Waters Micromass ZQ 2000, Micromass ZQ 4000 Operator's Manual
W a ters Micromass
ZQ Detector
Operator’s Guide
34 Maple Street
Milford, MA 01757
71500044702, Revision B
NOTICE
The information in this document is subject to change without notice and should not be
construed as a commitment by Waters Corporation. Waters Corporation assumes no
responsibility for any errors that may appear in this document. This document is believed
to be complete and a c cu rate at th e time o f p u blication. In no event shall Water s
Corporation be liable for incidental or consequential damages in connec tion with, or
arising from, the use of this document.
© 2002 WATERS CORPORATION. PRINTED IN THE UNITED STATES OF AMERICA.
ALL RIGHTS RESERVED. THIS D OCUMENT OR PARTS THEREOF MAY NOT BE
REPRODUCED IN ANY FORM WITHOUT THE WRITTEN PERMISSION OF THE
PUBLISHER.
Alliance, Micromass, and Waters are registered trademarks, and Empower, ESCi,
MassLynx, and SAT/IN are trademarks of Waters Corporation.
Microsoft, Windows, and Windows NT are registered trademarks of Microsoft Corporation.
All other trademarks or registered trademarks are the sole property of their respective
owners.
When you use the instrument, follow generally accepted procedures for quality
Note:
control and methods development.
If you observe a change in the retention of a particular compound, in the resolution
between two compounds, or in peak shape, immediately determine the reason for the
changes. Until you determine the cause of a change, do not rely on the separation results.
The Installation Category (Overvoltage Category) for this instrument is Level II. The
Note:
Level II Category pertains to equipment that receives its electrical power from a local level,
such as an electrical wall outlet.
STOP
Atención:
responsible for compliance could void the user’s authority to operate the equipment.
Importan t :
par l’autorité responsable de la conformité à la réglementation peut annuler le droit de
l’utilisateur à exploiter l’équi pem ent .
Achtun g :
ausdrückliche Genehmigung der für die ordnungsgemäße Fun ktion stüchtigkeit
verantwortlichen Personen kann zum Entzug der Bedienungsbefugnis des Systems
führen.
Avvertenza:
espressamente approvate da un ente responsabile per la conformità annulleranno
l’autorità dell’utente ad operare l’apparecchiatura.
Atención:
expresamente aprobado por la parte responsable del cumplimiento puede anular la
autorización del usuario para utilizar el equip o.
Changes or modifications to this unit not expressly approved by the party
Toute modification sur cette unité n’ayant pas été expressément approuvée
Jedwede Änderungen oder Modifikationen an dem Gerät ohne die
eventuali modifiche o alterazioni apportate a questa unità e non
cualquier cambio o modificación efectuado en esta unidad que no haya sido
Caution:
Use caution when working with any polymer tubing under pressure:
• Always wear eye protection when near pressurized polymer tubing.
• Extinguish all nearby flames.
• Do not use Tef zel tubing tha t has been severely stressed or kinked.
• Do not use Tefz el tubing with tetrahydrofuran (THF) or concentrated nitric or
sulfuric acids.
• Be aware that methylene chloride and dimethyl sulfoxide cause Tefzel tubing to
swell, which greatly reduces the rupture pressure of the tubing.
Attention :
Soyez très prudent en travaillant avec des tuyaux de polymères sous
pression :
• Portez toujours des lunettes de protection quand vous vous trouvez à proximité de
tuyaux de polymères.
• Eteignez toutes les flammes se trouvant à proximité.
• N'utilisez pas de tuyau de T efzel fortement abîmé ou déformé.
• N'utilisez pas de tuyau de Tefzel avec de l'acide sulfurique ou nitrique, ou du
tétrahydrofurane (THF).
• Sachez que le chlorure de méthylène et le sulfoxyde de diméthyle peuvent
provoquer le gonflement des tuyaux de Tefzel, diminuant ainsi fortement leur
pression de rupture.
Vorsicht:
Bei der Arbeit mit Polymerschläuchen unter Druck ist besondere Vorsicht
angebracht:
• In der Nähe von unter Druck stehenden Polymerschläuchen stets Schutzbrille
tragen.
• Alle offenen Flammen in der Nähe löschen.
• Keine T e fzel-Schläuche verwenden, die stark geknickt oder überbeansprucht sind.
• Tef zel-S chläuche nicht für Tetrahydrofuran (THF) oder konzentrierte Salpeteroder Schwefelsäure verwenden.
