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4-1

Operating the Waters TQ
Detector

This chapter is an introduction to operating your TQ Detector; it
explains these tasks:

•

Setting-up your TQ Detector.

•

Performing a sample tune.

•

Developing instrument methods.

•

Verifying the system.

Contents:

Topic

Page

Setting-up the instrument

4-2

Performing a sample tune

4-7

Developing experiment methods

4-9

Verifying the system using System QC

4-11

Содержание TQ Detector

Страница 2: ...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 conse...

Страница 3: ...r to suggest ideas for otherwise improving it Please help us better understand what you expect from our documentation so that we can continuously improve its accuracy and usability We seriously consid...

Страница 4: ...This protocol addresses good operating procedures and the techniques necessary to validate system and method performance Instrument specific safety considerations Solvent leakage hazard The source exh...

Страница 5: ...en supply fails High temperature hazard Waters TQ Detector high temperature hazard Warning Where significant quantities of flammable solvents are involved the source must receive a continuous flow of...

Страница 6: ...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 When the TQ Detector is in Operate mo...

Страница 7: ...modes The Waters TQ Detector can be used for general In Vitro Diagnostic applications only by professionally trained and qualified laboratory personnel Symbol Definition Authorized Representative of t...

Страница 8: ...nd run to run Data collected when quality control samples are out of range might not be valid Do not report these data until you are certain that the instrument performs satisfactorily When analyzing...

Страница 9: ...the United Kingdom with the Medicines and Healthcare Products Regulatory Agency MHRA at market Towers 1 Nine Elms Lane London SW8 5NQ The reference number is IVD000167 Waters Corporation Micromass UK...

Страница 10: ...x...

Страница 11: ...ntative information ix IVD authorized representative ix 1 Waters TQ Detector Overview 1 1 Overview 1 2 Waters TQ Detector 1 2 ACQUITY TQD UPLC MS system 1 4 MassLynx mass spectrometry software and dat...

Страница 12: ...ystem from the Tune window 1 18 Programming the MS method to operate the IntelliStart fluidics system 1 18 2 Preparing the Waters TQ Detector for Operation 2 1 Starting the TQ Detector 2 2 Configuring...

Страница 13: ...e ESI probe for ESCi operation 3 7 Required materials 3 7 Removing the corona pin 3 9 Required materials 3 9 Removing the ESI probe 3 11 Required materials 3 11 4 Operating the Waters TQ Detector 4 1...

Страница 14: ...xiv Table of Contents Caution symbol A 5 Warnings that apply to all Waters instruments A 5 Electrical and handling symbols A 13 Electrical symbols A 13 Handling symbols A 14...

Страница 15: ...d plumbing connections Contents Topic Page Overview 1 2 Ionization techniques and source probes 1 7 Ion optics 1 9 MS operating modes 1 10 MS MS operating modes 1 11 Sample inlet 1 14 Vacuum system 1...

Страница 16: ...speeds compatible with ultra performance LC Waters provides these ion sources with the instrument as standard equipment ZSpray dual orthogonal sampling interface Multi mode ESCi ionization switching...

Страница 17: ...software IntelliStart enables simplified set up of the system for use in routine analytical and open access applications The IntelliStart fluidics system is built into the TQ Detector It delivers samp...

Страница 18: ...UPLC system and the Waters TQ Detector ACQUITY UPLC system The ACQUITY UPLC system includes a binary solvent manager sample manager column heater optional sample organizer optional detectors and a sp...

Страница 19: ...analog and mass spectrometry data MassLynx software permits these major operations Configuring the instrument Creating LC inlet and MS MS methods that define operating parameters for a run Using Intel...

Страница 20: ...ole The ACQUITY UPLC Console is a software application with which you configure settings monitor performance run diagnostic tests and maintain the system and its modules The ACQUITY UPLC Console funct...

Страница 21: ...The multiply charged ions are of particular interest because the TQ Detector separates them according to their mass to charge ratios m z permitting the detection of high molecular weight compounds The...

Страница 22: ...hemical ionization APCI probe is offered as an option See also The Waters TQ Detector Operator s Guide for full details Atmospheric pressure photoionization Atmospheric pressure photoionization APPI i...

Страница 23: ...rge ratio m z The mass separated ions pass into the T Wave collision cell where they either undergo collision induced dissociation CID or pass to the second quadrupole Any fragment ions are then mass...

