 36: ... of the Surveyor MSQ Plus MS detector Table 2 States of Surveyor MSQ Plus MS Status LED Instrument Status Light Vented Red Venting Red Pumping down Flashing yellow Under vacuum above vacuum trip Red Under vacuum ready for use Yellow Operate On Surveyor MSQ Plus MS in use Green Source enclosure open Red Status LED ...

Page 37: ...ode the circuit breaker is kept in the On I position The power supply requirements for the Surveyor MSQ Plus MS detector are 230 Vac regulated to 5 at 50 or 60 Hz The Surveyor MSQ Plus MS detector ships with power cords appropriate to its shipping destination A USB port an eight terminal contact closure connector labeled USER I O and a reset button are located in the upper right corner of the rear...

Page 38: ...e with 6 mm OD PTFE tubing Figure 13 Rear panel of Surveyor MSQ Plus MS detector PUMP OUT MAINS IN MAINS ON OFF RESET USER I O START IN START IN USB READY OUT READY OUT GAS IN 6 BARS MAX SOURCE BACKING EXHAUST USB connection to data system computer Connector for contact closure Reset button for downloading firmware Power switch Power supply for forepump Connection to line power Connected to user s...

Page 39: ...on APCI Electrospray Ionization ESI The sample consisting of preformed ions in solution enters the source through a stainless steel insert capillary held at a voltage of 1 to 5 kV The insert capillary is surrounded by a tube that directs a concentric flow of nitrogen nebulizing gas past the droplets of liquid forming at the tip of the probe The action of the nebulizing gas and the high voltage pro...

Page 40: ... 15 View of the ESI probe showing the principal components and the pressure regions LC eluent Nebulizing gas N2 Sheath gas N2 Probe heater Insert capillary Entrance cone RF dc prefilter RF df prefilter vacuum region M Path vacuum region Atmospheric pressure region 1 Torr 10 3 Torr Forepump Exit cone ...

Page 41: ...heated nebulizer region A corona pin which is mounted between the heated region and the entrance cone ionizes the sample molecules with a discharge needle operating at a constant current of 2 to 10 μA in the positive polarity mode or 5 to 30 μA in the negative polarity mode The newly formed ions then enter the focusing region through the entrance cone and pass into the RF dc prefilter region See F...

Page 42: ...r mass to charge ratio and then passes them to the ion detection system In the Surveyor MSQ Plus MS detector the mass analyzer is a single quadrupole rod assembly The mass analyzer is described in detail in the following topics RF and DC Fields Applied to the Quadrupoles Mass Analysis RF and DC Fields Applied to the Quadrupoles In a quadrupole rod assembly rods diagonally opposite each other in th...

Page 43: ...e all other ions undergo unbounded oscillations These ions strike one of the rod surfaces become neutralized and are pumped away by the vacuum system See Figure 19 Then at a later time as the mass analyzer scans to a higher mass both RF and dc voltages change and ions of the next mass to charge ratio for example m z 181 are allowed to pass while all other ions including m z 180 become unstable and...

Page 44: ...al of 10 kV for negative ion detection or 10 kV for positive ion detection is applied to the conversion dynode When an ion strikes the surface of the conversion dynode one or more secondary particles are produced These secondary particles can include positive ions negative ions electrons and neutrals When positive ions strike a negatively charged conversion dynode the secondary particles of intere...

Page 45: ...he electron multiplier is a small cup located at the exit end of the cathode The anode collects the electrons produced by the cathode The anode screws into the anode feedthrough in the top cover plate Secondary particles from the conversion dynode strike the inner walls of the electron multiplier cathode with sufficient energy to eject electrons The ejected electrons are accelerated farther into t...

Page 46: ...el of noise The high voltage applied to the conversion dynode results in a high conversion efficiency and increased signal That is for each ion striking the conversion dynode many secondary particles are produced The increase in conversion efficiency is more pronounced for more massive ions than for less massive ions Because of the off axis orientation of the ion detection system relative to the m...

Page 47: ...clude the following Vacuum Manifold Turbomolecular Pump Forepump Pirani Gauge Vent Valve A functional block diagram of the vacuum system is shown in Figure 21 Figure 21 Functional block diagram of the vacuum system Atmospheric pressure region M Path region RF dc preﬁlter region Analyzer region 1 Torr 10 3 Torr 10 6 Torr Split ﬂow turbomolecular pump Exhaust Foreline Forepump Vent valve Air ﬁlter S...

Page 48: ...ich evacuates the transfer lens region is rated at 125 L s The high vacuum port of the turbomolecular pump which evacuates the mass analyzer region is rated at 200 L s Under normal operating conditions the pump provides a vacuum of approximately 10 3 Torr in the transfer lens region and 10 6 Torr in the mass analyzer region The main power circuit breaker switch turns the power to the turbomolecula...

Page 49: ...kPa 75 psi or 450 kPa 45 psi 99 purity enters the Surveyor MSQ Plus MS detector through a 6 mm port labeled GAS IN located on the rear panel of the MS detector See Figure 13 on page 22 The inlet gas hardware then controls the flow of nitrogen gas to the API probes and the reference inlet reservoir As Figure 22 shows the inlet gas hardware consists of two regulators three solenoid valves and two re...