• Durch Methylenchlorid und Dimethylsulfoxid können Tefzel-Schläuche quellen;
dadurch wird der Berstdruck des Schlauches erheblich reduziert.
Precauzio ne :
prestare attenzione durante le operazioni con i tubi di polimero sotto
pressione:
• Indossare sempre occhiali da lavoro protettivi nei pressi di tubi di polimero
pressurizzati.
• Estinguere ogni fonte di ignizione circostante.
• Non utilizzare tubi Tefzel soggetti a sollecitazioni eccessive o incurvati.
• Non utilizzare tubi Tefzel contenenti tetraidrofurano (THF) o acido solforico o
nitrico concentrato.
• Tenere presente che il cloruro di metilene e il dimetilsolfossido provocano
rigonfiamento nei tubi Tefzel, che riducono notevolmente il limite di pressione di
rottura dei tubi stessi.
Advertencia:
manipular con precaución los tubos de polímero bajo presión:
• Protegerse siempre los ojos en las proximidades de tubos de polímero bajo
presión.
• Apagar todas las llamas que estén a proximidad.
• No utilizar tubos Tef zel que hayan sufri do tensiones extrem as o hayan sido
doblados.
• No utilizar tubos Tefzel con tetrahidrofurano (THF) o ácidos nítrico o sulfúrico
concentrados.
• No olvidar que el cloruro de metileno y el óxido de azufre dimetilo dilatan los tubos
Tefzel, lo que reduce en gran medida la presión de ruptura de los tubos.
Caution:
The user shall be made aware that if the equipment is used in a manner not
specified by the manufacturer, the protection provided by the equipment may be
impaired.
Attention :
L’utilisateur doit être informé que si le matériel est utilisé d’une façon non
spécifiée par le fabricant, la protection assurée par le matériel risque d’être
défectueuses.
Vorsicht:
Der Benutzer wird darauf aufmerksam gemacht, dass bei unsachgemäßer
Verwenddung des Gerätes unter Umständen nicht ordnungsgemäß funktionieren.
Precau zion e :
l’utente deve essere al corrente del fatto che, se l’apparecchiatura viene
usta in un modo specificato dal produttore, la protezione fornita dall’apparecchiatura
potrà essere invalidata.
Adver tenc ia:
el usuario deberá saber que si el equipo se utiliza de forma distinta a la
especificada por el fabricante, las medidas de protección del equipo podrían ser
insuficientes.
Caution:
rating.
To protect against fire hazard, replace fuses with those of the same type and
Attention :
Remplacez toujours les fusibles par d’autres du même type et de la même
puissance afin d’éviter tout risque d’incendie.
Vorsicht:
Zum Schutz gegen Feuergefahr die Sicherungen nur mit Sicherungen des
gleichen Typs und Nennwertes ersetzen.
Precauzio ne :
per una buona protezione contro i rischi di incendio, sostituire i fusibili con
altri dello stesso tipo e amperaggio.
Advertencia:
sustituya los fusibles por otros del mismo tipo y características para evitar
el riesgo de incendio.
Caution:
To avoid possible electrical shock, disconnect the power cord before servicing
the instrument.
Attent i on :
Afin d’éviter toute possibilité de commotion électrique, débranchez le cordon
d’alimentation de la prise avant d’effectuer la maintenance de l’instrument.
Vorsicht:
Zur Vermeidung von Stromschlägen sollte das Gerät vor der Wartung vom
Netz getrennt werden.
Precauzio ne :
per evitare il rischio di scossa elettrica, scollegare il cavo di alimentazione
prima di svolgere la manutenzione dello strumento.
Precaución:
para evitar descargas eléctricas, desenchufe el cable de alimentación del
instrumento antes de realizar cualquier reparación.
