X Series Getting Started Guide

Issue 1.3 : January 2004Ref. No. : S419MA

X Series ICP-MSGetting StartedGuide

This page is left blank intentionally

Contents

A: Optimizing the Signal 1STEP 1: Instrument Pre-Start-up Status 2STEP 2: Switching the Instrument on 3STEP 3: Configuration Setup 3STEP 4: Accessories Control 5STEP 5: Manually Optimizing the Signal 5STEP 6: Autotune Procedure 10

B:Initial Performance Checks 19STEP 1: New Experiment Creation 21STEP 2: Experiment Setup 22STEP 3: Acquisition Parameter Setup 26STEP 4: Isotope Ratio Selection 27STEP 5: Creating a Sample List 28STEP 6: Running aPerformance Report test 30

C:Instrument Calibrations 37STEP 1: Detector Calibration 40STEP 2: Mass Calibration 47STEP 3: Detector Monitoring 53

D: Sample Analysis 55STEP 1: New Experiment Creation 57STEP 2: Experiment Setup 58STEP 3: Acquisition Parameters 62STEP 4: Internal Standard Selection 63STEP 5: Calibration Method Setup 65STEP 6: Creating a Sample List 67STEP 7: View Data Acquisition 69STEP 8: Viewing the Spectra 70STEP 9: Semi-Quantitative Results 73STEP 10: Fully Quantitative Results 75STEP 11: Reporting Data 81

i

E: Operating PlasmaScreen 85STEP 1: Installing PlasmaScreen 87STEP 2: PlasmaScreen Configuration Setup 89STEP 3: Tuning PlasmaScreen 90STEP 4: Edit New Analyte Database 92STEP 5: Create New Experiment 94

F: CCT Operation 99STEP 1: CCT Setup 101STEP 2: Tuning CCT 102STEP 3: Tuning CCTED 103STEP 4: Create an Experiment 105STEP 5: Data Interpretation 108

G: Routine Maintenance &Troubleshooting 109

Part A: Routine Maintenance 111STEP A1: Peristaltic Pump Tubing 111STEP A2: Spray Chamber 112STEP A3: Removing the Glassware 113STEP A4: Cleaning the Glassware 115STEP A5: Nebulizer Maintenance 116STEP A6: Refitting the Glassware 117STEP A7: Cleaning the Cones 118STEP A8: Replacing the Multiplier 121Routine Maintenance Checklist 129

Part B: Troubleshooting 130STEP B1: Instrument not Starting 130STEP B2: Sensitivity Problems 132STEP B3: Signal Drifts with Time 134STEP B4: Poor Stability 135

ii

Copyright noticeAll rights reserved.

Information in this document is subject to change without notice anddoes not represent a commitment on the part of Thermo ElectronCorporation. No part of this manual may be copied or distributed,transmitted, transcribed, stored in a retrieval system or translated intoany human or computer language, in any form or by any means, elec-tronic, mechanical, magnetic, manual or otherwise, or disclosed to thirdparties without the expressed written permission of:

Thermo Electron Corporation Elemental AnalysisIon PathRoad 3WinsfordCheshireCW7 3BXUK

AcknowledgmentsThermo Electron, PlasmaQuad, X Series ICP-MS, PlasmaLab,MicroProbe, PrepLab are trademarks of Thermo ElectronCorporation.

Pentium is a registered trademark of Intel Corporation

Windows NT , Excel and Access are registered trademarks ofMicrosoft Corporation

C

iii

PlasmaLab™SOFTWARE LICENSE AGREEMENTThe software (which term shall include discs, computer program andrelated materials) supplied with the goods is the Confidential andProprietary Information of the Vendor. Subject to the provisions of thisagreement, the Vendor warrants that it is authorized to grant you a rightto use the software with the goods. Installation of the goods and/orsoftware is deemed to be your unconditional acceptance of thisagreement.

Grant of Single User License of the GoodsIn consideration of payment of the license fee which is part of thepurchase price, the Vendor grants a right to use the software on asingle computer with a single instrument.

If the Purchaser wishes to use the software on more than one computeror instrument then the Purchaser expressly agrees to purchase anadditional user license for each additional user copy from the Vendor.

TermThis agreement is effective from the date of delivery of the goods and/or software and continues until either or both are disposed of. TheVendor may terminate this agreement forthwith without notice if thePurchaser is in breach of the terms of this agreement.

Ownership of the SoftwareThe Purchaser owns the magnetic or other physical media on which thesoftware is originally or subsequently recorded or fixed, but an expresscondition of this agreement is that the Vendor retains title andownership of the software recorded on the original disk copy(ies) andall subsequent copies of the software regardless of the form or mediain or on which the original and other copies may exist. This agreementdoes not constitute a sale of the software or any copy.

iv

Copy RestrictionsThe software and the accompanying manuals are copyrighted.Unauthorized copying of the software including software which hasbeen modified, merged or included with other software or of the writtenmaterials is expressly forbidden. The Purchaser may be heldresponsible for any copyright infringement which is caused orencouraged by a failure to abide by the terms of this agreement.

User RestrictionsThe Purchaser may physically transfer the software from one computerto another provided that the software is used on only one computer at atime. The Purchaser may not distribute copies of the software oraccompanying written materials to others. The Purchaser may notmodify, adapt, translate reverse, engineer, decompile, disassemble orcreate derivative works based on the written materials without the priorwritten consent of the Vendor.

Disclaimer of Warranty and Limited WarrantyThe Purchaser acknowledges that the software in general and the usermanuals may not be error free and agree that the existence of sucherrors shall not constitute a breach of this agreement. However, theVendor warrants that for a period of 12 months after installation or 13months after delivery, whichever is the sooner, that under normal use thematerial of magnetic media and the user manuals will not provedefective. Furthermore and for the same period, the Vendor warrantsthat the software will prove to operate substantially complete andcontain all information which the Vendor deems necessary for the useof the software.

The above is the only warranty of any kind, either express or implied,statutory or otherwise, including but not limited to the implied warrantiesof merchantability or fitness for a particular purpose that is made by theVendor. No oral or written advice given by the Vendor, its dealers,distributors, agents or employees shall create a warranty or in any wayincrease the scope of this warranty and you may not rely on any suchinformation or advice. The warranty gives you specific legal rights. Youmay have other rights which vary from location to location.

v

Your sole remedies and the entire liability of the Vendor and itssuppliers are set forth above. In no event will the Vendor or its suppliersbe liable to you or any other person for any damages whatsoever orhowsoever arising including without limitation any direct, indirect,special, incidental or consequential damages, expenses, lost profits,lost savings or other damages arising out of use or inability to use thesoftware.

AssignmentYou may not sub-license, assign or transfer this agreement or thesoftware without the prior written permission of the Vendor. Any attemptotherwise to sub-license, assign or transfer any of the rights, duties orobligations herein is void.

Thermo Electron CorporationJune 2003

Intended use of the equipment

The equipment is intended to be used by trained personnel within alaboratory environment, for the purpose of chemical analysis. It shouldnot be used for any other purpose or within any other environment. Theinstrument must not be used in an unspecified manner.

Reference Thermo Electron Corporation Pre-Delivery Pack forintended use of the equipment including technical specifications,environmental conditions, laboratory preparation requirements andother health and safety issues.

vi

1 Practical A: Optimizing the Signal

Practical A: Optimizing the Signal

STEP 1: Instrument Pre-Start-up Status

STEP 2: Switching the Instrument on

STEP 3: Configuration Setup

STEP 4: Accessories Control

STEP 5: Manually Optimizing the Signal

STEP 6: Autotune Procedure


A: Optimizing the Signal

Objective:This exercise will lead you through the first basic operational steps fromswitching the instrument on, obtaining the first signal and optimizing theinstrument.

A: Optimizing the Signal

STEP 1: Instrument Pre-Start-up Status

STEP 2: Switching the Instrument on

STEP 3: Configuration Setup



STEP 6: Autotune Procedure

Solution required for this practical:10ppb Tuning Solution (Li, Be, Bi, Ce,Co, In, Ba, Pb, Tl, U) in 2% HNO3.

STEP 1: Instrument Pre Start-up Status

Do the following checks before switching the instrument into operatestate: -i) Ensure glassware and cones are in positionii) Check the peristaltic pump tubing is in good condition andtubing is clamped.iii) Ensure Faraday cage is in its forward position and that the Faradaycage door is closed.


1. Click once on the On button andthe instrument will go automaticallythrough the start-up cycle which lastsapproximately 90 - 120 seconds.During the sequence, the sampleintroduction system is purged withargon, the neb gas is then switchedoff before the RF power is startedand the ICP ignited; the interfacevalve is opened, and the slide valveseparating the interface from the highvacuum region is opened (this occurswhen the expansion pressure hasreached < 3mbar). Once On, checkthe Peltier chiller temperature (ifrequired).

STEP 2: Switching the Instrument On

STEP 3: Configuration Set-up

1. Click on the Instrument icon to open up the instru-ment control.

2. Open the Configuration page, which displays the ConfigurationEditor. From this page the correct configuration can be selected.Configurations are usually setup for different sample introduction set-ups, i.e. Autosamplers, Low flow nebulizers, Laser Ablation, USN6000etc.The Accessories and Devices that are to be used can be selectedby ticking the appropriate box , or setup using the accessory wizard.The instruments settings can be selected here if a particular set oftuning parameters are required, or left unticked if the current instru-ment settings are to be used.

1


3. Click on New Configuration if different settings other than defaultor those already displayed are required. The Description is editableto indicate which options are being used. Each configuration has itsown related tune settings which when saved appear under Instrumentsettings. Click on the required configuration to use it.

4. Click on Accessories Wizard if a required accessory is not avail-able for selection. The wizard guides the user through the selection andconfiguration of new accessories.

5. Tick the use box on the Available Accessories and Devices toselect which accessory is to be used for future experiments. (i.e. if anautosampler is selected here, when a new experiment is opened, it willautomatically configure the experiment for autosampler sample posi-tions).

3 4

5



Use the standard tuning solution containing 10ppb of Li, Be, Co, In, Ba,Ce, Pb, Bi, Tl and U. Place the sample uptake tube into the 1ppb tunesolution and ensure that the solution is taken up smoothly. Ensure thesolution uptake and the drainage is working correctly.

1. Click on Tune Page in the instrument section.2. Ensure Pulse Counting is selected for Real Time Display.

3. Click on the Accessories Window in the Tune page to display theAccessories control. The peristaltic pump or autosampler can beinitialized and pump speeds optimized, also autosamplers can bemanually set to go to different positions from here if required, e.g. tosend the autosampler to the tune solution via an autosampler position.