Страница 24: ...n switching rapidly between MS and MS MS operation for example in survey scan mode It also provides a useful tool for instrument tuning and calibration before MS MS analysis and for fault diagnosis Th...

Страница 25: ...t ion mode Typical applications Structural elucidation for example peptide sequencing MS MS operating modes Operating mode MS1 Collision cell MS2 Product daughter ion spectrum Static at precursor mass...

Страница 26: ...hat is to complement or confirm product scan data by scanning for all the precursors of a common product ion Multiple reaction monitoring mode MRM mode is a highly selective MS MS equivalent of SIR As...

Страница 27: ...R a chromatogram is produced Constant neutral loss mode Constant neutral loss mode detects the loss of a specific neutral fragment or functional group from an unspecified precursor or precursors The s...

Страница 28: ...by direct or combined infusion Vacuum system An external roughing rotary vane pump and an internal split flow turbomolecular pump combine to create the source vacuum The turbomolecular pump evacuates...

Страница 29: ...65444751 VACUUM SOURCE VENT API GAS 6 9 BAR MAXIMUM V 200 240 Hz 50 60 VA 1200 RS 232 ETHERNET PUMP COLLISION GAS 1 0 BAR MAXIMUM IVD Not Used Switch 4 Ground Ground Stop Flow Switch 4 Ground Switch 3...

Страница 30: ...to enable optimization at analytical flow rates The IntelliStart system incorporates a multi position valve with these attributes An input connection from an external LC column An input connection fr...

Страница 31: ...and extent of the automation you want IntelliStart to perform See also The TQ Detector online Help for further details of IntelliStart Operating the IntelliStart fluidics system from the ACQUITY UPLC...

Страница 32: ...pties When the syringe is empty the system becomes idle 14 Click to refill the syringe or to purge the system 15 Click to stop the current action Operating the IntelliStart fluidics system from the Tu...

Страница 33: ...ts 3 In the Method events dialog box select the appropriate flow state as shown in the following table Tip At instrument power up the LC state is waste See also MassLynx online Help topic Advanced Met...

Страница 34: ...1 20 Waters TQ Detector Overview...

Страница 35: ...or Operation This chapter describes how to start and shut down the TQ Detector Contents Topic Page Starting the TQ Detector 2 2 Preparing the IntelliStart fluidics system 2 9 Rebooting the TQ Detector...

Страница 36: ...must be dry and oil free with a purity of at least 95 Regulate the supply at 600 to 690 kPa 6 0 to 6 9 bar 90 to 100 psi See also Figure titled TQ Detector rear panel on page 1 15 2 Ensure that the c...

Страница 37: ...power LED shows green During initialization the binary solvent manager s and sample manager s status LED flashes green After the instruments are successfully powered on all power LEDs show steady gre...

Страница 38: ...for Operation 8 Click Control Pump to start the roughing pump The operate LED remains off Tip There is a 20 second delay during which the turbopump is starting before the roughing pump starts Intelli...

Страница 39: ...ode When the TQ Detector is in good operating condition IntelliStart displays Ready Tip Clicking Resolve should prepare the system for operation putting the TQ Detector into Operate mode If clicking R...

Страница 40: ...or an item highlight it and click Properties 4 Click Apply OK Verifying the instrument s state of readiness When the TQ Detector is in good operating condition the power LED shows constant green and t...

Страница 41: ...s IntelliStart automatically sets these when you enter a flow rate according to the following table Note Under low ambient temperature high moisture and high flow rate conditions condensation can occu...

Страница 42: ...he system is waiting for an instrument component to reach operational conditions The LED could for example flash while the system reaches a programmed temperature set point or vacuum level The instrum...

Страница 43: ...olvent manifold drip tray Required materials Chemical resistant powder free gloves To install the solvent manifold drip tray Install the solvent manifold drip tray as shown below Warning The solvent m...

Страница 44: ...r free gloves To install the reservoir bottles 1 Remove the reservoir bottle caps 2 Screw the reservoir bottles onto the TQ Detector as shown below Warning The reservoir bottles can be contaminated wi...

Страница 45: ...d waste is open The syringe is empty and the flow path between it and waste is open LC position In the LC position the flow path between the LC and probe is open and the flow path between the syringe...

Страница 46: ...nfusion position in infusion mode Combined position with LC flow and syringe in idle mode Column Infusion LC Waste Probe Syringe Reservoir A Reservoir B Off On B A Infusion Column Combined LC Waste Pr...