Commonly Used Symbols
Direct current
Courant continu
Gleichstrom
Corrente continua
Corriente continua
Alternating current
Courant alternatif
Wechselstrom
Corrente alternata
Corriente alterna
Protective conductor terminal
Borne du conducteur de protection
Schutzleiteranschluss
Ter m ina le di conduttore con protezione
Borne del conductor de tierra
Commonly Used Symbols (Continued )
Frame or chassis terminal
Borne du cadre ou du châssis
Rahmen- oder Chassisanschluss
Ter m ina le di struttura o telaio
Borne de la estructura o del chasis
Caution or refer to manual
Attention ou reportez-vous au guide
Vorsicht, oder lesen Sie das Handbuch
Prestare attenzione o fare riferimento alla guida
Actúe con precaución o consulte la guía
Caution, hot surface or high temperature
Attention, surface chaude ou température élevée
Vorsicht, heiße Oberfläche oder hohe T emperatur
Precauzione, superficie calda o elevata temperatura
Precaución, superficie caliente o temperatura elevada
Commonly Used Symbols (Continued )
Caution, risk of electric shock (high voltage)
Attention, risque de commot ion électri que (haut e tension )
Vorsicht, Elektroschockgefahr (Hochspannung)
Precauzione, rischio di scossa elettrica (alta tensione)
Precaución, peligro de descarga eléctrica (alta tensión)
Caution, risk of needle-stick puncture
Attention, risques de perforation de la taille d’une aigui lle
Vorsicht, Gefahr einer Spritzenpunktierung
Precauzione, rischio di puntura con ago
Precaución, riesgo de punción con aguja
Caution, ultraviolet light
UV
Attention, rayonnement ultrviolet
Vorsicht, Ultraviolettes Licht
Precauzione, luce ultravioletta
Precaución, emisiones de luz ultravioleta
Commonly Used Symbols (Continued )
Fuse
Fusible
Sicherung
Fusibile
Fusible
1
0
Electrical power on
Sous tension
Netzschalter ein
Alimentazione elettrica attivata
Alimentación eléctrica conectada
Electrical power off
Hors tension
Netzschalter aus
Alimentazione elettrica disat tivata
Alimentación eléctrica desconectada
Waters Micromass ZQ Detector Information
Intended Use
Waters designed the Waters® Micromass® ZQ™ Detector to with an HPLC system to
determine mass-to-charge ratio (m/z) for a wide range of analytes.
Biological Hazard
When you analyze physiological fluids, take all necessary precautions and treat all
specimens as potentially infectious. Precautions are outlined in “CDC Guidelines on
Specimen Handling,” CDC – NIH Manual, 1984.
Calibration
Follow the calibration methods set forth in this guide, using pure standards. The
concentration range should cover the entire range of quality-control samples, typical and
atypical specimens.
Quality Control
Routinely run three quality-control samples. Quality-control samples should represent
subnormal, nor m al, and above-norm al levels of a compound. Ensure that quality-control
sample results are within an acceptable range, and ev aluate precision from day to day and
run to run. Data collected when quality-control samples are out of range may not be valid.
Table of Contents
Preface ....................................................................................... 23
Chapter 1
Overview ........ .............. .............. ............... ......... ............... .............. . 27
1.1 About the Micromass ZQ Detector........................................ 27
1.2 Theory and Principles of Operation ...................................... 28
1.3 MassLynx 4.0 Software......................................................... 29
Chapter 2
Installing .......................................................................................... 30
2.1 Site Selection and Power Requirements............................... 31
2.2 Unpacking and Inspecting..................................................... 32
2.3 Installing the Detector ........................................................... 33
2.3.1 Installing the Rotary Pump ........................................ 33
2.3.2 Installing the Oil Return Connection Kit..................... 34
2.3.3 Connecting the Nitrogen Supply and Exhaust........... 35
2.3.4 Connecting the Rheodyne Injector (for Manual
Injections).................................................................. 37
2.3.5 Installing the ESI Probe............................................. 38
2.3.6 Connecting the Workstation....................................... 39
2.3.7 Preparing the Syrin ge an d Syringe Pump ................. 40
Table of Contents 15
Chapter 3
Tuning ............................................................................................ 41
3.1 Opening MassLynx and Starting the Instrument................... 41
3.2 Tuning in ESI Mode............................................................... 43
3.2.1 Specif ying Parameter Settin gs on the ES+
Source Page....................... ..... .... ..... ..... ................... . 44
3.2.2 Specif ying Parameter Settin gs on the
Analyser Page ........................................................... 46
3.3 Tuning in APCI Mode ............................................................ 47
3.3.1 Preparing the Source for APCI Operation ................. 48
3.3.2 Installing the Tee Fitting............................................. 49
3.3.3 Specifying Parameters on the APCI+ Source
Page.......................................................................... 49
3.4 Readbacks............................................................................ 52
Chapter 4
Calibrating ....................................................................................... 54
4.1 Setting Up the Calibration File.............................................. 54
4.2 Setting Calibration Parameters ............................................. 55
4.2.1 Tune Window Setting s ............. .... .................... .... ..... . 55