Page 50: ...ervoir This regulator which is inside the MS detector is preset at the factory The first solenoid valve is the On Off control for the flow of nitrogen gas into the Surveyor MSQ Plus MS detector To turn this valve on or off you click the Nitrogen Gas On Off toggle button in the Per Method Parameters table of the Tune window see Figure 24 After you turn on the nitrogen gas you can hear the jet of ni...

Page 51: ...s open to the mobile phase stream from the LC pump The stream pushes the calibrant out of the sample loop and through the API probe After the microinjection valve switches to the inject position the third solenoid valve switches to the On position allowing the nitrogen gas to vent to atmosphere and depressurizing the reference inlet reservoir The first restrictor allows a constant low flow of nitr...

Page 52: ...tem consists of a cone wash pump PEEK tubing and a cone wash nozzle Red 0 005 in ID PEEK tubing connects the cone wash pump to the Surveyor MSQ Plus MS detector Inside the Surveyor MSQ Plus MS detector the red PEEK tubing is connected to one end of a union Green 0 030 in ID PEEK tubing is connected to the other end of the union The green PEEK tubing is connected to the back of the source block beh...

Page 53: ...oftware that handles the communication between the Surveyor MSQ Plus MS detector and the data system PC The Xcalibur data system also processes data that is acquired by the Surveyor MSQ Plus MS detector Information about the status of the Surveyor MSQ Plus MS detector is available from the Xcalibur HomePage Information view and from the Server LED icon The data system for the Surveyor MSQ Plus MS ...

Page 54: ...vices The Xcalibur software package for the Surveyor MSQ Plus MS detector includes the application programs listed in Table 3 Xcalibur Home Page version 2 0 is required for the MSQ 2 0 Plus version of the Surveyor MSQ Plus detector software The firmware versions of the LC devices controlled by Xcalibur 2 0 with Quan Devices are listed in your Surveyor MSQ Plus Getting Connected Guide When you laun...

Page 55: ...stem Tray of the Windows Taskbar just to the left of the time display Figure 27 View of taskbar showing the Server icon The Server icon provides you with information about the status of the Surveyor MSQ Plus MS detector and mimics a tri state LED display red green yellow showing Steady red when the mains are on and the instrument is vented or an error has occurred within the system Flashing yellow...

Page 56: ...repump without turning off the MS detector set the On Off switch on the forepump to the Off position Choose Exit to close the server If Xcalibur is running exiting the server is not allowed and the error message shown in Figure 29 appears Figure 28 Server shortcut menu Figure 29 Error message displayed when Xcalibur is running and you attempt to exit the Server application Tune Window The Surveyor...

Page 57: ...desktop Then double click the Server icon that appears in the System Tray of the Windows taskbar From the Windows XP taskbar choose Start All Programs Xcalibur Tune Then double click the Server icon that appears in the System Tray of the Windows taskbar Note When you create an instrument method to control your LC MS instrument during a sequence run you import the tune file that contains the empiri...

Page 58: ...le name of the currently active tune file For example default tune is the name of the Surveyor MSQ Plus default tuning file Menu Bar The Tune window menu bar contains the following menus File View and Help Toolbar You can use the toolbar buttons to start and stop acquiring data and to print a tune report Menu bar Toolbar Per Method Parameters table Title bar Peak Display Scan Events table Status b...

Page 59: ...is working correctly Scan Events Table Use the Tune Scan Events table or Peak Display controls to define all the scan events that you want to acquire when performing a manual tune Per Method Parameters Table Use the Tune Per Method Parameters table to enter values and define the settings for the per method tuning parameters The table also provides individual tuning parameter readbacks You can adju...

Page 60: ...hip a printer with the Surveyor MSQ Plus MS detector If you choose to connect a printer that communicates through a USB cable connect the cable to one of the USB ports on the front of the data system computer You set up the printer from the Print Setup dialog box To open the Print Setup dialog box choose File Print Setup in any window ...

Page 61: ...ply Checking the Disk Space Checking the Oil Level in the Oil Mist Filter Checking the Nitrogen Supply Check the nitrogen supply on the regulator of the nitrogen gas tank or liquid nitrogen boil off tank Make sure that you have sufficient gas for your analysis Typical nitrogen consumption is 15800 liters per day based on a 24 hr day If necessary replace the tank Verify that the pressure of nitroge...

Page 62: ...tage of the current drive that is available Total capacity of the current drive 2 To select another disk drive so that you can determine its disk space click the Directory button 3 When you have completed this procedure click OK to close the dialog box If necessary free space on the hard disk by deleting obsolete files and by moving files from the hard disk drive to a backup medium First copy file...

Page 63: ...gs to Do After Operating the MS Detector This section contains the following procedures that you might want to perform after you complete your analyses Flushing the API Probes Placing the System in the Off Mode Draining the Oil Mist Filter and Purging the Pump Oil Emptying the Solvent Waste Bottles EDWARDS 30 Oil Mist Filter EMF 20 EDWARDS To exhaust vent Maximum oil level mark Oil return tubing G...

Page 64: ... weekends In the Off mode the system is left under vacuum but the nitrogen flow is reduced to a bleed through the API probe the electron multiplier and conversion dynode are turned off the power to the ion optics is turned off and the power to the probe heater is turned off Refer to Placing the System in the Off Mode on page 97 for instructions on turning the system to the Off mode Draining the Oi...