1. Click on Tune in the Instrument section, which is already open.Otherwise click on the Instrument icon to open this section.

2. Click on the hide/show button to either hide or show the manual slidecontrols. For users who only use the autotune functions, the manualslider controls are usually hidden. The setting of the hide/show button isremembered on a per user basis from the Windows logon.

3. Click on Major. These parameters are the most common parametersfor tuning and have the greatest effect on signal stability and sensitivity.

4. Click here to start the Real Time Display (RTD)


You can optimize the signal either manually or automatically. Usually theAutotune option is used, but it is good practise to be familiar with themanual tuning process, which will be explained briefly. Optimize for thehighest sensitivity while obtaining low levels of oxides and doublycharged species.

3

12


5. Use the slider to select the default settings as shown. The largebutton is the slider bar to change the voltage setting. The small resetbutton underneath the slider resets the voltage to the last saved setting.The red colour underneath the slider indicates the voltage region whichshould not be used, the yellow indicates caution and the grey range is therecommended settings for voltage tuning. Gently drag the slider by mov-ing the mouse pointer to the grey rectangle, and while holding down theleft button, move it along.

2

2


The voltage will be changed when the slider is released. Assuming thatthe torch is generally centered on the sample cone, start with D1, fol-lowed by Extraction, Lens 1, Focus, then Pole Bias, monitoring how thesignal changes with each adjustment. Continue adjusting each of thelenses in sequence, until the optimum signal has been obtained. Clickin the light grey region for coarse tuning and the arrows at the ends ofthe slider bar for fine tuning.Note that the Figure below shows the default settings.

6. Click on Minor for fine adjustment of the tuning. The Horizontal andVertical positions of the torchbox might need re-positioning slightlywhen using different torch types or if the torch has been replaced.

1

23

4

55


7. It is possible to change the masses to be displayed in the RTD atany time. Select the masses Co59, In115 and Bi209 by selectingthe tickbox Enable next to their mass. To change the masses moni-tored, click into the Symbol field and then on the downward arrow,which will display a periodic table. Select the analyte or interferenceyou wish to monitor from the periodic table.

7

10. Monitor the masses selected in the RTD. When tuning the ionoptics, a decrease and increase of the signal in CPS can be observed,when changing the voltage to the lenses. Tune for the maximum sensi-tivity, while obtaining a flat mass response across the whole massrange, ensure that the oxides and doubly charged do not exceed the

8. Enter a Dwell time of 100ms, drag and drop can be used to fill down.

9. Select CeO (156) and Ce++(70) as Numerators ratioed to Ce(140) asDenominator, to monitor the oxide and doubly charged species levels,(levels of <2% CeO and <3% Ce++ are acceptable). Note that these mustfirst be added to the mass list before Numerator and Denominator can beselected.

10 8


11. In the Global tune page, the settings for the resolution and detectorvoltages are displayed. This seldom needs to be changed, as for mostpurposes the resolution is factory set and the detector voltages can besetup automatically using the Instrument Calibration Wizard(seesection C).

12. Save the optimized parameters.

12

11

acceptable levels. The responses measured will depend on the inter-face type used and the mass monitored (i.e. Be does not ionize aswell as Li and therefore will not be as sensitive).


STEP 6: Autotune procedure

1. The autotune can be started manually by clicking on the Start theAutotune Wizard icon.

1Click on the icon to start theautotune procedure.

2. Click on either the Autotune icon or the arrow next to it. Both willinitiate the Autotune Wizard. The Autotune Wizard will now guide youstep by step through the procedure. Click on Next after each step.

2

Click on Run anAutotune se-quence.

Alternatively you canedit existing se-quences or create anew user-definedsequence.

1. The Tune page contains a further icon to perform the Autotune .This function replaces the manual tuning procedure explained in Step5. The Autotune procedure is fully user-definable to allow tuning forspecific application needs. A list of autotune procedure templates issupplied in the software and each procedure indicates which tuningsolution should be used.

The autotune procedure is subdivided into different stages, for eachstage individual minimum and maximum criteria can be defined.


3. This page allows you to select an existing Autotune sequence and ifmore than one version of the sequence exists, a specific version.Select the sequence from the list which suits your current application andconfiguration. For example, a higher sensitivity specification for the highmass end and/or lower oxide levels could be defined for specific applica-tions.

3

Each autotune sequence is listed as a folder. Clicking on the + sign nextto the folder will list the archived versions of the autotune sequence. Thegreen tick mark shows the currently active version of the sequence. Click-ing on the folder will automatically select the currently active version. Toselect any of the archived versions, expand the folder and just click on therequired version.

The text box on the right of the page shows the description of the currentlyselected sequence.

If the wizard is being used to run a sequence pressing the Next button willshow the stage ordering for the Autotune sequence allowing the user toconfirm that this is the correct autotune sequence to use.


4. For each se-quence, a tuningsolution is recom-mended, which youshould aspirate.

5. Click on Next tostart the autotune.

4

5

The detailed steps of theautotune sequence arelisted. This page allows theuser to review the order andcontents of the stages forthe autotune sequencebefore running and editing it.Each autotune stage islisted as a folder.

The user can choose tointroduce the samplemanually or via theautosampler. If theautosampler is selected,the rack, row, column andheight of the tune solutioncan be specified.


6. The progress of the autotune process is displayed in-situ in thedialogue box. The autotune process can also be viewed in the RealTime Display. A full autotune procedure will take approximately 10minutes. The range for each parameter can be pre-defined by the useror by the default template. By editing the parameters appropriately, theduration of the autotune process can be shortened.

The autotune script selected for this example is divided into threestages:Stage 1: It will optimize the horizontal and vertical position of the torchwhile maximizing the In signal.Stage 2: It will then optimize all the lenses one at a time, while maximiz-ing the signal for a defined mass.Stage 3: Tuning the nebulizer gas flow. It will go through maximizing thesignal as well as minimizing the oxides at the same time.


During the torch optimization, the In signal istuned for maximum sensitivity.

During the horizontalalignment procedure,the torch is changedbetween pre-definedsettings.

While the torch is moved between the horizon-tal pre-defined positions, the In signal is plottedover time. The software will then define thehorizontal position, where the maximum signalwas determined.

6

Helpful Hint: It is recommended that you create an autotune updatesequence once the instrument is fully optimized. This option gener-ates a new sequence which uses the new parameters as the defaultsetting and automatically narrows the range over which each param-eter is adjusted. Thus, the autotuning time can be significantly re-duced. An update is created automatically if the sequence has theCreat Update tickbox marked at the end of the editing process.


While the nebulizer gas setting is changed, not onlyIn is monitored for maximum sensitivity , but alsothe CeO/Ce ratio (blue line) is monitored in orderto minimize it.

When tuning the nebulizer gas flow, the effect is onlyvisible in the RTD after approximately 5sec, due to thetime taken for the nebuliser back pressure to adjust.For this reason, a default setting change is set in thesoftware between each change in the gas flow rate.

The RTD display can show both the analyte signal (black) and the CeO/Ce ratio (blue). The nebulizer gas flow is slowly increased or de-creased and the effect on the analyte and oxide signal can be illustratedin the RTD display.


7. Once the autotune procedure is completed, an Autotune report isgenerated which shows the chosen setting as well as the results foreach stage of the tuning process. The autotune report can be printed bysimply clicking on the printer icon. In this example, all set criteria werepassed. If any criteria were not passed, it would be highlighted in red.

The three stages - Torch position, Lenses and Nebulizer are listed aswell as the analytes and/or oxides monitored.

7

Printer iconAs can be seen,during stage 1, (torchposition) only the Insignal was optimized,whereas during stage2 (lenses), the signalwas optimized for Be,In and U. In stage 3(nebulizer), the sensi-tivities for the threeanalytes were moni-tored, while the CeO/O ratio was mini-mized.

8. After completion, the settings found during the autotune procedureare automatically saved in the Configuration page.

8


PlasmaLab allows you to view the results of successful autotunesequences. Right mouse clicking on the instrument settings grid on theconfiguration page will bring up the following menu.

The top menu item View autotune report only appears for settings thathave a User of Autotune. Selecting this menu item will bring up a dialogshowing the stage by stage progress of the autotune sequence used tocreate the settings.

To print this report, click on the printer icon, or click on the print previewbutton to preview what the print will look like.



19 Practical B: Initial Performance Checks

STEP 1: New Experiment Creation

STEP 2: Experiment Setup

STEP 3: Acquisition Parameter Setup

STEP 4: Isotope Ratio Selection

STEP 5: Creating a Sample List

STEP 6: Running a Performance Report test

B: Initial Performance Checks


ObjectiveTo set up a short term stability test with monitoring the oxides anddoubly charged species as isotope ratios. This is the daily checkingroutine prior to commencing the analysis of unknowns. A survey scanis also performed to check for good peak shapes and check the masscalibration and peak resolution.





STEP 3: Acquisition Parameter Setup




Solution required for this practical:10ppb tuning solution (Li, Be, Bi, Ce,Co, In, Pb, U)


Short term stability experiments can provide a great deal of usefulinformation on the performance of your instrument and should be under-taken as a daily checking routine every morning after optimizing theinstrument, and to archive the data so that day to day performance canbe monitored. The short term test lasts only 10 minutes and should beundertaken as part of the standard start-up routine by all users. Theinstrument should be allowed to stabilize for 15 minutes after starting upbefore attempting the short term stability test.A Survey Scan can be performed as part of this test, to give a greatdeal of useful information about peak shapes, resolution and masscalibration.

STEP 1: Creating a new experiment

1. Click on the Experiment Icon.

2. Click on Create a new blank experiment in the experiment wizard.

1

2



1. If the Setup pages are not shown click on the Setup Tab to showthem.

2. Click on the Configuration Editor to select the correct configurationfor the experiment.

3. You will be automatically prompted to choose a database. SelectDefault.tea as the analyte database for this experiment .

3

12


3. By default the ICP-MS will use the current configuration and tunesettings, which are shown in purple. If different conditions are required,select the correct Configuration for the experiment by ticking the Usebox. The software will now display the selected configuration in purple.By selecting a configuration for an experiment it allows multiple experi-ments to be queued with different conditions.

5. The instrument settings box can remain unticked if only one set ofinstrument settings is being run, this will enable the experiment to usethe last set of saved instrument settings. If different settings are used(i.e. Standard mode and PlasmaScreen mode), then the relevantinstrument settings should be ticked in each experiment.