4.2.2 Instrum en t Thresh old Settin gs Dialog Box ...... .... ..... . 58
4.2.3 Automatic Calibration Check Dialog Box ................... 59
4.2.4 Calibration Parameters Dialog Box............................ 60
4.2.5 Mass Measure Dialog Box......................................... 62
4.2.6 Automatic Calibration Dialog Box .............................. 63
4.2.7 Calibration Acquisition Dialog Box............................. 64
Table of Contents 16
Chapter 5
Maintaining ...................................................................................... 73
5.1 Considerations...................................................................... 73
5.2 Routine Maintenance............................................................ 75
5.2.1 Checking the Rotary Pump Oil .................................. 75
5.2.2 Replacing the Pump Oil............................................. 75
5.2.3 Gas-Ballasting the Rotary Pump............................... 78
5.2.4 Replacing the Oil Mist Filter....................................... 79
5.2.5 Cleaning the Source Assembly.................................. 80
5.2.6 Cleaning the APCI Probe Tip..................................... 91
5.2. 7 Cleaning and Replacing th e Corona Discharge
Needle....................................................................... 91
5.3 Replacing Parts..................................................................... 92
5.3.1 Replacing the Ion Block Cartridge Heater................. 92
5.3.2 Replacing the Stainless Steel Capillary..................... 93
5.3.3 Replacing the ESI Probe Tip ..................................... 95
5.3.4 Replacing the APCI Fused Silica Capillary and
Filter Pad.................. ..... ..... ..... ................... ..... .... ..... . 96
5.3.5 Replacing the APCI Probe Heater............................. 98
Chapter 6
Troubleshooting ............................................................................... 99
6.1 Safety and Handling.............................................................. 99
6.2 Component Hardware Troubleshooting............................... 101
6.3 Inspecting the APCI Probe.................................................. 107
Table of Contents 17
Appendix A
Using the ESCi Multi-Mode Ionization Source................................ 108
A.1 Preparing for Oper ation . ..... ..... ................... ..... ..... ..... ........ 108
A.1.1 Installing the Corona Discharge Needle.................. 108
A.1.2 Setting Up MassLynx .............................................. 110
A.2 Daidzein Test ... ..... ..... .... ..... ..... ..... ................... ..... ..... .... .... 117
A.2.1 Test Conditions ...................................................... 118
A.2.2 Signal-to-Noise Ratio .............................................. 118
Appendix B
Specifications ................................................................................. 119
B.1 ZQ Detector Specifications ................................................ 119
B.2 ESCi Multi-Mode Ionization Source Specifications ........... 121
Appendix C
Accessories and Spare Parts ......................................................... 122
Index ..................................................................................... 129
Table of Contents 18
List of Figures
2-1 Installing the Detector....................................................................30
2-2 Pump Oil Level...............................................................................33
2-3 Fitting the Gas Ballast and Hose adaptors to the Rotary Pump.... 35
2-4 ZQ Detector Rear Panel ................................................................36
2-5 Nitrogen Stud.................................................................................36
2-6 Drying Gas Exhaust Bottle ............................................................37
2-7 Rheodyne Injector........... ......... ......... .......... ......... ..........................38
2-8 ESI Probe in Situ...........................................................................39
2-9 Syringe Pump................................................................................40
3-1 MassLynx Login Dialog Box...........................................................41
3-2 MassLynx Main Window................................................................ 42
3-3 Tune Window Displaying the ES+ Source Page ............................ 43
3-4 Syringe Selection Dialog Box ........................................................45
3-5 Tune Window Displaying the Analyser Page..................................47
3-6 Combined Flow into the Tee..........................................................49
3-7 Tune Window Displaying the APCI+ Source Page.........................50
3-8 Readbacks Dialog Box................................ ...................................52
3-9 Diagnostics Page Readbacks........................................................53
4-1 Calibration Window........................................................................54
4-2 Open Dialog Box............................................................................55
4-3 Tune Window Displaying the ES+ Source Page ............................ 57
4-4 Tune Window Displaying Analyser Page Parameters....................58
4-5 Instrument Threshold Settings Dialog Box ....................................59
4-6 Automatic Calibration Check Dialog Box.......................................59
4-7 Calibration Pa rameters Dialog Box................................................60
4-8 Mass Measure Dialog Box.............................................................62
4-9 Automatic Calibration Dialog Box ..................................................63
4-10 Calibration Acquisition Setup Dialog Box ......................................65