Page 65: ... by clicking the Nitrogen Gas On Off toggle button 3 Open the gas ballast valve on the Edwards forepump by turning it six rotations counter clockwise 4 Operate the Edwards forepump for approximately 15 minutes with the gas ballast valve open The oil in the oil mist filter returns to the forepump relatively quickly The prescribed time period of 15 minutes for ballasting is for the removal of volati...

Page 66: ......

Page 67: ...ose Turn Device Off from the menu Open the Per Method Parameters table in the Tune window Take the system out of the Operate mode by clicking the Operate On Off toggle button and then turn off the nitrogen gas by clicking the Nitrogen Gas On Off toggle button 3 Allow the probe heater to cool 4 Unscrew and remove the PEEK fingertight fitting from the ESI probe 5 Turn the locking plate on the ESI pr...

Page 68: ...tor setup for the APCI mode Figure 33 shows the corona pin in the operational position for the APCI mode 8 Turn the corona pin knob 90 degrees to its horizontal position 9 Insert the PEEK fingertight fitting into the APCI probe and screw in 10 Adjust the nitrogen gas pressure to 310 kPa 45 psi Figure 32 Surveyor MSQ Plus MS detector setup for the APCI mode CAUTION Take care not to damage the capil...

Page 69: ...s table in the Tune window Take the system out of the Operate mode by clicking the Operate On Off toggle button and then turn off the nitrogen gas by clicking the Nitrogen Gas On Off toggle button 3 Allow the probe heater to cool 4 Unscrew and remove the PEEK fingertight fitting from the APCI probe 5 Turn the corona pin knob 90 degrees to its vertical position 6 Turn the locking plate of the APCI ...

Page 70: ...shown in Figure 34 Then turn the locking plate counterclockwise to the closed position 9 Insert the PEEK fingertight fitting into the ESI probe and screw in See Figure 34 which shows the Surveyor MSQ Plus MS detector setup for the ESI mode 10 Adjust the nitrogen gas pressure to 520 kPa 75 psi Figure 34 Surveyor MSQ Plus MS detector setup for the ESI mode ESI probe Corona pin knob Source housing Pr...

Page 71: ...ur Surveyor MSQ Plus MS detector in optimal working condition Maintenance Schedule Table 4 contains a list of routine maintenance procedures that you must perform at the intervals specified The maintenance schedule provides only a rough guide to the maintenance tasks you are responsible for The appropriate frequency for these tasks depends on instrument usage and the level of system induced contam...

Page 72: ... that required buffered solvents Refer to Flushing the API Probes on page 48 Replace the capillary if it becomes clogged Refer to Maintaining the ESI Probe on page 56 or Maintaining the APCI Probe on page 67 Clean the probe if it becomes contaminated Refer to Maintaining the ESI Probe on page 56 or Maintaining the APCI Probe on page 67 Drain the oil from the oil mist filter and purge the oil in th...

Page 73: ...hat it is turned off 2 Turn off the nitrogen gas the probe heater and the ion optics by doing one of the following From the Info view Status page in the Xcalibur data system right click the Surveyor MSQ listing and choose Turn Device Off from the shortcut menu Open the Per Method Parameters table in the Tune window Take the system out of the Operate mode by clicking the Operate toggle button and t...

Page 74: ...lary To clean or replace the ESI capillary or to replace the ceramic sleeve you must remove the ESI capillary from the probe See Figure 83 on page 114 for the part numbers of the ESI probe components Y To remove the capillary from the ESI probe 1 Remove the ESI probe from the MS detector as described in Removing the ESI Probe on page 57 CAUTION Because its capillary tip and ceramic sleeve are frag...

Page 75: ...locking plate 3 Using the front end of the probe clamp unscrew the capillary retaining nut adaptor and remove it from the ESI probe See Figure 38 Figure 38 Removing the capillary retaining nut adaptor 4 Place a lint free cloth on the workbench and then gently shake the ESI capillary P N FM102598 graphite ferrule P N 6070119 and PEEK tube insert P N FM102591 assembly out of the ESI probe onto the c...

Page 76: ...I capillary 1 Remove the ESI probe from the probe heater as described in Removing the ESI Probe on page 57 2 Remove the ESI capillary from the probe as described in Removing the ESI Capillary on page 58 3 If the capillary is reusable clean its surface with 50 50 methanol water 4 Reinstall the clean capillary or a new capillary as described in Installing the ESI Capillary on page 63 ESI capillary G...

Page 77: ...e the capillary as described in Removing the ESI Capillary on page 58 3 Use the 2 5 mm Allen key to unscrew the two M3 8 cap head stainless steel screws from the ESI probe mount See Figure 42 4 Pull the ESI probe mount out of the ESI ceramic sleeve and ceramic mount assembly 5 Remove the ESI ceramic sleeve from the ESI ceramic mount by pulling the sleeve forward through the top of the mount As Fig...

Page 78: ...e 42 7 Place the O rings in position in the ESI ceramic mount and then insert the ESI probe mount into the ESI ceramic mount and ceramic sleeve assembly 8 Insert the two M3 8 cap head stainless steel screws into the ESI probe mount and tighten with the 2 5 mm Allen key 9 Reinstall the ESI capillary and reassemble the probe as described in Installing the ESI Capillary on page 63 4 00 mm OD 3 90 mm ...