3

4

4. The Accessories used with this configuration are shown. Should thesebe incorrect, the configuration will need to be edited in the Main InstrumentSection of the software before continuing.


6. Click on the Timings Tab to set up the sample introduction timings.Select the Uptake time for the time taken for the sample to reach theplasma and Washout times as shown above. Monitored uptake andwash will allow masses to be used to automatically determine when asample has been introduced or washed out. Consult the on-line help forfurther information on this function.

7. Click on the Analyte tab. Select the following analytes by doubleclicking to select the default isotope:Li, Be, Co, In, Ce, Pb, Bi, U and Bkg

The masses Bkg and Ce are monitored for checking the backgroundnoise, oxides and doubly charged species. The other analytes aremonitored for the short term stability test.

6

7


9. To monitor the doubly charged species, select Ce++ from thepolyatomic list and select 140Ce++.

10. To monitor the oxides, select CeO from the polyatomic list andselect 156CeO.

8. Click once on Bkg to manually select the masses 5 and 220 in orderto monitor the background noise for the low and the high mass. Twoblue dots will now appear for Bkg, indicating that two isotopes havebeen selected.

8

10

9


STEP 3: Setting the Acquisition Parameters

1. Now the acquisition parameters can be defined. Select from theexperiment section: Setup.

2. Select Acquisition parameters.

3. Select Survey Run (light grey when selected).

4. Select the main run to be Peak jump this will just run the elementsselected in the analyte menu.

5. Enter the same value for the number of Sweeps as shown above.

6. Select the Start and End Mass for the skip regions and Dwell time,Channels per AMU as shown for the Survey run. These parametersonly become available when the Survey run has been selected. TheAcquisition time will be automatically calculated. The survey run isalways performed in scanning mode. The parameters shown aredefault and should already be present.

1 23 4

56

7

8



1. To define the Isotope Ratios, click on Setup and Isotope Ratio.

2. The ratios for the oxides and doubly charged species can now bedefined. Click on the downward arrow to display the list of analytes tochoose the Numerator and Denominator.

3. After selecting first the Numerator and then the Denominator, click onthe Add ratio button.

4. After clicking the Add ratio button, both analytes will be displayed inthe table. Select the ratios as shown below for Ce++/Ce and CeO/Ce. Ifa ratio is incorrectly added, it can be removed by clicking the grey boxnext to the ratio in the grid and press the Delete ratio button.

12

34

7. For the Main Peak jump run select the number of sweeps to be 110.

8. As the Main run is normally performed in Peak Jumping mode, thenumber of Sweeps, Dwell time and Channels per AMU are differentto the survey run. Enter the Dwell times for the analytes previouslydefined in the element menu. Use a Dwell time of 30ms for the analytes,oxides and doubly charged species and 100ms for the backgroundmasses. The acquisition time will be automatically calculated, thisshould be approximately 60s for a short term stability test.


3. It is recommended to build up a libraryof templates for routine analysis types,e.g. for tuning, short term stability testetc.

To create a template at any stage ofbuilding an experiment or even postacquisition, choose the File, Save AsTemplate option when the experiment isopen.


1. Now the sample list can be defined. Click on Sample List and thenagain Sample List.

2. Enter all fields as shown below. The Survey Run will be used tocheck the mass calibration and peak shapes for the full mass rangeand then the 10 Main Runs will be used for the short term stability test.

1

2

3


To perform the short term stability test in thefuture, click on Template at the lower left cornerand select Survey and stabilities.

Alternatively, click on the Experiment Icon,create an experiment from a template andselect Survey and stabilities.tet. It is also pos-sible to add extra samples or analytes to theoriginal experiment if desired.

5. The list of Templates available can be viewedby clicking on Template at the lower left corner ofthe screen and the currently defined Templateswill be shown.

4. File Save as Template, file name ‘Survey and stabilities’.

6. When the sample list is complete click on the Experiment Queuebutton to start the Acquisition.

5

4

6



The Tune page contains two further icons to either perform theAutotune or to Start the Performance Report Wizard. Those twofunctions replace the manual tuning procedure and the short termstability test as explained in the earlier steps of this practical.

Autotune icon Start the performance report wizard icon

The autotune and performance report functions are designed to replacethe manual tuning procedure and the short term stability test. A user-defined performance report can be set up similar to the short termstability test, in which the user will define the daily performance specifi-cations for their instrument. If the criteria are met, the instrument isready to commence sample analyses. If the criteria are not met, then anautotune must be performed, after verifying that all other possiblesources of the performance test failure have been excluded.

The performance report is a user-definable procedure, although thesoftware is supplied with pre-defined examples. It is generally set up torun a short term stability test, in which the user can define the pass/failcriteria. These criteria could entail different sensitivity specifications forthe analytes, RSD limits, and/or limits on oxide levels, double chargedspecies, background counts etc. These limits can be set to eitherminimum or maximum values and the user can specify the action to betaken if any of the criteria are not met. The user can also define whatanalytes to analyze in that short term stability test, which could be thetune solution or it could contain analytes closer to the analytes in thesamples. After the analysis, the software will evaluate the pass criteria.

If it passes, the user can carry on with the analyses of standards andunknown samples. If it fails, the autotune procedure should be per-formed. If this passes, the performance test should be repeated.

The performance report and autotune routines can be fully automated inan experiment. Refer to the on-line help for further information aboutthis option.

1


1. After the instrument has been switched on and has warmed up, clickon the icon for the Performance Report and a wizard will automaticallyopen up. The toolbar button provides access to the Performance reportconfiguration and execution functions. Clicking on the icon starts thePerformance report aquisition wizard.The first item in the menu allows the user to start the Performancereport aquisition wizard, which is the same action as clicking on thetoolbar button. Listed at the bottom of the menu are up to eight of thelast Performance reports that have been run. Clicking on one of theseitems will start the currently active version of the Performance report.

2. Follow the steps of the Performance Report Wizard, as shownbelow. Click on Aquire a Performance Report. Click on Next aftereach step.

3. Select the reportthat matches yourconfiguration from thelist.

If no report suitable foryour configuration isavailable, Cancel thewizard and either editan existing report orcreate a new one atthe start of the perfor-mance report wizard.

2

3


4. Select if you wishto introduce thesample manually orvia the autosampler.

5. Load the sampleand click on Next tostart the performancereport sample update.

6. The performancereport aquisitionwizard displays everystep of the process, eguptake delay in secs.

Each Performance report is listed as a folder. Clicking on the + signnext to the folder will list the archived versions of the Performance report.The green tick mark shows the currently active version of the report.Clicking on the folder will automatically select the currently active version.To select any of the archived versions, expand the folder and just click onthe required version.The text box on the right of the page shows the description of the currentlyselected report.

4

5

6


7. After the uptakedelay, the aquisitionprocess is shown indetail.

8. The results of the performance report aquisition wizard are displayed.In this example, the criteria were not met, and the performance validationhas failed. The wizard will list possible explanations for the failure. If thecorrect solution and performance report for the current instrument configu-ration were chosen, it is recommended to re-tune the instrument.

This is the final page for the Performance report wizard. Clicking on theFinish button will finish the wizard. The view report button will display thereport and allow it to be printed. This report can also be viewed using theView Performance Report Results off the menu of the PerformanceReport button. The Save log file button allows the progress of the perfor-mance report to be saved to a file for diagnostic purposes if a failingperformance report test needs troubleshooting.

7

8


All failed criteria are highlighted in red

9

Helpful Hint: Generally, the performance testwill be passed first time. It is then possible tocommence with the sample running immedi-ately afterwards.

It is also possible to run the autotune prior tothe performance test by clicking its icon.

9. The Performance report is automatically displayed. The tuning pa-rameters are listed at the top of the page. The report can be printed bysimply clicking on the Print icon.

In this example, some of the criteria failed, such as the sensitivity speci-fication, as well as the oxide level. The failed criteria are highlighted inred.


PlasmaLab allows you to view the results of Performance reports that areacquired from the Instrument Tune page. Selecting the View Perfor-mance report results menu item from the Performance reports dropdown menu shows the following dialog.Each Performance report result is listed in the list window. Clicking on theheader of each column will sort that column, toggling between ascendingand descending for each click.To select a result to view just click on the name in the list. If you wish toviewmore than one result then hold down the Ctrl key whilst using themouse to click on each of the required results in the list.



37 Practical C: Instruments Calibrations

C: Instrument Calibrations

STEP 1: Detector Calibration

STEP 2: Mass Calibration

STEP 3: Detector Monitoring



ObjectiveThis section will take you through all steps of instrument calibration. TheX Series ICP-MS periodically needs to be calibrated for optimumperformance. The Instrument Calibration Wizard allows you to adjustthe mass calibration, as well as the detector calibration to ensure agood wide dynamic range with a cross calibration of the pulse countingand analogue modes of the detector.

Instrument CalibrationsThere are two types of calibration routines to perform on a regular basis,the detector calibration and the mass calibration. These calibrationsare made through the Instrument Calibration Wizard in the Instrumentsection or an experiment using an Instrument Setup Sample. When-ever an instrument Setup Sample is analysed, the data is always copiedback to the Instrument Database for subsequent experiments to use aswell as a copy being kept in the experiment itself.

The Instrument Calibrations page also shows the Detector Monitor-ing page which allows the user to track the lifetime of the detector cur-rently installed. For each new detector a new lifetime dataset is createdas well as a new section for the Detector Calibrations.




STEP 3: Detector Monitoring


The sample used for the detector setup wizard needs to be a multi-ele-ment solution which meets the following criteria:

• At least one analyte peak between masses 100-140 amu musthave a count rate between 500,000 and 2,000,000 cps. This maybe a minor isotope which is not normally used for measurement inan experiment (i.e. 117Sn). The software will use as many peaksas it can between 100 and 140 amu to setup the voltage on theanalog detector section. It will normally use more than one peak butunless it can find one peak that meets the criteria then the calibra-tion will fail and an appropriate message will be given in the wizarddialog.

• If possible, all the analyte elements that are to be measuredusing analog mode for any part in the experiment should bepresent in the solution with count rates exceeding 500,000 cps. Itdoes not matter if any (or most) of the peaks exceed the maximumcount rate allowed for the pulse counting detector section as thesoftware will automatically detect this during the calibration and usepoints at the side of the peak to make the cross calibration.

• To ensure a reasonable interpolation of the cross calibration whenno analytes are present in a mass range it will be better if both verylow mass and very high mass analytes are present at count ratesexceeding 500,000 cps in the calibration solution.