List of Figures 19
4-11 Display Calibration Graphs Dialog Box..........................................67
4-12 Calibrate Window Showing ZQ-4000 Calibration Graphs..............69
5-1 Rotary Pump Assembly Fitted with Oil Mist Filter..........................76
5-2 Rotary Pump Oil Filler Plug, Drain Plug, and Sight Glass.............77
5-3 Isolation Valve................................................................................79
5-4 Oil Mist Filter Assembly.................................................................80
5-5 Pumping Block Assembly..............................................................82
5-6 Ion Block Assembly .......................................................................83
5-7 Probe Assembly in Position on the Source ....................................84
5-8 ZQ Detector Front View.................................................................85
5-9 Source Showing the Corona Discharge Needle............................86
5-10 Ion Block........................................................................................86
5-11 Sample Cone and Cone Gas Nozzle.............................................87
5-12 Ion Block Rear View ......................................................................88
5-13 Hexapole Assembly.......................................................................89
5-14 Ion Block Cartridge Heater............................................................92
5-15 Replacing the Heater Car tridge.....................................................93
5-16 ESI Probe Tip with Capillary Protruding 0.5 mm...........................95
A-1 ZQ Mass Detector, Front View ...................................................109
A-2 Installing the Corona Needle ...................................................... 110
A-3 Tune Window ..............................................................................110
A-4 Tune Window Showing Options List with ESCi Mode Selected .111
A-5 Tune Window, Diagnostics Page ................................................112
A-6 Selecting the ESCi+ or ESCi- Ionization Mode ...........................112
A-7 Selecting the Ion Mode in the MassLynx Peak Editor ................ 113
A-8 Tune Window as it Appears During ESCi Operation ..................114
A-9 Function List Editor Window (Blank) ...........................................115
A-10 Function:n MS Scan Dialog Box ................................................. 115
A-11 Function List Editor Window Showing Specified Functions ........116
A-12 ESCi Mode Disabled ...................................................................117
A-13 Daidzein (m/z = 255.2 [M + H] and 253.2 [M – H]) ..................... 117
List of Figures 20
List of Tables
2-1 Installation Site Requirements ......................................................31
3-1 ES+ Source Page Parameters ......................................................43
3-2 Source and Desolvation Temperature Settings........................ 44
3-3 Analyser Page Parameters...................................................... 46
3-4 APCI+ Source Page Parameters ............................................. 49
4-1 Recommended Calibration Acquisitions Setup Parameters ......... 65
4-2 Calibration Failure Troubleshooting ......................................... 69
5-1 Maintenance Schedule .................................................................74
6-1 Hardware Troub lesh ooting .................................. ......... ............... 101
A-1 HPLC Conditions ........................................................................118
A-2 MS Conditions ............................................................................ 118
B-1 ZQ Detector Operational Specifications .....................................119
B-2 ZQ Detector Environmental Specifications................................. 120
B-3 ZQ Detector Dimensions ............................................................ 120
B-4 ZQ Detector Electrical Specifications......................................... 120
B-5 ESCi Environmental Specifications............................................ 121
B-6 ESCi Electrical Specifications..................................................... 121
C-1 Fuses .......................................................................................... 122
C-2 Probe Components..................................................................... 122
C-3 Vacuum Components................................................................. 123
C-4 Valves and Flow Meters ............................................................. 124
C-5 Kits........................................... ..................................... .......... .... 125
C-6 Power Supplies........................................................................... 125
List of Tables 21
C-7 Source and Analyser Components............................................. 126
C-8 Washers, Screws, and Nuts....................................................... 127
C-9 Miscellaneous Components........................................................ 128
List of Tables 22
Preface
The Waters Micromass ZQ Detector Operator’s Guide descr ibe s procedures for
unpacking, installing, using, mai nta ining, and troubleshooting the Waters
ZQ™ Detector. Its appendixes ex pl ain how to use the optional ESCi™ Multi-Mode
Ionization Source, and list instrument specifications, accessories, and spare part s.
This guide is intended for individuals who need to install, operate, maintain, and/or
troubleshoot the Micromass
ZQ Detector.
®
Organization
This guide contains the following:
Chapter 1
Chapter 2
liquid line, gas, signal, and other hardware connections.
Chapter 3
calibrate it.
Chapter 4
in MassLynx™.