Page 79: ...K tube insert and graphite ferrule Adjust the graphite ferrule such that 2 mm of the PEEK tube insert is visible on the back end of the assembly See Figure 43 Figure 43 Capillary PEEK tube and graphite ferrule assembly 2 While holding the ESI probe in the vertical position use tweezers to insert the capillary PEEK tube insert and graphite ferrule assembly into the ESI probe See Figure 44 ESI probe...

Page 80: ... PEEK tube insert into the probe until it meets resistance b Using tweezers push the capillary into the probe until it is flush with the PEEK sleeve c Visually check that the capillary is protruding from the tip of the probe As Figure 45 shows the capillary should protrude from the tip of the probe Figure 45 View of capillary inserted into the ESI probe mount ESI capillary Graphite ferrule PEEK sl...

Page 81: ...s the capillary protruding from the probe tip Figure 46 View of the ESI probe with the capillary retaining nut screwed in finger tight 6 Using the probe clamp tighten the capillary retaining nut by one half turn Do not overtighten the nut Overtightening the nut can cause solvent leakage 7 Finish reassembling the ESI probe a Place the locking plate and probe clamp in position b Insert the M3 10 cap...

Page 82: ...e the ESI probe into the probe heater 3 Turn the locking plate counterclockwise to the closed position to lock the probe in place See Figure 35 on page 57 4 Connect the PEEK fingertight fitting to the ESI probe See Figure 35 Hole in middle of spacer 0 7 mm 0 64 mm 0 01 mm depth of ESI spacer CAUTION Take care when inserting the ESI probe into the probe heater The capillary protruding from the end ...

Page 83: ...e 1 Removing the APCI Probe 2 Removing the APCI Capillary 3 Installing the APCI Capillary 4 Installing the APCI Probe Removing the APCI Probe Y To remove the APCI probe from the probe heater 1 Ensure that the flow from the LC pump is turned off 2 Turn off the nitrogen gas the probe heater and the ion optics by doing one of the following In the Status page of the Xcalibur data system right click th...

Page 84: ...SQ Plus MS detector set up for the APCI mode Figure 49 Remove the APCI probe from the probe heater Removing the APCI Capillary Y To remove the capillary from the APCI probe 1 Using a 2 5 mm Allen key unscrew the M3 10 cap head stainless steel screw P N FM103046 from the probe clamp See Figure 50 2 Remove the probe clamp and the locking plate PEEK fingertight fitting Locking plate in locked positio...

Page 85: ...partially disassembled APCI probe with capillary removed 5 Pull the APCI capillary out of the PEEK tube insert and then do one of the following If the capillary is partially blocked or blocked dispose of it If the capillary is reusable clean its surface with 50 50 methanol water CAUTION Exercise care when handling the APCI capillary because it is fragile and can be damaged easily Probe clamp Locki...

Page 86: ...d Figure 52 3 Adjust the position of the APCI capillary a Holding the APCI probe in the vertical position carefully shake the PEEK tube insert into the probe until it meets resistance b Using tweezers push the capillary into the probe until it is flush with the PEEK sleeve c Visually check that the capillary is protruding from the tip of the probe Figure 51 Inserting the capillary PEEK sleeve and ...

Page 87: ...otrudes from the tip of the probe See Figure 53 Figure 53 View of APCI probe with the capillary retaining nut screwed in finger tight 6 Using the probe clamp tighten the capillary retaining nut by one half turn Do not overtighten the screw 7 Finish reassembling the probe a Place the locking plate and probe clamp in position b Insert the M3 10 cap head stainless steel screw P N FM103046 and tighten...

Page 88: ...probe heater See Figure 49 on page 68 2 Turn the locking plate counterclockwise to the closed position to lock the probe in place See Figure 48 on page 68 3 Connect the PEEK fingertight fitting to the APCI probe See Figure 48 0 41 mm depth of APCI spacer 0 5 mm 10 mm CAUTION Take care when inserting the APCI probe into the probe heater The capillary protruding from the end of the probe is fragile ...

Page 89: ...n or repair the probe heater follow these procedures 1 Removing the Probe Heater 2 Cleaning the Probe Heater or Replacing the Detent Screw Insulator 3 Installing the Probe Heater Removing the Probe Heater Y To remove the probe heater from the probe mount 1 Remove the ESI or APCI probe Refer to Removing the ESI Probe on page 57 or Removing the APCI Probe on page 67 2 Rotate the black knobs of the p...

Page 90: ...View of the probe heater and its connections to the front panel of the MS detector Figure 56 View of the probe heater knobs in the removal position Grounding cable Green Thermocouple connector Probe mount Probe heater knobs in locked position Green Thermocouple connector White Power connector Probe heater knobs in removal position ...

Page 91: ...ensor The white connector connects the probe heater to its power source 4 Store the probe heater in the holder to the left of the source compartment until you are ready to clean it See Figure 58 5 To remove the probe heater from the MS detector use a 1 Phillips head screwdriver to detach the grounding strap from the probe heater See Figure 58 Figure 57 View of power connector and thermocouple conn...

Page 92: ...to repair the probe See Figure 86 on page 117 Y To replace a broken detent screw insulator 1 Disassemble the detent screw assembly a Using a flat blade screwdriver loosen and remove the spring screw Figure 59 View of the slot in the top of the spring screw b Remove the spring from the spring cup and set the spring aside Because the spring is reusable it is not provided in the repair kit c Pull the...