Страница 47: ...the infusion syringe with the solution that you are going to use next Tip Depending on the solutions used the IntelliStart fluidics system can require more then one purge cycle to minimize carryover T...

Страница 48: ...nitialize Immediately following software download Rebooting the TQ Detector by pressing the reset button Tip The reset button shuts down the electronics momentarily and causes the TQ Detector to reboo...

Страница 49: ...t shutdown You might want to shut down the instrument for a relatively brief period like overnight while maintaining the LC flow To put the TQ Detector in Standby mode 1 In the ACQUITY UPLC Console cl...

Страница 50: ...valve opens and the instrument is automatically vented The operate LED changes from green to red and then turns off 5 Exit MassLynx 6 After the roughing pump shuts off operate the power button on the...

Страница 51: ...n the front of the TQ Detector 2 Disconnect the power cable from the back of the TQ Detector Warning The TQ Detector s power switch does not isolate the instrument from the main power supply To isolat...

Страница 52: ...2 18 Preparing the Waters TQ Detector for Operation...

Страница 53: ...i combined electrospay and atmospheric pressure chemical ionization If your system uses APCI mode refer to Chapter 6 of the Waters TQ Detector Operator s Guide Contents Topic Page Introduction 3 2 Ins...

Страница 54: ...7 Installing the ESI probe Required materials Chemical resistant powder free gloves To install the ESI probe 1 Prepare the instrument for working on the source See also Chapter 5 of the Waters TQ Det...

Страница 55: ...e the ESI probe into the hole in the probe adjuster assembly 5 Secure the ESI probe by tightening the two thumbscrews See also Figure titled ESI probe mounted on the source enclosure showing the conne...

Страница 56: ...r ID Tip Two tubes of different ID are supplied with the instrument Requirement If you are replacing the tubing supplied with the instrument you must minimize the length of the tube connecting the div...

Страница 57: ...probe and source can be contaminated with biohazardous and or toxic materials Always wear chemical resistant powder free gloves while performing this procedure Warning To avoid electric shock ensure...

Страница 58: ...pin to the mounting contact Requirement Ensure that the corona pin is securely mounted and that its tip aligns with the sample cone orifice Warning The corona pin tip is sharp To avoid puncture wound...

Страница 59: ...e showing the connections to the front panel on page 3 4 7 Close the source enclosure door and fasten the handle 8 Close the instrument s access door Optimizing the ESI probe for ESCi operation Requir...

Страница 60: ...nd Corona A in the current mode or kV in the voltage mode to produce the most intense ESI and APcI signal 13 Use the vernier probe adjuster to gradually move the probe bi directionally to determine th...

Страница 61: ...source can be contaminated with biohazardous and or toxic materials Always wear chemical resistant powder free gloves while performing this procedure Warning To avoid electric shock ensure that the i...

Страница 62: ...plug to the corona pin mounting contact See also Figure titled Corona pin mounting contact on page 3 6 6 Close the source enclosure door and fasten the handle 7 Close the instrument s access door Warn...

Страница 63: ...6 Undo the two thumbscrews securing the ESI probe to the probe adjuster assembly 7 Carefully remove the ESI probe from the probe adjuster assembly Warning The ACQUITY UPLC system connections ESI probe...

Страница 64: ...3 12 ESI and ESCi Modes of Operation 8 If available fit the protective sleeve to the ESI probe tip 9 Close the instrument s access door...

Страница 65: ...Detector it explains these tasks Setting up your TQ Detector Performing a sample tune Developing instrument methods Verifying the system Contents Topic Page Setting up the instrument 4 2 Performing a...

Страница 66: ...aterials Sodium cesium iodide solution 2 ng L Sulfadimethoxine solution 100 pg L To prepare the IntelliStart fluidics system See also IntelliStart fluidics system operation on page 1 17 1 Ensure that...

Страница 67: ...1 In the ACQUITY UPLC Console system tree click TQ Detector 2 Ensure that Ion Mode is ES 3 In the ACQUITY UPLC Console system tree click IntelliStart 4 Ensure that Instrument Setup is selected 5 If yo...

Страница 68: ...every time you select a new calibration reference file Instrument Setup Parameters dialog box Instrument Setup tab with default parameters Tip You can use alternative reference solutions to calibrate...

Страница 69: ...the Sample Tune tab 2 Click Copy Instrument Setup masses Rationale The Tune Masses from the Instrument Setup tab are copied into the Sample Tune Masses boxes Instrument Setup Parameters dialog box Sa...