Solutions required for instrumentcalibration:It is recommended to use a ME solutionin the 50-100ppb range, containing low,mid and high mass elements.



The X Series ICP-MS can operate over a wide dynamic range, allowingthe user to analyze trace, minor and major element concentrations.Trace elements produce very low signals, which in turn require a largeamount of amplification. These elements are detected in the pulsecounting part of the detector. Large concentrations are measured withthe detector operating in analogue mode.

In order to achieve a continuous and wide dynamic range, the pulsecounting and analogue acquisition modes operate together. It is impor-tant to have the correct correlation between the two modes of operationto ensure continuity over the complete dynamic range. The correlationbetween pulse counting and analogue detection is mapped by thedetector cross calibration.

A conversion factor is calculated for each of the valid masses and thisis used to calculate a polynomial equation which is then used to gener-ate a lookup table of correction factors for each integer mass over thewhole mass range. Before being stored in the experiment and theinstrument database, for any masses where a factor has been mea-sured, the lookup table is replaced by the measured value.

As the instrument calibrations are automated procedeures, the user is notrequired to input any analyte information. The software automaticallydetects the analytes present in the solution, and chooses the most appro-priate ones to use.The detector calibration software is designed to work with solutions thathave high analyte concentrations which collect data in the analog detectormode. The software will automatically measure points at the side of apeak which trips the detector gate at its maximum.

The Instrument Calibration Wizard will perform all the steps necessaryto setup the detector.

1


1. Click on Set up the detector, a dialog will open to present the userwith options to do a calibration between the pulse counting and analogdetector modes (cross calibration) or to fully set up the detector voltagesand then do a cross calibration. Click on Next.

2. The user caneither present thesolution manuallyor via theautosampler.2

1


4. First the pre-scan is started,followed by themain aquisition.

Start the calibration process by pressing the Next button. This will give asample uptake timer which can be paused if required. To begin the cali-bration before the timer completes press the Next button. During theacquisition of data for the detector calibration the wizard will show thesteps being undertaken whilst the Real Time Display will show the actualdata acquired.

3. Click on Next tostart the sampleuptake.

3

4


5. Upon a successfulcompletion, the usercan click on Save logfile or click on Finish.

5

6. Enter afilename tosave theinstrumentcalibrationlog file.

6


The detector cross calibration is used to convert the data acquired usingthe analogue detector mode into the equivalent pulse counting data. Theresults of a successful calibration are shown on the Detector CrossCalibration page. This page is shown in both the experiment and theinstrument views.

The current cross calibration is shown in bold at the top of the tree-list. If anew detector has been fitted then the old cross calibrations are archivedunder the “old calibrations” part of the tree. To view a cross calibrationgraph and its data, click on the date and time for the calibration in the list.

The graph shows the measured data points with error bars showing the+/- acceptable errors from the calculated curve. The raw data for eachpoint can be seen by clicking on the point in the graph or on the row for ameasured analyte in the table.

7. The Detector Cross Calibration can be viewed in the Instrumentsection.

8. Before queueing the experiment, aspirate an appropriate solution,see solution required.

8


9. To View the results of the detector calibration go to the Instrumenticon.

9

10. Select Calibrations and Detector Cross Calibration, click on thedetector cross calibration that has just been performed, shown by thedate and time stamp.

11. The graph will show the calculated cross calibration factor for eachmass found on the y-axis against the mass on the x-axis, a polynomialfit will be applied through the enabled points. The cross calibrationfactor should be approximately 20000 - 40000 at mid mass.

10

Helpful Hint: A non-matching cross calibration pointcan be viewed and edited by clicking on the point. Allthe values used to determine the point are shown andthe values can be edited to inprove the fit if required.More information is available in the on-line help.


Alternately, the detector calibration can be performed via the instru-ment setup sample.1. Click on Sample List, Sample List in an Experiment.

2. Enter a sample Label for the detector cross calibration.

3. Click in the Type column and then on the downward arrow and selectInstrument Setup.

4. Click on Show Advanced to view the Advanced Properties.

5. To perform a detector calibration, check the appropriate box.

1

2 34

5

HELPFUL HINT: More diagnostic information oncalibration is provided by using the Instrument Cali-bration Wizard rather than the Instrument SetupSample in an experiment.


PlasmaLab uses the following default set of acquisition parameters forthe mass calibration.

Dwell 1000usChannels per AMU 20Scan Regions 4.5 to 10.5

23.5 to 27.550.5 to 78.581.5 to 245.5

PlasmaLab converts the mass ranges into DAC values using thecurrently selected mass calibration. These parameters are then sent tothe instrument which acquires 10 sweeps.

The software uses a mass calibration equation so that when a mass isselected for measurement, the control electronics can set the quadrupoleto transmit that mass. The mass calibrations are stored such that anyexperiment can access them when the experiment is being run.



A mass calibration set comprises the mass calibrations for both thestandard and high resolution quadrupole modes which are automati-cally done at the same time by the Mass Calibration Wizard or as partof an Instrument Setup Sample in an experiment.Follow the mass calibration wizard step by step.

1. Click on the Instrument Calibration Wizard icon, then onMass calibrate the quadrupole.

1


The mass calibration can be viewed in Instrument, Calibration, MassCalibration.


The quadru-pole resolu-tion at whichthe data wasacquired.

The date and timeat which the datawas acquired.

These are the 3 coefficientscalculated by applying asecond order polynomial fit tothe data that has been ac-quired.

A space to enternotes relating to thecalibration.

The massof theanalytewhere apeak wasfound.

The digital value atwhich the centre ofthe peak was found.

The width of the peakin Atomic Mass Unitsat 10% of the peakmaximum.

The difference betweenwhere the centre of thepeak was found and whereit is calculated that it shouldbe found using the polyno-mial line fit.

Whether or notto include thepoint in thecalculation forthe polynomialfit.


The top grid lists all of the mass calibrations that have successfully ac-quired and calculated. Clicking the right mouse button on the grid shows amenu that allows a mass calibration to be set as the current one.

The current mass calibration set is highlighted in green in the top grid.Clicking on any row will show the data for the mass calibration in the lowergrid and the relevant graph.

The graph will show the peak width and error between the found peakcentre and the calculated peak centre on the y axis against the mass onthe x-axis for each mass at which a peak has been found.

Data points can be included or excluded by either clicking on the point onthe graph or changing the state of the include box for the mass in the lowergrid.

Every time an experiment is queued, the current mass calibration asselected in the instrument view is copied from the instrument database.The top grid lists all of the mass calibrations that have been copied intothe experiment. Clicking the right mouse button on the grid shows a menuthat gives the option to import a mass calibration from the instrumentdatabase and to apply a mass calibration to all of the data in an experi-ment.

Instrument setup samples can be placed anywhere in the sample list andthey can also have repeat rules applied. However for most applications,only one will be required at the start of the experiment. The data collectedby an instrument setup sample for the instrument calibrations or autotuneis also copied to the Instrument database for use by subsequent experi-ments.


Once the calibrations have been completed the data can be viewedeither in the experiment that has just used the Instrument Setup Sampleunder the Instrument Calibrations tab or a complete list of all calibra-tions can be viewed in the Instrument section of the software under theCalibrations tab.

The Instrument Setup for the Instrument Setup Sample is divided intotwo parts, the first enables the mass calibration and Detector set up,whereas the second part enables the performance report and autotune.


STEP 3: Detector monitoring

After a new detector has been installed and the automatic outgas proce-dure has been completed (see Practical G: Maintenance), the detectorwill be monitored throughout its lifetime. The Detector Monitoring pagewill show the information for the new detector. The various parameterscan be displayed using the options on the right of the page.

The software will track various events during the lifetime of a detector fordiagnostic purposes. The various parameters measured can be viewedon the Calibrations pages of the Instrument section. Should a detectorlifetime issue arise this information will be able to help track the cause ofthe problem.



55 Practical D: Sample Analysis

D: Sample Analysis



STEP 3: Acquisition Parameters

STEP 4: Internal Standard Selection

STEP 5: Calibration Method Setup


STEP 7: View Data Acquisition

STEP 8: Viewing the Spectra

STEP 9: Semi-Quantitative Results

STEP 10: Fully Quantitative Results

STEP 11: Reporting Data


D: Sample Analysis

Objective:

To set up an experiment for the analysis of standards and unknownsamples. Calibration graphs will be created showing the quantitativeand semi-quantitative results.

D: Sample Analysis











STEP 11: Reporting Data


Solutions required for this practi-cal: 2% HNO3 blank and unknown in 2%HNO3 matrix.A series of standards at concentrationsof 5ppb, 10ppb and 20ppb from atuning solution (e.g. CLMS-2), contain-ing 1ppm of the following analytes: Li,Be, Co, Ni, In, Ba, Tl, Pb, Ce and U.Add internal standard solution contain-ing Ga, Rh and Bi at 10ppb.


1. Click on the Experiment icon to open the Experiment Wizard

2. Create a new blank experiment from the experiment wizard andselect Continuous mode of operation.

3. You will be automatically prompted to choose a database. SelectDefault.tea as the analyte database for this experiment .

1

2



1. In the selected new experiment click on the Configuration Editorin the Setup page to select the correct configuration.

2. Click on the Use box to select the standard default configuration, ifnot already selected.

1

3. Ensure the correct accessories for the experiment are visible asshown (e.g. for a peristaltic pump for manual operation or anautosampler for unattended operation).

4. If an accessory is not shown for the experiment, it must first be set upusing the Instrument icon and the Accessory wizard in the Configu-ration Editor page. This will help you to select and configure the avail-able accessories, which will then be available when opening newexperiments. The accessories are setup in the instrument and shown inthe experiment section only for reference purposes.

4

2

3


5. The Instrument settings box can remain unticked if only one set ofinstrument settings is being run, this will enable the experiment to usethe last set of saved instrument settings. If different settings are used(i.e. Cool Plasma and Hot Plasma mode), then the relevant instrumentsettings should be ticked in each experiment (if not available these canbe set up and edited in the instrument control). Note that a Delay timecan be inserted to allow the instrument to settle between settings.


6. Select Timings tab in the Experiment Setup to select the Uptaketime for the time taken for the sample to reach the plasma and Wash-out time, as appropriate. Note that timings can be shortened consider-ably by the use of monitored uptake and wash (which can be selectedhere by ticking the Use Monitored and selecting a mass, such as theinternal standard, whose signal can be monitored) and rabbit (fastpumping) on uptake and wash. The rabbit option is set in the instrumentsection using accessory control language (ACL) scripts. See the onlinehelp about editing ACL scripts.

