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Waters SQ Detector Quick Start Manual

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Waters SQ Detector
Quick Start Guide
71500126603 Revision F
Copyright © Waters Corporation 2006–2010
All rights reserved

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  • Page 1 Waters SQ Detector Quick Start Guide 71500126603 Revision F Copyright © Waters Corporation 2006–2010 All rights reserved...

  • Page 2: Copyright Notice

    Corporation assumes no responsibility for any errors that may appear in this document. This document is believed to be complete and accurate at the time of publication. In no event shall Waters Corporation be liable for incidental or consequential damages in connection with, or arising from, its use.

  • Page 3: Customer Comments

    Contacting Waters ® Contact Waters with enhancement requests or technical questions regarding the use, transportation, removal, or disposal of any Waters product. You can reach us via the Internet, telephone, or conventional mail. Waters contact information Contacting medium Information...

  • Page 4: Safety Considerations

    Considerations specific to the SQ Detector Solvent leakage hazard The source exhaust system is designed to be robust and leak-tight. Waters recommends you perform a hazard analysis, assuming a maximum leak into the laboratory atmosphere of 10% LC eluate.
  • Page 5 High temperature hazard To avoid burn injuries, avoid touching the source enclosure Warning: with your hand when operating or servicing the instrument. SQ Detector high temperature hazard Source enclosure assembly PO W ER O PER ATE NEBULIZER NEBULIZER DESOLVATION DESOLVATION...
  • Page 6 High voltage hazard Warning: • To avoid electric shock, do not remove the SQ Detector’s protective panels. The components they cover are not user-serviceable. • To avoid non-lethal electric shock, any equipment connected to the ESI and IonSABRE™ APCI probes must be grounded.

  • Page 7: Operating This Instrument

    Consult instructions for use Intended use Waters designed the Single Quad (SQ) Detector for use as a research tool to deliver authenticated mass measurement in MS mode. The Single Quad (SQ) Detector is for research use only and is not intended for use in diagnostic applications.

  • Page 8: Quality Control

    When calibrating mass spectrometers, consult the calibration section of the operator’s guide for the instrument you are calibrating. In cases where an overview and maintenance guide, not operator’s guide, accompanies the instrument, consult the instrument’s online Help system for calibration instructions.

  • Page 9: Ism Classification

    Class A products are suitable for use in commercial (that is, nonresidential) locations and can be directly connected to a low voltage, power-supply network. EC authorized representative Waters Corporation (Micromass UK Ltd.) Floats Road Wythenshawe Manchester M23 9LZ United Kingdom...

  • Page 11: Table Of Contents

    Copyright notice ....................ii Trademarks ......................ii Customer comments .................... iii Contacting Waters ....................iii Safety considerations ..................iv Considerations specific to the SQ Detector ............iv Safety advisories ....................vi Operating this instrument ................vii Applicable symbols ................... vii Intended use...................... vii Calibrating ......................
  • Page 12 MS operating modes ..................1-9 Sample inlet ......................1-9 Leak sensors ....................... 1-9 Vacuum system ....................1-9 Rear panel ......................1-10 IntelliStart Fluidics system ................1-11 Overview......................1-11 System operation ................... 1-12 2 Preparing for Operation ..............2-1 Starting the instrument .................. 2-2 Configuring IntelliStart...................
  • Page 13 Warning symbols ....................A-2 Task-specific hazard warnings................ A-2 Specific warnings ..................... A-3 Caution symbol ....................A-5 Warnings that apply to all Waters instruments ......... A-5 Electrical and handling symbols ..............A-11 Electrical symbols ..................A-11 Handling symbols ..................A-12 Table of Contents...
  • Page 14 Table of Contents...

  • Page 15: Waters Sq Detector

    Waters SQ Detector This chapter describes the instrument, including its controls and gas and plumbing connections. Contents Topic Page Overview Ionization techniques and source probes Ion optics MS operating modes Sample inlet Leak sensors Vacuum system Rear panel 1-10 IntelliStart Fluidics system...

  • Page 16: Overview

    (APCI) and electrospray ionization (ESI). Optional ionization modes are IonSABRE™ APCI and APPI (atmospheric pressure photoionization). For instrument specifications, see the Waters SQ Detector Site Preparation Guide. Waters SQ Detector TP02592 Waters SQ Detector...
  • Page 17 Waters SQ Detector, with doors open PO W ER O PER ATE DESOLVATION DESOLVATION NEBULIZER NEBULIZER APPI APPI PROBE PROBE IntelliStart technology IntelliStart™ technology monitors LC/MS performance and reports when the instrument is ready for use. The software automatically tunes and mass calibrates the instrument and displays performance readbacks.