Page 93: ... screw insulator into the underside of the probe heater body b Slide the probe screw sleeve over the top of the detent screw insulator c Insert the spring that you removed from the broken assembly into the spring cup d Align the bottom of the spring cup with the probe screw sleeve e Insert the spring screw into the spring cup and tighten the assembly with a flat blade screwdriver Spring screw Spri...

Page 94: ...to the probe heater See Figure 58 on page 75 3 Rotate the black knobs of the probe heater so that they face away from each other See Figure 56 on page 74 4 Insert the tube portion of the probe heater into the probe mount 5 Rotate the black knobs of the probe heater forward to their locking position See Figure 55 on page 74 6 Plug the green connector and the white connector into their respective re...

Page 95: ...ove the source block assembly from the MS detector and disassemble it To clean any or all of the components of the source block assembly follow these procedures 1 Preparing the LC MS System for Maintenance 2 Clearing Access to the Source Block Assembly 3 Removing the Entrance Cone and the Cone Wash Nozzle 4 Cleaning the Entrance Cone and the Cone Wash Nozzle 5 Removing the Source Block Assembly 6 ...

Page 96: ...Surveyor MSQ Plus MS detector is under vacuum vent it Right click the Server icon and choose Vent from the shortcut menu Venting the Surveyor MSQ Plus MS detector turns off the turbomolecular pump It does not turn off the Edwards forepump 5 Wait 2 or more minutes before proceeding so that the system has time to vent 6 Turn off the Edwards forepump by doing one of the following Turn off the power t...

Page 97: ...tector is set up in the APCI mode rotate the corona pin knob downward to its vertical position Removing the Entrance Cone and the Cone Wash Nozzle Y To remove the entrance cone and the cone wash nozzle 1 If you have not already done so vent the MS detector as described in Preparing the LC MS System for Maintenance on page 80 and clear the access to the source block as described in Clearing Access ...

Page 98: ...rnal components of the source block assembly go to Removing the Source Block Assembly on page 85 Figure 63 Entrance cone with cone facing upwards Tip It is easy to drop small objects such as the entrance cone and the cone wash nozzle into the drain at the bottom of the source enclosure Temporarily blocking the drainage holes in the bottom of the source enclosure will prevent small objects from fal...

Page 99: ...64 Backside of the entrance cone showing its O ring BS010 2 Sonicate the entrance cone in 100 methanol If methanol does not remove the contamination sonicate the cone in a 10 v v aqueous solution of formic acid rinse with distilled water and then rinse with 100 methanol 3 Using a microscope set to 30x magnification inspect the inside of the cone to ensure cleanliness See Figure 65 Figure 65 View o...

Page 100: ... following If the internal components of the source block assembly do not need cleaning go to step 7 If the internal components of the source block assembly need cleaning go to the next procedure Removing the Source Block Assembly 7 Holding the cone wash nozzle by its base insert it into the source block and then turn the nozzle to the right See Figure 62 on page 82 8 Insert the entrance cone into...

Page 101: ... instrument and disassemble it Y To remove the source block assembly from the MS detector 1 If you have not already done so do the following Prepare your LC MS system for maintenance as described in Preparing the LC MS System for Maintenance on page 80 Remove the probe and the probe heater as described in Clearing Access to the Source Block Assembly on page 81 Remove the entrance cone and the cone...

Page 102: ...block assembly with the three screws connecting the RF dc prefilter to the source block Table 5 Cleaning schedule for RF dc prefilter Sample Solvent Type Cleaning Frequency Pure samples and solvents 6 months Standard samples 3 to 6 months Complex matrices for example crude plasma and urine 1 to 4 weeks with operation of cone wash Non volatile buffer Weekly with operation of cone wash IMPORTANT You...

Page 103: ...y perform a deep cleaning as described in the following procedure Y To perform a deep cleaning of the RF dc prefilter 1 Immerse the RF dc prefilter in a graduated cylinder containing 100 distilled water Sonicate for 15 min 2 Decant the water and fill the graduated cylinder with 100 methanol Sonicate for 15 min 3 Decant the methanol and fill the graduated cylinder with 100 acetone Sonicate for 15 m...

Page 104: ... d Examine the screws of the differential aperture plate to ensure that they are burr free and flush or below the plane of the aperture plate If you do not need to clean the remaining components of the source block assembly proceed to Assembling the Source Block Assembly on page 90 Figure 70 View of differential aperture plate Cleaning the Extraction Cone and the Source Block If you use buffered m...

Page 105: ...of the source block and its components b Remove the three O rings Top left O ring 9 12 mm ID 3 53 mm THK viton black P N 00107 01 00047 Bottom left O ring BS207 viton black P N FM101417 Right O ring BS225 viton black P N FM103048 O ring BS207 O ring BS225 Extraction cone insulator O ring 9 mm ID 3 mm THK Extraction cone with the cone facing the source block Hexapole screw insulator CAUTION When th...

Page 106: ...ee o rings see Figure 71 Top left O ring 9 12 mm ID 3 53 mm THK viton black P N 00107 01 00047 Bottom left O ring BS207 viton black P N FM101417 Right O ring BS225 viton black P N FM103048 2 First install the extraction cone insulator P N FM102264 Then install the extraction cone P N FM102263 with the cone facing the source block And finally install the hexapole screw insulator P N FM102248 See Fi...