6

8. To select the Analytes which are required to be measured click onAnalyte from the Experiment Setup page.

9. Select all Analytes required by double clicking the left button on themouse on the analytes required, this selects the default isotope with theleast interference, these default isotopes are setup in the analyte data-bases. Alternatively, single click will display a choice of isotopes whichcan be manually ticked for selection. The number of isotopes selectedwill be highlighted as dark blue dots above the analytes. The lightblue dots automatically appear if analytes are required for an interfer-ence correction equation. Select all analytes that are required for useas internal standards, these will appear as yellow when selected asinternal standards (see Step 4). To remove an analyte use the righthand mouse button menu over the analyte in question.


10. To disable any interference correction equations not required, righthand mouse click on the row in the grid with the equation and choosethe disable equation option.

10

8

9


2. The default parameters for the Survey are shown below. The scanregion can be adjusted if required by a right mouse click to Add orRemove scan regions on the mass scan graphic. Alternatively thevalues in the numerical grid can be edited and the changes will berepeated in the graphic.


1. In Experiment Setup click on Acquisition Parameters to set up thesurvey and main run for the acquisition. The Main run selection can beeither scanning or peak jump, depending on the application being run.The light grey areas show the selection made. Survey can be per-formed on all samples as a back up to the Main run, from which semi-quantitative data can be obtained, it can also be used to identify inter-ferences. The Main run can be selected either as Peak Jump for bestdetection of a small number of isotopes (<20) in the shortest time orScan for full spectral information.

1

2


3. The main run Peak jump default parameters are shown below. Peakjump mode is the preferred method for fast acquisition with best detec-tion. All the analytes selected in the Analyte menu will automaticallyappear in the symbol column.

4. If multiple tune settings have been chosen for the experiment, theycan be associated with different analytes or scan regions here. Theorder of the settings and any stabilization times between tune sets issetup on the configuration page of the experiment. It is possible here tochoose which of the quadrupole’s two Resolution settings are to beused for each analyte or region. Typically the resolutions are set to 0.8and 0.4 amu at 10% peak height. The narrower peak (higher resolution)will improve interference removal for small peaks next to very largeones and will also extend dynamic range even further for high concen-tration analytes.


1. In the Setup menu click on Internal Standards to select internalstandards for the experiment. It is recommended to select an internalstandard at low, middle and high mass for a multi-element analysis, toensure that any changes in response due to drift or matrix suppression /enhancement are compensated for. Internal standards are selected thatare (if possible) close in ionization potential to the analyte massesselected, near to 100% abundance and not present in the samples. Toselect an internal standard, these must be present in the Analyte menufor them to appear under the Symbol column.


4. Enter the concentration for the internal standard.

5. The default internal standardization method is Interpolate. Interpolatetakes the response of two internal standards (i.e. 9Be and 115In) andinterpolates a linear response between the two masses. That is if 9Be is80% of its reference value and 115In is 90% of its reference value then ananalyte at mass 62 amu (Ni) would have an interpolated value of 85%for the correction.

By default all internal standards are added to the profile for interpola-tion. It is possible to remove internal standards from the profile so theymay be used only as reference points for specific analytes, for example197Au for 202Hg correction. Even internal standards that are used ininterpolation can also be used for specific references.

To specifically reference an internal standard to an analyte choose it inthe drop down menu in the Technique column.

2. To select an internal standard, highlight the required internal standardas shown above for Bi (Be and In have already been selected).

3. Click on the forward arrows to move the analyte across to the inter-nal standard selected box on the right hand side.

1

2

34


3. For the internal standard analytes select none in the method column,by selecting none, a concentration file and calibration will not be as-signed to these analytes.

4. In the right hand table under the Calibration Method menu, select inthe Forcing column the option Through blank by clicking on thedownward arrow to display the dropdown list. Select the Forcingmethod of choice for each isotope (The Through blank option isrecommended).


1. From the menu, select Calibration Method. It is possible to selectdifferent calibration methods for each analyte.

2. To select the calibration method click on the drop down arrow next toeach analyte, to display the dropdown list. Select the calibrationmethod of choice as shown below for each analyte.

1

2

3


6. Select the External drift correction. Calibration blocks are setup,typically every 10-20 samples and a drift correction can be appliedbetween them if this check box is ticked. Note: to enable external driftcorrection to be performed on all samples there must also be a calibra-tion block at the end of the sample list.

7. Select the Calibration concentrations by Element. They can also bedefined by Isotope, but this is only for use when non-natural isotopicabundances occur.

4

5

6 7

5. Tick the boxes in the Semi-Quant column to select the isotopes thatwill be used to create the response curve. This will then be used forsemi-quantitative analysis if required. To build a reasonable semi-quantcurve you need only choose 3-5 analytes which cover the mass range ofinterest and are easily ionized in the ICP, for example Li, Co, In, Tl andU would build a good curve, representative of the mass response of theX Series ICP-MS.



1. Select the Sample List and then again Sample List.

2. Define the Blanks, Standards and Unknowns using the dropdownlist as shown. The blank and standards will turn light blue, this is theCalibration block and can be copied at the end of the sample list andused for External drift correction. (Highlight any sample in the cali-bration block to be copied and right mouse click to append copy - acopy of the whole block will be made).

3. Select number of survey runs and main runs as shown.

4. Select the Fully Quantitative Concentrations for all analytes in allstandards. Enter standard concentrations, use drag and drop to copyacross the columns. The row fill multiplier is very useful when workingwith multi-element standard stocks. Define the concentrations forstandard one and then change the multiplier to 10. Select all the cells inthe first row and then move to the end of the row. Click on the bottomright corner of the selected cells and drag the box down to standard 3.The rows will then be filled as x10 and x100 of standard 1.

1

2


5. Click on File in the Menu bar and select Save as to save the currentexperiment. Alternatively, click on the Queue button to start the acquisi-tion and for any unsaved files it will ask for the experiment to be saved.

5

4



1. To monitor the data acquisition , double click on the MS icon in thelower right corner of the screen to view the PlasmaLab service win-dow.

2. The Real Time Display can be monitored during the acquisition viathe Technician page.

12



1. After the survey run is completed, the results can be viewed. Go toResults, Spectra. A spectra can be viewed by clicking on the crossnext to the sample i.e. survey and stability run to enlarge the menu,then double click on the survey run. The graph below shows thecomplete mass range for the survey run.

2. Select a ‘zoom’ option by clicking the right hand mouse button on thegraph and choosing ‘mode’ from the menu and then ‘zoom fixing y atzero’.

3. Zoom in on an analyte you wish to view more closely (e.g. Pb peaks).Hold down the left mouse button and drag over the Pb peaks(204-210amu).

1

2


The dropdown menu gives a list of options. You can either Undo zoom,this will step back to the previous zoom or Restore to return to theoriginal full mass region. The spectrum can be viewed for either detec-tor mode, or the detector analogue noise can be eliminated. To elimi-nate the analogue noise, place the cursor over View Options and afurther dropdown menu will be displayed, select Eliminate AnalogueNoise.

4. Now the mass spectra shows a zoom in of the mass region. Thespectrum shows both the pulse counting and the analogue data. Clickonce using the right mouse key to show this dropdown menu.

4


4. To identify the analytes with respect to their isotopic fingerprint, clickon the peak of interest and double click on the element of interest ormost likely interferent as shown in box 4. Note: Fingerprinting onlyworks effectively if the analogue noise has been removed.

4


3. Select the SQ-FQ Block from the drop down menu.

4. The response curve is displayed. Any point in the curve can beexcluded by clicking on it (it is then displayed in red when excluded).The response curve values in the grid can then be recalculated byclicking on Refresh.

5. The results of the mass response are displayed in the table.

12

3 4

5


Any standard entered for fully quantitative analyses can also be used toestablish the semi-quantitative response curve. Semi-quantitativeresults can be obtained for any analyte found in the Survey or Mainruns that does not have a standard calibration, by using the responsecurve.

1. Click on Results.

2. Click on Calibration Data to view the results.


6. The accuracy of semiquant values can be refined by adjusting theRSF value of the analyte. This Relative Sensitivity Factor is the mea-sure of the analyte’s response in the ICP-MS compared to the theoreti-cal response. The RSF will change for different plasma and sampleintroduction conditions and it can be useful to build a library of valuesfor different conditions. If a calibrated analyte has not been used tobuild the semiquant curve, it is still displayed and if necessary its cor-rect RSF value can be recalculated. To recalculate a RSF, first dese-lect the point to be recalculated by clicking on it with the leftmousebutton. Then click on the right hand mouse button to select thedropdown list and select Calculate RSF. The corrected RSF valuescan be exported to any Analyte Database for later use with the AnalyteDatabase Wizard on the tool menu.

8. The results of the semi-quantitative analyses of the entire massrange are shown in purple. Selected from Numerical Results and thenSurvey Analyte Dilution Concentration. 20-30% accuracy can beexpected for semi-quantitative analysis, when appropriate RSF valuesare used (see Step 7).

7. Click again in the RSF cell with the left mouse button to display thecorrected RSF value.



1. Click on Results.2. Click on Calibration Data to view the results.3. Select the fully quantitative calibration block for viewing.4. Select the analyte to view its calibration graph.

5. Erroneous points can be excluded from the calibration by clickingwith the left hand mouse button on the point to be excluded as illustratedfor Ba Std 1, the point changes red when excluded.

6. Using the drop down menus in the Curve Fitting Options box achoice of weighting the calibration can be made, default is none. Thecalibration can also be modified to Force through zero, through originor through blank, the latter is recommended.

12

3

4


7. Changes to weighting or forcing can be seen immediately on graph,click on Refresh button to change the grid underneath and recalculatethe whole database.

8. Click on Results and then Numerical Results to view the results,the concentrations can be viewed in the analyte dilution concn. file,the data, mean, SD and %RSD are displayed for all standards andunknown samples.

9. Check the accuracy of the data, and the %RSD should be ingeneral less than 2% (where the concentration is equivalent to approxi-mately >300x the standard deviation of the blank). Any excluded pointsfrom the calibration are shown as shaded regions. To exclude errone-ous data points right mouse click over the cell to be excluded andselect Exclude.