Chapter 5
Chapter 6
Appendix A
describes the instrument, including its features and options.
describes how to unpack and install the instrument and how to make power ,
describes how to configure the instrument, start it operating, and tune and
describes how to set up a calibration file and specify calibration parameters
explains routine maintenance procedures.
describes troubleshooting procedures.
explains how to use the ESCi Multi-Mode Ionization Source option.
Micromass®
Appendix B
Appendix C
presents instrument specifications.
lists recommended and optional accessories and spare parts.
Related Documentation
Waters Licenses, Warranties, and Support: Provides software license and warranty
information, describes training and extended support, and tells how Waters handles
shipments, damages, claims, and returns.
Online Documentation
MassLynx Help
dialog boxes f or the base software and software options. Also includes reference
information and procedures for performing all tasks required to use MassLynx software.
Included as part of the MassLynx software.
: Describes all MassLynx windows, menus, menu selections, and
23
Printed Doc um entation for Base Product
MassLynx User’ s Guide
MassLynx Interfacing Guide
MassLynx Security User’s Guide
MassLynx 4.0 Guide to Inlet Control
MassLynx 4.0 Guide to ZQ Data Acquisition
Wate rs Micro mass ZQ wit h MassLynx v4.0 Software a nd Instrument Verification
Procedure
Related Adobe Acrobat Reader Documentation
For detailed information about using Adobe® Acrobat® Reader, see the Adobe Acrobat
Reader Online Guide. This guide covers procedures such as viewing, navigating, and
printing electronic documentation from Adobe Acro bat Reader.
Printing This Electro nic Docu men t
Adobe Acrobat Reader lets you easily print pages, page ranges, or the entire document by
selecting File > Print. For optimum print quantity, Waters recommends that you specify a
PostScript
resolution.
®
printer driver for your printer. Ideally, use a printer that supports 600 dpi print
Documentation Conventions
The following conventions can be used in this guide:
Convention Usage
Purple
Italic Italic indicates information that you supply such as variables. It also
Courier
Courier Bold
Purple text indicates user action such as keys to press, menu selections, and commands. For example, “Click Next to go to the next
page.”
indicates emphasis and document titles. For example, “Replace
file_name with the actual name of your file.”
Courier indicates examples of source code and system output. For
example, “The SVRMGR> prompt appears.”
Courier bold indicates characters that you type or ke ys you press in
examples of source code. For example, “At the LSNRCTL> prompt ,
enter set password oracle to access Oracle.”
24
Convention Usage
Underlined Blue I ndi cates hypert ext cross-references to a specific chapter, section,
subsection, or sidehead. Clicking this topic using the hand symbol
brings you to this topic within the document. Right-clicking and
selecting Go Back from the shortcut menu returns you to the origi-
nating topic. For example, “Monitoring Readbacks are described in
Section 3.4,
Keys T he word key refers to a computer key on the keypad or keyboard.
Screen keys ref er to the ke ys on the instrument located immediately
below the screen. For example, “The A/B screen key on the 2414
Detector displays the selected channel.”
… Three periods indicate that more of the same type of item can
optionally follow. For e xample, “You can store filename1, filename2,
… in each folder.”
>
Notes
Notes call out information that is helpful to the operator. For example:
Record your result before you proceed to the next step.
Note:
A right arrow between menu options indicates you should choose
each option in sequence. For example, “Select File > Exit” means
you should select File from the menu bar, then select Exit from the
File menu.
Readbacks”
Attentions
Attentions provide information about preventing damage to the system or equipment. For
example:
To avoid damaging the detector flow cell, do not touch the flow cell
STOP
Attention:
window.
25
Cautions
Cautions provide information essential to the safety of the operator. For example:
Caution:
To avoid burns, turn off the lamp at least 30 minutes before removing it for
replacement or adjustment.
Caution:
To avoid electrical shock and injury, unplug the power cord before
performing maintenance procedures.
Caution:
To avoid chemical or electrical hazards, observe safe laboratory practices
when operating the system.
26
Chapter 1 Ov erview
This chapter describes the Waters® Micromass® ZQ™ Detector, its features and options.
1.1 About the Micromass ZQ Detector
The ZQ Detector is a quadrupole mass analyser that can determine the mass-to-charge
ratio (m/z) of diverse analytes. An HPLC system, or syringe pump, delivers liquid sample
to the instrument’s analyser source. There the sample molecules ionize by means of one
of two ionization modes: electrospray (ESI) or atmospheric pressure chem ical ionization
(APCI). In ESI mode, sample molecules ionize in solution before they reach the source.