  • Page 18: Acquity Sqd Uplc/Ms System

    The ACQUITY UPLC system includes a binary solvent manager, sample manager, column heater, optional sample organizer, optional detectors, and an ACQUITY UPLC column. WatersEmpower™ chromatography software or MassLynx mass spectrometry software controls the system. For further instruction, see the ACQUITY UPLC System Operator’s Guide or Controlling Contamination in LC/MS Systems (part number 715001307).

  • Page 19: Software And Data System

    Software and data system The instrument is controlled by either Empower chromatography software or MassLynx mass spectrometry software. Each is a high-performance application that acquires, analyzes, manages, and distributes ultraviolet (UV), evaporative light scattering, analog, and mass spectrometry data. Both Empower and MassLynx software enable these major operations: •...

  • Page 20: Ionization Techniques And Source Probes

    ESCi, the standard ESI probe is used in conjunction with a corona pin to allow alternating acquisition of ESI and APCI ionization data, facilitating high throughput and wider compound coverage. ESCi mode ESI probe tip RP00029 Corona pin Sample cone tip Waters SQ Detector...

  • Page 21: Atmospheric Pressure Chemical Ionization

    Atmospheric pressure chemical ionization A dedicated high-performance, atmospheric-pressure, chemical ionization (APCI) probe is offered as an option. Atmospheric pressure photoionization Atmospheric pressure photoionization (APPI) is offered as an option. It uses photons generated by a krypton-discharge ultraviolet (UV) lamp (10.2 eV) to produce sample ions from vaporized LC eluent.

  • Page 22: Ion Optics

    The transmitted ions are detected by the photomultiplier detection system. The signal is amplified, digitized, and sent to the Empower chromatography or MassLynx mass spectrometry software. Ion optics overview Sample cone Sample inlet Transfer optics Conversion dynode Isolation valve Z-Spray ion source Quadrupole Detector Waters SQ Detector...

  • Page 23: Ms Operating Modes

    Leak sensors Where fitted, leak sensors in the drip trays of the ACQUITY UPLC system and the SQ Detector continuously monitor system components for leaks. A leak sensor stops system flow when its optical sensor detects about 1.5 mL of accumulated, leaked liquid in its surrounding reservoir.

  • Page 24: Rear Panel

    V V A 900 PUMP PUMP API Gas API Gas Roughing pump 6.9 Bar Maximum 6.9 Bar Maximum relay switch Nitrogen inlet VACUUM VACUUM SOURCE VENT SOURCE VENT Source vent VACUUM VACUUM Turbo vacuum 01757 U.S.A. Source vacuum RP00001 1-10 Waters SQ Detector...

  • Page 25: Intellistart Fluidics System

    IntelliStart Fluidics system Overview The IntelliStart Fluidics system is built into the instrument. The system delivers sample directly to the MS probe in one of two ways: • From the LC column. • From two integral reservoirs. The integral reservoirs can also deliver sample through direct or Tip: combined infusion to enable optimization at analytical flow rates.

  • Page 26: System Operation

    You can edit the parameters, frequency, and extent of the automation you want IntelliStart to perform. See the instrument’s online Help for further details on IntelliStart software and operation of the instrument’s solvent delivery system. 1-12 Waters SQ Detector...

  • Page 27: Preparing For Operation

    Preparing for Operation This chapter describes how to start and shut-down the instrument. Contents Topic Page Starting the instrument Preparing the IntelliStart Fluidics system Rebooting the instrument 2-11 Leaving the mass spectrometer ready for operation 2-12...

  • Page 28: Starting The Instrument

    Using incompatible solvents can cause severe damage to the Caution: instrument. For more details, refer to the following sources: • Appendix C of the Waters SQ Detector Operator’s Guide for solvent information. • Appendix C of the ACQUITY UPLC System Operator’s Guide for on solvent compatibility with ACQUITY™.
  • Page 29 • After the instruments are successfully powered-on, all power LEDs show steady green. The binary solvent manager’s flow LED, the sample manager’s run LED, and the SQ Detector’s Operate LED remain off. Start Empower or MassLynx software. You can monitor the ACQUITY Console for messages and LED Tip: indications.