5

6

7


8

9

10. The results display can be modified to display the run times, byclicking on the icon shown.

9

11. Unit sets can be adjusted for individual elements by using the dropdown menu in the cell below the element.

11


13. Using the drop down menu as shown below, the sample list isdisplayed and sample results can be selected.

12. The display parameters can be modified using the Edit displayparameters icon.

12


14. The internal standard is shown in yellow, the table below showsthe mass uncorrected ICPS, and can be used to check that the re-sponse does not change significantly throughout the run. The internalstandard can be displayed as the Internal Response Factor (used in thecalculations) or % internal standard recovery (which is the reciprocal ofthe ISR expressed as a percentage). The % recovery is the value mostpopularly monitored by analysts throughout the world.

14


15. To make any changes to the internal standard, i.e. if the internalstandard is at a higher concentration than expected or unexpectedly ina sample and needs to be deselected, these changes can be made inthe Sample list, click on the sample that needs correcting and selectShow advanced. In the Internal standard folder select New InternalStandard set for this sample, any changes in concentration or select-ing different internal standards or deselecting internal standards can bemade, and a new name will be set for the internal standard for thissample.

15


STEP 11: Printing the Report

NOTE: - Internet Explorer 6 is required to preview and print reports.Internet Explorer should be set up to enable printing of colored back-grounds.

1. This is set up in Internet Explorer, Tools, Internet Options...

1

2. In Internet Options select Advanced, scroll down to Printing andensure the box is ticked for Print background colors and images.

2


3. To display the results for printing, click on Reports.

4. Select the Sections which require reporting by ticking the relevantboxes.

5. Click on the Refresh button to display the report on screen

35

4

6. Click on the Configure the reports settings icon to enable apreview in PlasmaLab or open the report in a windows-associatedpackage, click on Refresh to view the report.

7. Use the Save icon to store the report in the appropriate folder.

8. Results can also be copied and pasted from the results page, byhighlighting the results and right mouse click to copy with headings andthen paste into a Windows associated package i.e. Excel or Word.

9. It is possible to export the data directly to a CSV file (Comma Sepa-rated Variable) from the results grid’s right hand mouse menu. This canbe used for LIMS or MS Excel data processing. The data exported isUNICODE characters to allow international characters to be recog-nized, this means that to import into MS Excel requires the Excel wizardto be used to choose comma as the variable separator.


9


This page is left blank intentionally.

85 Practical E: PlasmaScreen Operation

E: Operating PlasmaScreen

STEP 1: Installing PlasmaScreen

STEP 2: PlasmaScreen Configuration Setup

STEP 3: Tuning PlasmaScreen

STEP 4: Edit New Analyte Database

STEP 5: Create New Experiment


E: How to Operate PlasmaScreen

Objective:To familiarize yourself working with the PlasmaScreen mode of opera-tion. The optimization and the usage of PlasmaScreen in cool plasmaand hot screen modes will be explained in detail. Cool plasma allowsselective reduction of molecular interferences (e.g. Ar, ArO) to aid theanalysis of trace analytes whose nominal mass is identical to that of theinterfering species such as K, Ca and Fe. It is also useful for the analy-sis of easily ionizable elements such as Li and Na. Hot Screen modeallows higher sensitivities to be obtained compared to normal plasmaswith the plasma screen fitted. Tuning is similar to normal plasma exceptthat a little more care is required on the nebulizer flow rate to obtaingood oxide levels (<6% for hot screen mode).

Sample Preparation: Prepare a 10ppb Coand In solution in deionized water, this isused for Cool Plasma tuning. Prepare thesolution just prior to the analysis:1. Blank DI water + 0.05% HNO32. 10 ppb Co and In in fresh Milli-Q water3. 1 ppb screen tune containing Li, Na, K,Ca and Fe

Practical E: PlasmaScreen Operation


STEP 2: PlasmaScreen Configuration Setup

STEP 3: Tuning PlasmaScreen



STEP 6: Viewing the Data



1. The torch has been removed for cleaning and is ready for re-fitting.

The correct alignment of the screen is absolutely vital toperformance. The torch, screen and bonnet are designed so that thescreen location is fixed in the optimum position by way of a quartz pip onthe torch body and a corresponding hole in the screen leg. The pip fixesthe screen position and also serves to fix the bonnet position when thisitem is placed over the screen and pushed back until it touches the pip.

It is important that the screen is located correctly via the pip. If it is not,and is set up such that the screen is protruding from the end of the torch,the plasma is likely to fail to ignite as the ignition spark will arc to theprotruding tip of the nickel screen. This will also damage the screen. Thequartz bonnet must completely cover the screen. If the bonnet does notcover the screen correctly i.e. is not pushed fully back to the screen locat-ing pip or if the bonnet is not fitted at all, the plasma will again fail to igniteand the screen will be damaged.


Ensure that the tab on the screen is fitted correctly into the holder in theblock. The cool gas push fit connector is connected to the torch and linedup with the groove in the cartridge, for accurate alignment of the torch.

Ensure that the cool and auxiliary gas lines are connected securely to thetorch then close the PTFE locking block over the torch and clip it intoplace.

The torch is then connected back to the spraychamber and the torch boxarea is closed ready for operation

One last point to note is that the grounding tab of the Screen must besituated completely squarely over the grounding pin. A good connectionbetween the grounding tab and pin is essential for PlasmaScreen Plus towork effectively. The grounding pin itself should not be visible, as the tabshould cover it completely.


STEP 2: PlasmaScreen Operation & Configuration Setup

1. Switch on the plasma and allow to stabilize for approximately 15minutes.

2. The PlasmaScreen Configuration is setup from the Instrument Con-trol. Click on the Instrument Icon. The configuration relates to thehardware manually fitted to the X Series ICP-MS. A new configurationshould be setup for each hardware configuration. The PlasmaScreen isphysically removed or fitted by the user and so it should have its ownconfiguration (or multiple configurations for different sample introductionsetups if required, i.e. glass concentric nebulizer or ultrasonic nebu-lizer).

3. Click on the Configurations page and Configuration Editor.Setting up of the configuration allows the selection of available acces-sories and the selection of particular preset instrument settings, alsofuture saved tune parameters will be stored here.

21

34


3. If the required Configuration is not available, create a new configura-tion from the icon shown and edit the description.

4. If a required accessory is not available, a new accessory can beselected by following the accessory wizards instructions.

STEP 3: Tuning PlasmaScreen for Cool Plasma mode

The aim when optimizing the tuning parameters for Cool Plasma is toobtain the maximum analyte signal (typically 10ppb 59Co in de-ionizedwater) with minimum 40Ar16O signal.

The main changes in tuning parameters compared to standard modeare: -Reduced RF Power, range 480 to 600WNegative Pole Bias, -10VReduced Extraction, range -80 to -150VHexapole Bias -5VIncreased Sampling Depth, range 100 to 300 (100 steps back fromnormal operating position)Reduced Focus, range 2 to 15VIncreased Neb gas flow 1.0 - 1.1 L/minIncreased Aux gas flow 1.0 - 1.2 L/minIncreased Coolgas flow 14 - 15 L/min

Aim for a Co signal of approximately 10Mcps/ppm and a 40Ar16O contri-bution of approximately 100cps.

The ratio of 59Co/40Ar16O should be a minimum of 100. If it is provingdifficult to reduce the 40Ar16O to 100cps whilst aspirating the 10ppb Cosolution, record the Co signal and aspirate the blank solution (DI water)to remove the possibility of 56 Fe contamination in the Co stock solution.

2. Click on the required PlasmaScreen configuration. Select the re-quired accessory.

5 6


1. Click on Tune in the instrument section. Click on Major, these pa-rameters have the greatest effect on the tuning.

2. Use the slider to select the default settings as shown.

3. Click on Minor, these parameters are generally for fine tuning, how-ever, for Cool Plasma mode of operation ensure that the ForwardPower is set to low power as shown.

1

3

2

4. Aspirate the 10ppb Co solution to optimize the tuning. Adjust the RFpower, lens settings and nebulizer flow rate to obtain the required ratio.Once the required 59Co/40Ar16O ratio has been achieved, save theinstrument settings. The ratio can be monitored in the real time display.



1. For the use of PlasmaScreen with Cool Plasma an Analyte Data-base is required to enable the monitoring of 40Ar for the major Caisotope. A default analyte database for cool plasma operation is pro-vided but this can be edited or a new one created if required. Click onFile, New and Analyte Database to create a new one.

2. The database scan regions have to be altered to enable the analy-sis of 40Ar. Select the scan and skip regions by clicking on them in thegraphic. Click the right hand mouse button on the graphic to add orremove scan regions. Alternatively, type in values in the box on left handside for each individual scan region.

2

1


4. Save As a new analyte database in Data folder as DefaultPlasmaScreen.tea.

3. Add matrix and polyatomics in the database as shown. Click onNew to add any polyatomics or matrix ions common to the samplesbeing analyzed. The species shown below are defaults to all data-bases, any unwanted ones can be removed by right hand mouse click-ing on the highlighted species in the list and choosing delete.

4

3



Aim: Detection Limit determination of PlasmaScreen elements.

1. Select Create a new blank experiment from the experiment wiz-ard, by clicking on the experiment icon.

2. Select the PlasmaScreen Analyte Database previously created forthis experiment, or the default database for cool plasma provided withPlasmaLab.

1


3. In the Setup and Configurations Editor select the Configurationfor PlasmaScreen by ticking the Use box. This can be left ifPlasmaScreen is the current configuration anyway.

4. The Available Accessories and Devices are pre-selected in theinstrument control. If an accessory is not available select the accessoryusing the instrument icon and accessory wizard as described in Sec-tion A, before continuing to edit the Experiment.

5. Select the current Instrument settings by ticking the Use box. Thiscan be left unticked if the current instrument settings are to be used.However, instrument settings must be selected if multiple settingssets are to be used (i.e. Cool Plasma and Hot Screen mode in thesame acquisition).

3

4

5

6. In Setup, Timings select the time for the uptake, measured by thetime taken for the sample to reach the plasma and washout is typicallyset between 30 to 90 sec depending on the sample matrix and concen-tration.

6


7. Select the analytes from Setup and Analyte menu as shown, for theDetection Limit determination the analytes 7Li, 23Na, 39K, 40Ca and 56Feare selected. Note that 40Ca can now be selected, which is the mostabundant isotope of Calcium. CAUTION!! Take care not to use 40Ca innormal or hot screen plasma conditions as the high levels of 40Ar

7

8. Set up the Acquisition Parameters for a Survey run and PeakJump Main run. The default parameters are shown below.

produced will cause high count-rates to be seen on the detector. Eventhough the X series ICP-MS has a mechanism to handle trips on thedetector the detectors lifetime will suffer when exposed to high levels forprolonged periods.