On entering the ev acuated source, they begin a desolvation process. In APCI mode, an
electrical discharge inside the source ionizes the sample molecules whereupon they
undergo desolvation.
The ions ultimately reach the quadrupole, which separates them according to their
mass-to-charge ratios. A photomultiplier then detects the mass-separated ions, amplifies
their signals, and sends the mass information to the data syst em.
Probes
An electrospray ionization (ESI) probe or an atmospheric pressure chemical ionization
(APCI) probe introduces the sample to the ion source.
1
Sample Inlet
Either of two methods deliver solvent and sample to the installed probe:
• An HPLC system – Delivers the eluent from an HPLC analysis.
• A built-in syringe pump – Delivers standard solutions or infusions of unknown
samples.
Vacuum System
An external rotary (roughing) pump and an internal split flow turbomolecular pump
combine to create the source vacuum. The turbomolecular pump evacuates the analyser
and ion transfer region.
Vacuum leaks and electrical or vacuum pump failures cause vacuum loss, which
protective interlocks guard against. The system monitors turbomolecular pump speed and
About the Micromass ZQ Detector 27
continuously measures vacuum pressure with a built-in Pirani gauge. The gauge also
serves as a switch, discontinuing detector operation when it senses vacuum loss.
A vacuum isolation valve isolates the source from the mass analyser, allo wing routine
source maintenance without venting.
Mass Analyser (Quadrupole)
The mass analyser separates ions by mass-to-charge ratio (m/z).
Data System
The data system collects information from the mass analyser and includes these
components:
• MassLynx™ 4.0 software
• An external workstation
• An embedded PC
MassLynx software controls the workstation-based data system and mass detector
through the detector’s embedded PC. Using MassLynx, you tune the instrument, set up
and run the HPLC system, and acquire and process data. When they are part of the
system, the software also controls the autosampler and the divert and injector valves.
The workstation uses a Windows NT
environment and allows full user interaction with the keyboard or mouse. A network link
communicates between the workstation and the detector’s embedded PC.
®
, Windows® 2000, or Windows XP color graphical
1
MassLynx acquires and stores data from conventional LC detectors simultaneously with
data the mass detector acquires. It can also acquire data from selected systems, like
Waters 996/2996 Photodiode Array Detectors. Consult the MassLynx 4.0 Guide to Inlet
Control for details about MassLynx.
1.2 Theory and Principles of Operation
Electrospray Ionization (ESI)
In ESI, a high electrical voltage charges the eluent as it emerges from a nebulizer,
producing an aerosol of charged droplets. As the solvent evaporates, the droplets shrink,
developing a charge dense enough to eject ions from their s urfaces (ion evaporation). The
mass analyser then sorts the singly or multiply charged ions by mass-to-charge m/z ratio.
The analyser source can accommodate eluent flows of up to 1 mL/min. You can enhance
performance by reducing the rate of eluent flow at the ion source.
Overview 28
Atmospheric Pressure Chemical Ionization (APCI)
A heated nebulizer vaporizes the sample. The sample ions then merge with solvent ions in
the atmospheric source, enabling proton transfers between the solvent and sample ions.
APCI generally produces both protonated and deprotonated molecular ions from the
sample. For positive ions, this ionization occurs by means of a proton transfer mechanism.
For negative ions, the mechanism is proton abstraction.
1.3 MassLynx 4.0 Software
MassLynx 4.0 software permits these major operations:
• Configuring the instrument
• Creating HPLC inlet and MS methods that define operating parameters for a run
• Tuning and calibrating the mass detector
• Running samples
• Monitoring the run
• Acquiring data
• Processing data
• Reviewing data
• Printing data
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See the MassLynx 4.0 Guide to Inlet Control and MassLynx Help for more information on
installing and using MassLynx software.
MassLynx 4.0 Software 29
Chapter 2 Installing
This chapter describes how to unpack and install your Waters Micromass ZQ Detector.
Figure 2-1
summarizes these procedures.
Installation
Begins
Select and Prepare
Appropriate Site
Unpack and Inspect
Install Rotary Pump
Install Oil Retur n
Connection Kit
Connect N2 and
Exhaust
Connect Rheodyne
Injector Tubing
Install
ESI Probe
Connect
Workstation
Set Up
Syringe Pump
2
Figure 2-1 Installing the Detector
Installation
Complete
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