  • Page 30: Configuring Intellistart

    Click Configure > IntelliStart Configuration. In the IntelliStart Configuration dialog box, in the Checks list, select the check boxes for the items you want checked during SQ Detector startup. Clear the check boxes of items you do not want checked.

  • Page 31: Running The Instrument At High Flow Rates

    Running the instrument at high flow rates ACQUITY UPLC is run at high flow rates. To optimize desolvation, and thus sensitivity, you must run the ACQUITY SQD system at appropriate gas flows and desolvation temperatures. IntelliStart automatically sets these parameters when you enter a flow rate, according to the following table. Flow rate versus temperature and gas flow Flow rate Desolvation...

  • Page 32: Preparing The Intellistart Fluidics System

    Preparing the IntelliStart Fluidics system Installing the solvent manifold drip tray Required material Chemical-resistant, powder-free gloves To install the solvent manifold drip tray The solvent manifold drip tray can be contaminated Warning: with biohazardous and/or toxic materials. Always wear chemical-resistant, powder-free gloves while performing this procedure.

  • Page 33: Installing The Reservoir Bottles

    Installing the reservoir bottles An optional Low-volume Adaptor Kit is available for infusing smaller volumes. The low-volume vials have a volume of 1.5 mL. Required material Chemical-resistant, powder-free gloves To install the reservoir bottles The reservoir bottles can be contaminated with Warning: biohazardous and/or toxic materials.

  • Page 34: Diverter Valve Positions

    Screw the low-volume vial into the adaptor. TP02630 Diverter valve positions Column and syringe in home position after power-up After power-up, the flow path between the column and waste is open. The syringe is empty, and the flow path between it and waste is open. Probe Waste Idle...
  • Page 35 LC position In the LC position, the flow path between the LC and probe is open, and the flow path between the syringe and waste is also open. Probe Idle Column Syringe Waste Reservoir A Reservoir B Infusion position Probe Infusion Infusion Column...
  • Page 36 Combined position with LC flow and syringe in idle mode Probe Combined Idle Column Syringe Waste Reservoir A Reservoir B Waste position In the waste position, both the LC flow and the infusion syringe flow are directed to waste. The syringe mode can be only static or dispensing (that is, never drawing).

  • Page 37: Purging The Infusion Syringe

    Purging the infusion syringe Whenever you replace a solution bottle, purge the infusion syringe with the solution that you are going to use next. See the mass spectrometer’s online Help for details. Depending on the solutions used, the IntelliStart Fluidics system can Tip: require more than one purge cycle to minimize carryover.

  • Page 38: Leaving The Mass Spectrometer Ready For Operation

    Help for details. Emergency instrument shutdown To shut down the instrument in an emergency The SQ Detector’s power switch does not isolate the Warning: instrument from the main power supply. To isolate the instrument, you must disconnect the power cable from the back of the instrument.

  • Page 39: Esi And Esci Modes Of Operation

    ESI and ESCi Modes of Operation This chapter describes how to prepare the instrument for the following modes of operation: • ESI (electrospray ionization). • ESCi (combined electrospay and atmospheric pressure chemical ionization). If your system uses APCI mode, see Chapter “Optional APCI Mode of Operation”.

  • Page 40: Introduction

    Introduction The ESI and ESCi ionization mode options use the standard ESI probe that is fitted to the instrument when it is shipped from the factory. For ESCi operation, the corona pin is used in conjunction with the ESI probe. The following sections explain how to install and remove the ESI probe and corona pin.
  • Page 41 To avoid electric shock, ensure that the instrument is Warning: suitably prepared before commencing this procedure. Prepare the instrument for working on the source (see The Waters SQ Detector Operator’s Guide). The source can be hot. To avoid burn injuries, take Warning: great care while working with the instrument’s access door open.
  • Page 42 Ensure that the contacts on the ESI probe align with the probe adjuster assembly contacts, and carefully slide the ESI probe into the hole in the probe adjuster assembly. ESI probe Probe adjuster assembly Probe adjuster assembly contacts TP02632 ESI and ESCi Modes of Operation...
  • Page 43 Secure the ESI probe by tightening the 2 thumbscrews. ESI probe mounted on the source enclosure, showing the connections Vernier probe adjuster Thumbscrew Nebulizer gas connection Diverter valve POWER OPERATE Desolvation gas NEBULIZER DESOLVATION connection APPI ESI probe electrical lead PROBE Probe adjuster assembly...