Page 107: ...e MS detector 1 Insert the source block assembly P N FM102573 into the source block enclosure and then tighten the thumbscrews on the source block See Figure 67 on page 85 2 Handling the cone wash nozzle by its base because the tip is fragile insert the cone wash nozzle P N FM102521 into the source block and then carefully rotate the nozzle tip to the right See Figure 73 Properly aligned component...

Page 108: ...e 74 6 Install the API probe a Turn the locking plate clockwise to the open position and carefully insert the ESI probe P N FM102595 see Figure 36 on page 58 or the APCI probe P N FM102587 see Figure 49 on page 68 into the probe heater b Turn the locking plate counterclockwise into the closed position c Screw the PEEK fingertight fitting into the ESI probe assembly P N FM102595 or APCI probe assem...

Page 109: ...both the level and the color of the oil in the forepump at least once a month Check the oil by looking through the oil sight level window of the forepump See Figure 74 The oil level should be between the upper and lower marks positioned next to the window The oil color should be a clear straw color If the oil level is near or below the lower mark add more oil as described in the manual that comes ...

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Page 111: ...t to a new location we recommend that you perform a Full System Autotune Shutting Down the System in an Emergency If you need to turn off the MS detector in an emergency place the main power circuit breaker switch in the Off O position See Figure 75 The main power switch which is labeled MAINS ON OFF is located on the rear panel of the MS detector in the lower right quadrant Turning the main power...

Page 112: ...ts power switch to the Off position 2 Turn off the flow from your LC pump a If your LC pump is controlled from the Xcalibur data system turn it off from its respective Direct Control dialog box or place it in the Standby mode from the Info View Status page b If your LC pump is not controlled from the Xcalibur data system turn it off from its keypad control panel 3 If the Tune window is not open op...

Page 113: ...s left under vacuum but the nitrogen flow is reduced to a bleed through the API probe the electron multiplier and conversion dynode are turned off the power to the ion optics is turned off and the probe heater is turned off Therefore placing the instrument in the Off mode allows you to conserve your laboratory nitrogen supply and increase the lifespan of the electron multiplier In addition you can...

Page 114: ... the Status tab to open the Status page 4 To turn off the flow from the LC pump If your LC pump is controlled from the Xcalibur data system right click the pump listing on the Status page Then choose Turn Device Into Standby from the shortcut menu See Figure 76 If your LC pump is not controlled from the Xcalibur data system turn it off from its control keypad Figure 76 Info View Status page showin...

Page 115: ...f your LC pump is controlled from the Xcalibur data system turn it off from its respective Direct Control dialog box or place it in the Standby mode from the Info View Status page b If your LC pump is not controlled from the Xcalibur data system turn it off from its keypad control panel 3 If the Tune window is not open open it a Double click the Tune icon on the Windows desktop After you double cl...

Page 116: ... the System down for Non Routine Maintenance Y To shutdown the Surveyor MSQ system for a non routine maintenance procedure or to relocate the instrument 1 If you are using the optional cone wash pump turn it off by turning its power switch to the Off position 2 Open the Xcalibur data system by choosing Start All Programs Xcalibur Xcalibur from the Windows desktop 3 If the Info View is not displaye...

Page 117: ...s off the power to the Edwards forepump which gets its line power from the Pump Out receptacle on the rear panel of the MS detector 9 Close the nitrogen gas cylinder at the main regulator Restarting the System Following a Complete Shutdown Following a long term shutdown carry out the visual checks listed in the Pre switch on checklist shown in Table 6 and then follow the system start up procedure ...

Page 118: ...nnections required for the LC system have been made Vacuum Connections The Source manifold on the rear panel of the Surveyor MSQ Plus MS detector is connected to the forepump The Backing manifold on the rear panel of the Surveyor MSQ Plus MS detector is connected to the forepump Exhaust Connections The Exhaust manifold on the rear panel of the Surveyor MSQ Plus MS detector is connected to the solv...

Page 119: ...stem reaches the appropriate vacuum pressure the server light changes from flashing amber to solid amber Reaching high vacuum takes approximately 10 minutes c If the Surveyor MSQ Plus MS detector has not reached vacuum after 30 minutes The server light might still be red or flashing amber Refer to Table 2 on page 20 check for leaks in the system 4 Open the Tune window by double clicking the Server...

Page 120: ...he MS Detector If communication between the MS detector and data system computer is lost it might be necessary to reset the MS detector using the Reset button on the power panel Pressing the Reset button creates an interrupt on the CPU PCB of the embedded computer This causes the embedded computer to restart into a known default state The procedure given here assumes that the MS detector and data ...

Page 121: ... and Reset Resetting the MS Detector Thermo Scientific Surveyor MSQ Plus Hardware Manual 105 Figure 80 View of the upper right hand corner of the MS detector s rear panel START IN START IN READY OUT READY OUT USB USER I O RESET ...

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Page 123: ...as follows Consumables Keep a stock of each of these parts as you might need to replace them frequently Spares You can order these parts as required Connection Kits This is the interface kit that you use to connect an Agilent LC system to your MS detector You do not need an interface kit to connect a Surveyor LC to your Surveyor MSQ Plus MS detector The manuals for the Surveyor MSQ Plus MS detecto...