Страница 70: ...rt instrument set up 1 Click Start Result A message appears reminding you to ensure that the calibrant solutions calibration parameters and LC flow are set correctly 2 Click OK Result Instrument set u...

Страница 71: ...e four masses defined in the IntelliStart Setup Parameters dialog box When the sample tune is complete the results are written to the Sulfadimethoxine ipr file Performing a sample tune In the followin...

Страница 72: ...valid If so no sample tune is performed See also TQ Detector online Help topic IntelliStart flow diagram 7 Click Start 8 In the IntelliStart Setup Parameters dialog box s Sample Tune tab specify the...

Страница 73: ...solution in reservoir B See also To prepare the IntelliStart fluidics system on page 4 2 2 In the ACQUITY UPLC Console system tree click TQ Detector 3 Ensure that the Ion Mode is ES 4 In the ACQUITY U...

Страница 74: ...rs reminding you to ensure that the sample solutions sample tune parameters and LC flow are set correctly 12 Click OK Result Method development starts The ACQUITY UPLC Console displays the progress of...

Страница 75: ...e sequence or automatically based on a scheduled date and time Multiple injections are processed using the OpenLynx Application Manager Measurements are reported for each chosen parameter across the r...

Страница 76: ...method files from the System QC project SystemQC pro You must save the tune inlet and method files to the Aqudb folder of the System QC project before performing the verification To perform a manual...

Страница 77: ...ning method enter a Mass on which to perform peak detection 6 Select Print Report to print a report of the results 7 Select the Acceptance parameters Instrument Setup Parameters dialog box System QC t...

Страница 78: ...ears reminding you to ensure that the sample vial QC parameters and LC flow are set correctly 9 Click OK Result System QC starts The ACQUITY UPLC Console displays its progress Signal Noise In Signal N...

Страница 79: ...des also include the hazard symbols with accompanying text statements describing the hazards and telling you how to avoid them This appendix presents all the safety symbols and statements that apply t...

Страница 80: ...ks include burn injuries electric shocks ultraviolet radiation exposures and others When the following symbols appear in a manual s narratives or procedures their accompanying text identifies the spec...

Страница 81: ...around such tubing Wear eye protection Extinguish all nearby flames Do not use tubing that is or has been stressed or kinked Do not expose nonmetallic tubing to incompatible compounds like tetrahydro...

Страница 82: ...l surfaces of the mass spectrometer when the instrument is in Operate mode To avoid non lethal electric shock make sure the instrument is in Standby mode before touching areas marked with this high vo...

Страница 83: ...hen operating this device follow standard quality control procedures and the the equipment guidelines in this section Warning Waters instruments can be used to analyze or process potentially hazardous...

Страница 84: ...n oder Modifikationen an dem Ger t ohne die ausdr ckliche Genehmigung der f r die ordnungsgem e Funktionst chtigkeit verantwortlichen Personen kann zum Entzug der Bedienungsbefugnis des Systems f hren...

Страница 85: ...e trouvant proximit de l instrument Evitez d utiliser des tubes s v rement d form s ou endommag s Evitez d utiliser des tubes non m talliques avec du t trahydrofurane THF ou de l acide sulfurique ou n...

Страница 86: ...no rigonfiamento nei tubi non metallici riducendo notevolmente la resistenza alla rottura dei tubi stessi Advertencia se recomienda precauci n cuando se trabaje con tubos de pol mero sometidos a presi...

Страница 87: ...Warnings that apply to all Waters instruments A 9...

Страница 88: ...isque d tre d fectueuses Vorsicht Der Benutzer wird darauf aufmerksam gemacht dass bei unsachgem er Verwenddung des Ger tes unter Umst nden nicht ordnungsgem funktionieren Attenzione l utente deve ess...

Страница 89: ...de la m me puissance afin d viter tout risque d incendie Vorsicht Zum Schutz gegen Feuergefahr die Sicherungen nur mit Sicherungen des gleichen Typs und Nennwertes ersetzen Attenzione per una buona p...

Страница 90: ...prise avant d effectuer la maintenance de l instrument Vorsicht Zur Vermeidung von Stromschl gen sollte das Ger t vor der Wartung vom Netz getrennt werden Attenzione per evitare il rischio di scossa e...

Страница 91: ...ls 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 ter...

Страница 92: ...visories 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 Fragil...

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