  • Page 44: Installing The Corona Pin

    Using tubing greater than or equal to 0.004-inch (ID), connect the diverter valve to the ESI probe. Two tubes of different ID are supplied with the instrument. Tip: If you are replacing the tubing supplied with the Requirement: instrument, you must minimize the length of the tube connecting the diverter valve to the ESI probe.
  • Page 45 Do not apply any downward force to the source Caution: enclosure door while the door is open. Open the source enclosure door by releasing both spring-clips and lowering the door towards you. Use the needle-nose pliers to remove the blanking plug from the corona pin mounting contact.

  • Page 46: Optimizing The Esi Probe For Esci Operation

    Source, showing the corona pin, ESi probe tip, and sample cone ESI probe tip RP00029 Corona pin Sample cone tip Use the vernier probe adjuster to position the ESI probe tip so that it is pointing approximately midway between the tips of the sample cone and corona pin.
  • Page 47 To remove the corona pin The ACQUITY UPLC system connections, corona pin, Warning: ESI probe, and source can be contaminated with biohazardous and/or toxic materials. Always wear chemical-resistant, powder-free gloves while performing this procedure. To avoid electric shock, ensure that the instrument is in Warning: Standby mode when commencing this procedure.

  • Page 48: Removing The Esi Probe

    To avoid electric shock, ensure that the instrument is Warning: suitably prepared before commencing this procedure. Prepare the instrument for working on the source (see the Waters SQ Detector Operator’s Guide). The ESI probe and source can be hot. To avoid burn Warning: injuries, take great care while working with the instrument’s...
  • Page 49 Undo the 2 thumbscrews securing the ESI probe to the probe adjuster assembly. The ESI probe tip is sharp. To avoid puncture wounds, Warning: handle the probe with care. Carefully remove the ESI probe from the probe adjuster assembly. If available, fit the protective sleeve to the ESI probe tip. 10.
  • Page 50 3-12 ESI and ESCi Modes of Operation...

  • Page 51: Optional Apci Mode Of Operation

    Optional APCI Mode of Operation This chapter describes the optional atmospheric pressure chemical ionization (APCI) mode of operation, which uses the IonSABRE APCI source. Contents Topic Page Atmospheric pressure chemical ionization IonSABRE APCI probe Installing the IonSABRE APCI probe Installing the corona pin Removing the corona pin Removing the IonSABRE APCI probe...

  • Page 52: Atmospheric Pressure Chemical Ionization

    Atmospheric pressure chemical ionization APCI, an option for the instrument, produces singly charged protonated or deprotonated molecules for a broad range of nonvolatile analytes. APCI mode IonSABRE APCI probe Sample cone Corona pin Hot gas from the IonSABRE APCI probe passes between the sample cone and the corona pin, which is typically operated with a discharge current of 5 µA.

  • Page 53: Installing The Ionsabre Apci Probe

    Installing the IonSABRE APCI probe On instruments bearing the probe compatibility Warning: warning label (below), always use an APCI probe whose design incorporates a drain spout. In the event of a leak at the capillary union, using an older APCI probe model, whose design does not incorporate a drain spout, can lead to unmanaged solvent spillage and an associated risk of ignition.
  • Page 54 Ensure that the contacts on the IonSABRE APCI probe align with the probe adjuster assembly contacts, and carefully slide the IonSABRE APCI probe into the hole in the probe adjuster assembly. IonSABRE APCI Probe adjuster assembly probe Probe adjuster assembly contacts TP02632 Optional APCI Mode of Operation...
  • Page 55 Secure the IonSABRE APCI probe by tightening the 2 thumbscrews shown in the following figure. IonSABRE APCI probe mounted on the source enclosure, showing the connections to the front panel Vernier probe adjuster Thumbscrew Nebulizer gas connection Desolvation gas connection POWER OPERATE DESOLVATION...

  • Page 56: Installing The Corona Pin

    Connect the IonSABRE APCI probe’s electrical lead to the instrument’s probe connection. To avoid electric shock, do not use stainless steel Warning: tubing to connect the diverter valve to the IonSABRE APCI probe; use the PEEK™ tubing supplied with the instrument. Using tubing of the appropriate internal diameter (ID), connect the fluidics system’s diverter valve to the IonSABRE APCI probe.