Page 124: ...er Repair kit 60111 62010 Detent screw insulator FM102585 Screw sleeve FM102582 Spring screw FM102583 Spring cup FM102584 MSQ Plus Hardware and O ring kit 60111 62018 Sealing plug 2 each FM102277 Ferrule SGE 1 16 graphite vespel 10 each 6070119 Spring E type clip stainless steel MSQ only 3 each FM102574 Spring compression 4 6 mm OD 0 45 N mm 30 mm length 00111 01 00013 O ring 13 87 mm ID 3 53 mm T...

Page 125: ...be heater assembly 5711933 3 0 1 0 Source block assembly small sealing plug FM103016 3 3 2 40 Probe mount assembly FM101464 3 68 1 78 BS007 Cone wash nozzle 5711020 5 28 1 78 BS009 API probe 5711000 6 07 1 78 BS010 Entrance cone 00107 01 00026 9 12 3 53 Source block assembly FM100231 9 25 1 78 BS012 API probe FM101522 12 42 1 78 BS014 Source block assembly large sealing plug FM101417 13 87 3 53 BS...

Page 126: ...I probe assembly 5 28 mm ID P N 5711020 9 25 mm ID P N FM100231 Entrance cone 6 07 mm ID P N FM5711000 Cone wash nozzle 3 68 mm ID P N FM101464 ESI probe assembly 3 0 mm ID P N FM5711933 3 0 mm ID P N FM5711933 47 22 mm ID P N FM103048 13 87 mm ID P N FM101417 9 12 mm ID P N 00107 01 00026 12 42 mm ID P N FM101522 Probe mount assembly 3 3 mm ID P N FM103016 ...

Page 127: ...30 Thumbnuts source block FM101528 Hexapole screws 60111 20055 Tubing 6 mm OD PTFE for nitrogen line order by the foot length 00109 99 00004 Kits Kit tool Surveyor MSQ 60111 62100 Kit Surveyor MSQ Plus installation 60111 62006 Kit sensitivity test Surveyor MSQ system FM104284 Qualification OPTON 00915 Software CD kit MSQ Plus OPTON 20432 Source Block Assembly Figure 82 contains an exploded view of...

Page 128: ...01417 O ring 12 42 mm ID 1 78 mm THK BS014 BLK VITON FM101522 O ring 9 0 mm ID 3 0 mm THK BLK VITON 00107 01 00026 O ring 47 22 mm ID 3 53 mm THK BS225 BLK VITON FM103048 O ring 3 68 mm ID 1 78 mm THK BS007 BLK VITON for cone wash nozzle FM101464 Plug source block sealing FM101460 Screw M3 10 cap head stainless steel FM103046 Screw hexapole 60111 20055 Source block FM102279 Spring 00111 01 00013 ...

Page 129: ...01464 Plug sealing P N FM101460 O ring 3 0 mm ID 1 0 mm THK P N 5711933 O ring BS225 47 2 mm ID 3 5 mm THK P N FM 103048 Extraction cone insulator P N FM102264 Exit cone P N FM102263 Hexapole screw insulator P N FM102248 O ring 9 0 mm ID 3 0 mm THK P N 00107 01 0026 O ring BS207 13 87 mm ID 3 53 mm THK P N FM101417 O ring BS014 12 42 mm ID 1 78 mm THK P N FM101522 Plug source block sealing P N FM1...

Page 130: ...0231 O ring 5 28 mm ID 1 78 mm THK BS009 BLK VITON 5711020 PEEK tube insert FM102591 Screw M3 8 cap head stainless steel 10 each N A Screw M3 10 cap head stainless steel FM103046 Capillary retaining nut FM102590 Figure 83 ESI probe Assembly exploded view Graphite Vespel ferrule P N 6070119 M3 10 cap head screw P N FM103046 Locking plate ESI capillary P N FM102598 ESI mount sub assembly O ring BS00...

Page 131: ... ring 5 28 mm ID 1 78 mm THK BS009 BLK VITON 5711020 PEEK tube insert 12 each FM102591 Screw M3 8 cap head stainless steel 10 each N A Screw M3 10 cap head stainless steel FM103046 Figure 84 APCI probe assembly exploded view Graphite Vespel ferrule P N 6070119 M3 10 cap head screw P N FM103046 Probe clamp APCI capillary P N FM102594 APCI probe mount sub assembly Locking plate O ring BS012 P N FM10...

Page 132: ...air Kit P N 60111 62010 Probe heater assembly 60111 60023 Detent screw insulator FM102585 Spring screw FM102583 Spring cup FM102584 Probe screw sleeve FM102582 O ring 18 77 mm ID 1 78 mm THK BS018 BLK VITON 5711035 Figure 85 Probe heater assembly with a view of the O rings O ring BS018 18 77 mm ID 1 78 mm THK P N 5711035 Detent screw insulator P N FM102585 O ring BS006 2 9 mm ID 1 78 THK P N TORN0...

Page 133: ...100203 Vent valve with 1 m cable assembly FM104308 Hose blue exhaust 1 in ID order by the foot length 10 10 ft 00301 08301 Gas Flow Spares and Nitrogen Generator Flow controller Legris FM100205 Tubing 6 mm OD PTFE for nitrogen line order by the foot length 00109 99 00004 Nitrogen valve assembly 60111 60019 PEAK nitrogen generator OPTON 97104 Spring screw P N FM102583 Not provided in the kit Spring...