8


11. Enter the Sample list as shown for the DIW Blank and the 1ppbStd. Note that 10 repeats are selected for the blank for detection limitdetermination.

9. Select Calibration Method. Select the Method from the drop downmenu as Fully Quant for all analytes.

10. The remaining parameters are set as default as shown, with theexception of Forcing which is recommended to be set as ForceThrough Blank selected from the drop down menu.

12. Add the Fully Quantitative concentration of 1ppb.

12

9

10

11

13. Save and Queue the experiment.

14. Calculate the Detection Limits via the Analyte Dilution Conc page,by using a user pre-dilution factor of 3. This will show a blank standarddeviation of 3x the actual blank standard deviation i.e. equal to the 3sigma detection limit.



99 Practical F: CCT Operation

F: CCT Operation

STEP 1: CCT Setup

STEP 2: Tuning CCT

STEP 3: Tuning CCTED

STEP 4: Example CCT Experiment

STEP 5: Data Interpretation


F: CCT Operation

Objective:To familiarize yourself working with the CCT option. The optimizationusing Collision Cell Technology and the use of different gases will beexplained in detail.

F: CCT Operation

STEP 1: CCT Setup

STEP 2: Tuning CCT


STEP 4: Example CCT Experiment


Solution required for this practical:Prepare a 10ppb Tuning Solution con-taining Co, In, Ce and U in 2% HNO3.Recommended gas for multi-elementanalysis is a 8% H2 in He mix.


STEP 1: CCT Setup

1. The gases required to run CCT are setup within the instrument con-trol, the accessories required for the experiment can also be configuredfrom here. Click on the instrument icon to open the instrument control.

2. A new configuration can be created using Configurations menuand the Configuration Editor page, in which all the new instrumentsettings will be stored. Click on the New Configuration icon.

3. Enter a configuration description as shown (i.e. CCT Default) andtick the Use box for the new configuration.

4. The Additional Mass Flow Controllers required to control thegases for CCT must be set up within the Configuration Editor. Type inthe name of the CCT gas in the Identifier box and select the correctgas in the Conversion Factor box by clicking on the downward arrowin the right hand side of the box to display the menu. The conversion isrelated to Helium gas (i.e. He factor equals 1.0). For mixed gaseschoose the setting for the bulk gas.

2

3

4


5. To add a gas conversion or edit a gas conversion right mouse clickon the row to be edited, to display the options.

5

STEP 2: Tuning CCT

1. Before tuning the CCT it is recommended to have good standardmode tuning first.

2. Set the chosen CCT Mass Flow Controller(s) to 6 ml/min for a mini-mum of 30 seconds to purge the lines before tuning. If the CCT optionhas not been used for several days, the gas supply has been changedor if a leak in the lines has just been fixed, the gas lines will need to bepurged overnight, to remove entrained water vapour (this increasesoxide formation and affects CCT performance).

3. The typical tuning parameters for CCT are shown in the table below.The main differences between standard mode and CCT tuning is thatthe Pole Bias is set to negative, (usually -10 V), the Hex Bias is also setto negative, typically about -5V, and the Focus drops from around +19Vto approximately 0 to +5 V, depending on the type of interface conesbeing used.


5. Tune the gas flow rate and lenses to give low counts at mass 56 ArO,while keeping good transmission at 59Co, 115In and 238U. Typical gasflows when using 8%H2 in He mixture is in the range 4 - 7 ml/min.

6. Extra instrument parameters can also be monitored when tuning, byclicking on the downward arrow key in the Monitor box as shown.

4. In Instrument control / Tune, monitor the elements 59Co, 115 In(target 300000 cps) and 238U for maximum signal, also maximize theratio 59/56 (target >200).


The purpose of CCTED is to allow the interferences from the plasma tobe removed whilst screening out or preventing the formation of newinterferences in the collision cell.

1. Before tuning the CCTED mode, there must already be a good CCTtuning (see Step 2). Select a saved CCT tune file as shown below.


Example CCT Experiment:

Now that the signal has been optimized, the system is ready for analysis.An experiment can be set up to scan over the 70 to 90 mass region anduse the PlasmaLab fingerprint function to place the isotopic fingerprint ofSe on mass 80, and As mass 75. To demonstrate the removal of Ar2(mass 80) and ArCl (mass 75).

Solution required for this practical: :Prepare a 10ppb solution of Co, As andSe in 5%HCl and a 5% HCl blank.

2. Starting with the Hex Bias reduce the differential between it and thePole Bias towards zero, while monitoring the 115 In for maximum signal(target 50000cps) and minimizing the CeO/Ce ratio (target 0.03).

The Pole Bias can be increased slightly (typically to -9.5V) and theHexapole biasset to -10V to achieve CCTED conditions. This sets up asmall energy discrimination barrier between the hexapole and thequadrupole. By changing the magnitude of this barrier, oxide and otherpolyatomic interference transmission can be dramatically reduced, butat the expense of sensitivity .


STEP 4: Create an Experiment

1. Create a new blank experiment

1

2. Select the Default CCT.tea database, this database allows scan-ning over previously skipped regions such as 40Ar (40Ca), 75ArCl(75As), 80Ar2 (80Se). Due to interference attenuation of Argon basedpolyatomics.

3. Define the Analyte menu for Co, As and Se. The major Se isotope atmass 80 can now be selected.

4. Any default interference equations that were present for interferenceson As and Se can be removed by right mouse clicking on the Equationbox to view the drop down menu, and select Disable interferenceequation.


3 4

5. Select the Acquisition Parameters as shown below for Main-Scanonly.

6. Use the right mouse click to view the menu to change between Addor Remove Regions if required on the graphic of the mass range.

7. Set the scan region to include the range from mass 23 to 85, pointthe mouse over the scan region and left mouse click and drag over theregion to be included.

5


8. Define the sample list for the analysis.

8

9. Save the experiment as ‘CCT scan As, Se, Co’.

9

10. Queue the experiment.



View the spectra in Results, Spectra and double click on both blankand sample survey. Zoom in to region between mass 70-85 amu toshow removal of ArCl (mass 75) and Ar2 (mass 80), enabling 10ppb As(mass 75) and Se (mass 80) to be measured easily, in a high chloridematrix.

109 G: Maintenance and Troubleshooting

G: Routine Maintenanceand Troubleshooting

Part A: Routine Maintenance

STEP A1: Peristaltic Pump TubingSTEP A2: Spray ChamberSTEP A3: Removing the GlasswareSTEP A4: Cleaning the GlasswareSTEP A5: Nebulizer MaintenanceSTEP A6: Refitting the GlasswareSTEP A7: Cleaning the ConesSTEP A8: Replacing the MultiplierRoutine Maintenance Checklist

Part B: Troubleshooting

STEP B1: Instrument will not go from Vacuum Ready to OperateSTEP B2: Sensitivity ProblemsSTEP B3: Signal Drifts with TimeSTEP B4: Poor Stability


G: Maintenance and Troubleshooting

Objective:Part A takes you step by step through all aspects of routine mainte-nance. Part B goes through the most typical trivial problems whichmight occur with the instrumentation.


STEP A1: Peristaltic Pump Tubing

STEP A2: Spray Chamber

STEP A3: Removing the Glassware

STEP A4: Cleaning the Glassware

STEP A5: Nebulizer Maintenance

STEP A6: Refitting the Glassware

STEP A7: Cleaning the Cones

STEP A8: Replacing the Multiplier

Routine Maintenance Checklist


STEP B1: Instrument will not go from Vacuum Ready toOperate

STEP B2: Sensitivity Problems

STEP B3: Signal Drifts with Time

STEP B4: Poor Stability



This section contains general maintenance instructions for the X SeriesICP-MS. If followed these instructions will get the best possible perform-ance out of the instrument. The X Series ICP-MS is a precision instrumentwhich will give many years of high performance if it is properly and regu-larly maintained.

CautionTake care to wipe up any spillages that occur when handlingacids or organic solvents near the instrument, otherwise theenamel coating may corrode.Before using any cleaning or decontamination methods except thosespecified by the manufacturer, usersshould check with themanufacturer that the proposed method will not damage theequipment.

Pay particular attention to the area inside the Torch Box where the sampleintroduction glassware is mounted. Acids can tarnish the surface finish, sowipe up spills (wear protective gloves while doing this).If for any reason you wish to clean the instrument panels, use a dilute soapsolution and paper towels to wipe down the panels.

STEP A1: Peristaltic Pump Tubing

The condition of the Peristaltic Pump tubing can affect the stability of theion beam and therefore should be replaced regularly. For a typical 40 hourworking week it is recommended that the tubing is replaced weekly.

1. Remove the Sample Uptake tube from the sample and drain theSample Introduction Glassware and all tubing. Stop the Peristaltic Pumpusing Accessories Control.

2. Wipe the surface of the Peristaltic Pump rollers and tension arms with adry cloth to remove any dust.

3. Replace the Sample Uptake tubing with a length of 0-2 ml/min Tygon®

tubing with Orange/Yellow collars (Thermo Elemental P/N 1200211). If itproves difficult to insert the PTFE tubing in the ends widen them by insert-ing the end of a clean micro pipette tip.

4. Replace the drain tubing with a piece of 0-5 ml/min Tygon® tubing withWhite/Black collars (Thermo Elemental P/N 1200212).


STEP A2: Spray Chamber

Due to the acidic nature of most sample types in ICP-MS, the “O” ringsat the rear of the Impact Bead Spray Chamber which secure the Nebu-lizer in place can degrade and become brittle over time. This can beobserved as a discoloration of the “O” rings. This can lead to leakageof the Nebulizer gas from the rear of the Impact Bead Spray Chamberand poor signal stability. Old “O” rings should be carefully removedusing a set of tweezers and replaced with two Kalrez “O” ring seals(Thermo Elemental P/N 1201833). Ensuring that an adequate rinse isused at the end of a sample set with the rinse being a non-aggressivesolvent will prolong the lifetime of the “O” rings.

5. Place the two pieces of Tygon® around the barrel rollers, taking careto ensure they are not twisted, and secure in place using the collars andbrackets. Attach the tension arms. Ensure that the tygon tubes are fittedfor correct sample and drain flow direction when the peristaltic pump isoperating.

6. Switch the Peristaltic Pump back on; check that sample is beingtaken up into the instrument and being drained efficiently. If needed,adjust the tension on the Tygon® tubing using the thumbscrews on theperistaltic pump, but do not over-tighten, as this will reduce the tubinglifetime.