  • Page 57: Removing The Ionsabre Apci Probe

    Removing the IonSABRE APCI probe Chemical-resistant, powder-free gloves Required material: To remove the IonSABRE APCI probe To avoid electric shock, ensure that the instrument is Warning: suitably prepared before commencing this procedure. Prepare the instrument for working on the source (see “Preparing the instrument for work performed on the source”...
  • Page 58 Optional APCI Mode of Operation...

  • Page 59: A Safety Advisories

    Safety Advisories Waters instruments display hazard symbols designed to alert you to the hidden dangers of operating and maintaining the instruments. Their corresponding user guides also include the hazard symbols, with accompanying text statements describing the hazards and telling you how to avoid them.

  • Page 60: Warning Symbols

    Heed all warnings when you install, repair, and operate Waters instruments. Waters assumes no liability for the failure of those who install, repair, or operate its instruments to comply with any safety precaution.

  • Page 61: Specific Warnings

    The following warnings can appear in the user manuals of particular instruments and on labels affixed to them or their component parts. Burst warning This warning applies to Waters instruments fitted with nonmetallic tubing. Pressurized nonmetallic, or polymer, tubing can burst. Warning: Observe these precautions when working around such tubing: •...
  • Page 62 Biohazard warning This warning applies to Waters instruments that can be used to process material that might contain biohazards: substances that contain biological agents capable of producing harmful effects in humans.

  • Page 63: Caution Symbol

    Chemical hazard warning This warning applies to Waters instruments that can process corrosive, toxic, flammable, or other types of hazardous material. Waters instruments can be used to analyze or Warning: process potentially hazardous substances. To avoid injury with any of these materials, familiarize yourself with the materials and their hazards, observe Good Laboratory Practices (GLP), and consult your organization’s safety...
  • Page 64 Attention: Changes or modifications to this unit not expressly approved by the party responsible for compliance could void the user’s authority to operate the equipment. Important: Toute modification sur cette unité n’ayant pas été expressément approuvée par l’autorité responsable de la conformité à la réglementation peut annuler le droit de l’utilisateur à...
  • Page 65 • Keine Schläuche verwenden, die stark geknickt oder überbeansprucht sind. • Nichtmetallische Schläuche nicht für Tetrahydrofuran (THF) oder konzentrierte Salpeter- oder Schwefelsäure verwenden. • Durch Methylenchlorid und Dimethylsulfoxid können nichtmetallische Schläuche quellen; dadurch wird der Berstdruck des Schlauches erheblich reduziert. Warnings that apply to all Waters instruments...
  • Page 66 Attenzione: fare attenzione quando si utilizzano tubi in materiale polimerico sotto pressione: • Indossare sempre occhiali da lavoro protettivi nei pressi di tubi di polimero pressurizzati. • Spegnere tutte le fiamme vive nell'ambiente circostante. • Non utilizzare tubi eccessivamente logorati o piegati. •...
  • Page 67 농축 질산 또는 황산과 함께 사용하지 마십시오. • 염화 메틸렌(Methylene chloride) 및 디메틸술폭시드(Dimethyl sulfoxide)는 비금속 튜브를 부풀려 튜브의 파열 압력을 크게 감소시킬 수 있으므로 유의하십시오. 警告：圧力のかかったポリマーチューブを扱うときは、注意してください。 • 加圧されたポリマーチューブの付近では、必ず保護メガネを着用してください。 • 近くにある火を消してください。 • 著しく変形した、または折れ曲がったチューブは使用しないでください。 • 非金属チューブには、テトラヒドロフラン(THF)や高濃度の硝酸または硫酸などを流 さないでください。 • 塩化メチレンやジメチルスルホキシドは、非金属チューブの膨張を引き起こす場合が あり、その場合、チューブは極めて低い圧力で破裂します。 Warnings that apply to all Waters instruments...
  • Page 68 Warning: 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.

  • Page 69: Electrical And Handling Symbols

    Electrical and handling symbols Electrical symbols These can appear in instrument user manuals and on the instrument’s front or rear panels. Electrical power on Electrical power off Standby Direct current Alternating current Protective conductor terminal Frame, or chassis, terminal Fuse Recycle symbol: Do not dispose in municipal waste.

  • Page 70: Handling Symbols

    Handling symbols These handling symbols and their associated text can appear on labels affixed to the outer packaging of Waters instrument and component shipments. Keep upright! Keep dry! Fragile! Use no hooks! A-12 Safety Advisories...

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