Page 134: ...020 PCB source 60111 61030 PCB RF generator 60111 61040 PCB digital 60111 61050 PCB RF dc prefilter 60111 61080 Connection Kits LC Devices supports liquid chromatographs manufactured by Agilent and Thermo Fisher Scientific To connect an Agilent liquid chromatograph to your Surveyor MSQ Plus MS detector order the appropriate kit listed below Ethernet Communication Kit for Agilent 1100 LC system OPT...

Page 135: ...ion modes require different flow rates and column IDs The following guidelines apply when using the Surveyor MSQ Plus MS detector Electrospray can operate at all the flow rates described in Table 8 APCI cannot operate at flow rates below 0 2 mL min Therefore suitable column IDs are 2 1 mm 3 9 mm and 4 6 mm Contents Flow Rates LC Solvents and Mobile Phase Additives Cone Wash System Flow Splitting P...

Page 136: ...l for LC MS When using high percentages of water the probe temperature usually needs to be raised to aid desolvation Solvents that are less commonly used include Normal phase solvents Alcohols such as isopropanol 2 methoxyethanol ethanol and so on Dimethyl sulfoxide DMSO Normal phase solvents such as dichloromethane hexane and toluene are most suitable for use in APCI Alcohols have all been used w...

Page 137: ...hydroxide ammonia solution is suitable for increasing the pH of the mobile phase which can enhance LC separations When analyzing weakly acidic compounds in negative ion mode it is unlikely that there will be any suppression of ionization Volatile salts such as ammonium acetate or ammonium formate are often used to buffer mobile phases Use as little ammonium acetate or ammonium formate as possible ...

Page 138: ...suppression of sensitivity in positive ion mode TFA might completely suppress ionization in negative ion mode Triethylamine TEA can suppress the ionization of less basic compounds in positive ion mode as it also is readily ionized to give a M H ion at m z 102 TEA enhances ionization of other compounds in negative ion mode because it is basic This is a particularly useful additive for the analysis ...

Page 139: ...tem of the Surveyor MSQ Plus MS detector allows routine LC MS with chromatographic buffers such as phosphates or ion pairing agents and samples in dirty matrices The cone wash system consists of a cone wash nozzle internal tubing and a cone wash pump Refer to your Surveyor MSQ Plus Getting Connected manual for instructions on connecting the cone wash pump to the Surveyor MSQ Plus MS detector The r...

Page 140: ...greater than the backpressure exerted by the connection to the UV detector the flow to the API source probe is lower than the flow to the UV detector PEEK Tubing PEEK Poly Ether Ether Ketone tubing is a widely used alternative to stainless steel tubing in the high pressure parts of the system It is compatible with most LC solvents except THF tetrahydrofuran methylene chloride and concentrated nitr...

Page 141: ...gether to raise the blade b Insert your tubing through the appropriate guide hole c Release the tabs allowing the blade of the cutter to rest on the tubing d Holding the tubing spin the cutter around the tubing to begin the cut For PEEK tubing spin the cutter two to three times then remove the tubing and snap the tubing at the cut 2 Slip a fitting over the end of the tubing 3 As you insert PEEK tu...

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Page 143: ...CI probe removal 67 cleaning the entrance cone 80 85 disassembling the source block assembly 88 ESI probe removal 56 forepump power cord 33 removing the heater 73 removing the source block 79 Cautions phosphoric acid 122 tetrahydrofuran THF 122 changing ionization mode APCI to ESI 53 ESI to APCI 51 cleaning entrance cone 80 flushing capillaries 48 communications icon 43 computer features 38 cone w...

Page 144: ...embly 86 transfer lens 26 Tune window 42 USB connection 105 User I O 105 vacuum system 31 Xcalibur HomePage Roadmap view 39 firmware downloading the Surveyor MSQ firmware 21 versions for LC devices controlled by Xcalibur 38 flow rates columns 119 ESI mode 23 flow splitting procedure 124 forepump 32 checking the oil color 93 checking the oil level in the forepump 93 description 32 maintenance 93 ma...

Page 145: ...5 non volatile salts 121 normal phase solvents 120 Notes cone wash solvent 123 entering the needle voltage or corona current into a method 41 flushing the capillaries 48 forepump pump maintenance 93 O oil checking oil level in the forepump 93 checking the color of the oil in the forepump 93 purging volatile contaminants from the forepump oil 49 oil mist filter checking the oil level 46 Operate but...

Page 146: ...em 100 singly charged ions 4 7 software Xcalibur 38 solvent waste from autosampler 49 from MS detector 49 solvents compatibility with PEEK tubing 124 for liquid chromatography 120 solvents purity requirements xv source block allow to cool CAUTION 88 removing from the MS detector 85 replacing 91 source manifold 21 spares 111 spinning musical note icon 43 sulfuric acid 122 system shutdown emergency ...

Page 147: ...pump oil 49 voltages conversion dynode 28 electron multiplier cathode 29 W waste bottle for reference inlet system 17 waste solvent disposing 49 water 120 water vapor purging from forepump oil 49 X Xcalibur devices controlled by 15 Home Page 38 Instrument Configuration dialog box 15 introduction 38 launching 38 Server 39 turning off the MS detector from 98 ...

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