7. If an Autosampler is being used, renew the wash station tubingwhenever the sample uptake and drain tubing are changed. If thesample to be analyzed contains a high percentage of organic solvent,the Pump Tubing should to be replaced with solvent resistantIsoversinic Pump Tubing. The Uptake Tube has an inner diameter of 0.5mm (Thermo Elemental P/N 1200092) and the wider drain tubing hasan inner diameter of 2 mm (Thermo Elemental P/N 1200093).


STEP A3: Removing the Glassware

Removal and cleaning of ICP glassware and fittings is carried out toreduce blank levels for elements which tend to accumulate on theglassware. For higher productivity, Thermo Elemental recommendsthat two sets of glassware are available for use, one set in the X SeriesICP-MS and one set being cleaned in preparation for use. Alternatively,if the analytical program alternates between ultra trace determinationand relatively high level / complex matrix work, then a complete set ofglassware and cones should be assigned to each.

1. Switch the X Series ICP-MS into Operate Mode and rinse thesample tubing and glassware by aspirating de-ionized water into theImpact Bead Spray Chamber.

2. Switch the X Series ICP-MS off, into Vacuum ready and drain thecomplete Sample Introduction System.

3. Release the push-fit connector on the Nebulizer gas line, and withgreat care, gently remove the Nebulizer from the rear of the ImpactBead Spray Chamber.

Tip: To remove the push-fitconnectors, push the collartowards the connector bodywhilst gently pulling the tubeaway from the connector.


5. Lift up the slider that holdsthe Peltier cooler in placearound the Impact BeadSpray Chamber and place itinto the higher rest position,gently remove the SprayChamber from the X SeriesICP-MS.

6. Release the two push fit connectors that supply the coolant and auxiliarygases to the Torch.Release the metal clip on the PTFE block that holds the Torch in place,slide the transfer tube (elbow) backwards away from the torch and gentlypull the Torch clear of the block and coil.

4. Open the Torch box coverthen open the Torch box RFshield. Remove the metalclip which fixes the transfertube (the ‘elbow’) to the rearof the Torch.


STEP A4: Cleaning the Glassware

WARNING!When handling the corrosive acids required to perform the cleaningprocedure described below take the following precautions:• Wear protective clothing.• Always use acid resistant laboratory gloves and glasses.• Make yourself aware of all safety procedures in case of spillage

or exposure to the skin or eyes before commencing the cleaning.• The acid cleaning of the glassware should take place in a fume

hood.

1. The Torch, Impact Bead Spray Chamber , Transfer tube and Nebu-lizer may be cleaned by soaking them in a laboratory glassware cleaner(e.g. 5% Decon 90 or similar) for 30 minutes. Raising the temperaturespeeds up the process.WARNING! Do not boil the liquid when cleaning polypropylenecomponents as the plastic will degrade; 50 - 60 degrees is suffi-cient.

2. Rinse at least three times with de-ionized water. Insert the ImpactBead Spray Chamber in 10-20% Analar grade nitric acid and until theglassware is required for use. For a thorough clean, the soaking periodshould exceed 6 hours. Alternatively items can be cleaned in less thanan hour with an ultrasonic bath and the same cleaning solution.

Release the metal clip

Release the push fit forthe Aux and Cool gas.


STEP A5: Nebulizer Maintenance

The X Series ICP-MS is supplied with a Glass Concentric type Nebu-lizer. With use these Nebulizers may become blocked. A blockage istypically caused by either particulate matter present in the supply gasor in the sample. To prevent Nebulizer blockage follow these generalrules.1. Filter the supply gas by installing a low impedance gas filter in-line. This prevents particulate matter present in the gas or gas lineslodging in the Nebulizer.

2. Filter the sample. This is recommended provided the solidmaterial present in the sample is not of analytical importance. Typicallythe Nebulizer will not lose efficiency when analyzing samples contain-ing small particle size matter because the design of the sample capil-lary is sufficiently robust for the analysis of such samples.

3. Rinse the Nebulizer. This is extremely important when switchingthe X Series ICP-MS off at the end of a sample analysis. Solids maydeposit in the nozzle restricting the Nebulizer and causing a loss inperformance. Allow the Nebulizer to dry before turning off the gassupply. Make sure that the sample uptake tube is disconnected orarranged so as to prevent siphoning into the Nebulizer when the gas isswitched off. This procedure also extends the lifetime of the “O” ringsfitted to the Impact Bead Spray Chamber.Should the Nebulizer become blocked, apply compressed gas to the

3. Prior to re-installing the glassware, remove from the nitric acid andwash at least three times in fresh de-ionized water. Finally allow to airdry completely. If any components are to be stored for some time be-fore use, they should be placed in metal free sealed plastic bags.

4. The Torch should be replaced (Thermo Elemental P/N 3600969) ifsignificant devitrification of the injector tip is evident, as this can pro-duce high blanks for sodium and other analytes.

5. Using a magnifying glass inspect the tip of the Nebulizer. If the tipappears damaged in any way, it should be replaced (Thermo ElementalP/N 4600294). Damaged Nebulizers can give rise to poor stability andsample transport efficiencies.Replace the “O” rings in the rear of the Impact Bead Spray Chamber ifthe nebulizer seal is not good. If there is any damage evident to theImpact Bead Spray Chamber, then it should be replaced.


Warning!When handling the corrosive acids such as aqua regia take thefollowing precautions:• Wear protective clothing.• Always use acid resistant laboratory gloves and glasses.• Make yourself aware of all safety procedures in case of spillage

or exposure to the skin or eyes before commencing the cleaning.• Preferably the acid cleaning of the glassware should take place

in a fume hood.• Follow local health and safety procedures.

If the nozzle is coated in crystalline deposits then a soak in dilute nitricacid (2%) is sufficient.

Caution!DO NOT use an ultrasonic bath to remove blockages or duringNebuliser cleaning as cavitation and ultrasonic vibrations can causeirreparable damage to the Nebuliser tip.

STEP A6: Refitting the Glassware

1. Attach the push fit connectors containing the auxiliary and cool gaslines to the arms of the Torch. The cool gas arm of the torch is lined upwith the groove in the cartridge, in this way the torch is always aligned inthe same place.

2. The PTFE block cartridge is closed over the torch and the metal clipis secured in place.

3. Replace the transfer tube, then the Impact Bead Spray chamber.Secure the transfer tube to the torch and spraychamber using the clipsprovided. If using a peltier cooler, lift the top half of the peltier cooler intoplace around the spraychamber from its rest position.

4. Attach the Nebulizer to the Nebulizer gas line using the push fit con-nector.

5. Plug the Push-Fit connector of the Nebulizer sample uptake tube intothe Nebulizer supply and gently push the Nebulizer into the rear of theImpact Bead Spray Chamber. Take care not to damage the tip.Attach the drain tube to the drain adapter, and secure onto the ImpactBead Spray Chamber. Replace the Torch box RF shield and close theTorch Box door.

nozzle and backflush the blockage. Alternatively flush the Nebulizer witha 3%-5% solution of aqua regia.


STEP A7: Cleaning the Cones

The condition of the cones affects sensitivity, blank levels and themagnitude of signals from some background species, particularly oxidespecies. The actual intervals at which cleaning is required depends onthe analytical workload and the nature of the samples being analysed,particularly the level of dissolved solids in the samples being aspirated.The cones are manufactured to high precision from pure Ni and shouldbe handled with care, particularly the skimmer. The tip of the skimmercone is fragile and as such is easily damaged.

1. Open the Torch Box door, to release the clip between the Torch Boxturret and the interface region. Push the Torch Box enclosure away fromthe rest of the instrument to reveal the interface region.

2. Using the sample cone tool provided, unscrew the locking collarholding the sampler in place. Should the sample cone be stuck, care-fully insert a small flat screwdriver into the edge of the sampler to gentlyprise it away from the Interface front plate. If the graphite gasket isdamaged, it should be replaced (Thermo Elemental P/N 3004382).

Remove the samplingcone first.

Use the sample conetool to unscrew thelocking collar of thesample cone.


3. Inspect the sample cone for excessive wear around the orifice, replaceif necessary (Thermo Elemental P/N 3004661 for X7/HPI interface orP/N 3600812 for X5/Xi interface)).

4. To clean the sample and skimmer cones, place in an ultrasonic bath in~5% Decon 90 (or similar laboratory detergent) for approximately 15min.Rinse with de-ionized water, then ultrasonicate for 15min with de-ionizedwater. Dry carefully with a non-fibre shedding laboratory wipe, or leave toair dry..

5. If further cleaning is required, (i.e. if performance expectations cannotbe met), clean the front and rear surfaces of the sample cone by gentlyrubbing from the center out with an abrasive pad such as Scotchbrite™(Thermo Elemental P/N 1026048) or alternatively apply a fine abrasivemetal polish such as Polaris (Thermo Elemental P/N 1041300) madeinto a paste with de-ionized water. Pay most attention to the area aroundthe orifice. All polish or abrasive fibres must be removed before refitting.Place the sample cone in 2% nitric acid in an ultrasonic bath for 2 min-utes then rinse thoroughly with de-ionized water and finally dry carefullywith a non-fibre shedding laboratory wipe, or leave to air dry.

Caution!: Do not rub abrasive material over the tip of the cones, theedges of which must be sharp and regular.

When removing the lockingcollar, hold the skimmercone in place with onefinger as illustrated. Thenremove the skimmer conefor cleaning.


6. The skimmer cone is less mechanically robust than the sample coneparticularly at the tip, the edges of which must be sharp and regular. Ifthere is evidence of damage to the tip it should be replaced (ThermoElemental P/N 3200860 for X7/HPi interface or P/N 3600811 for X5/Xiinterface). The skimmer cone must therefore be handled with extremecare. The procedure for removal is as follows;· Remove the skimmer cone through the sample cone hole in the frontplate, by inserting the recessed cone tool and aligning the two lugs inthe cone tool in the outer edge of the cone surface, then turning counterclockwise, it will be held in place magnetically.· Inspect the skimmer and reject it if damage is apparent.· Clean the skimmer cone by placing in an ultrasonic bath in ~5%Decon 90 (or similar laboratory reagent) for approximately 15min.Rinse with de-ionized water, then ultrasonic for 15min with de-ionizedwater. Dry carefully with a non-fibre shedding laboratory wipe, or leaveto air dry.· If further cleaning is required clean the front and rear surfaces of thecone by gently rubbing from the center out with an abrasive pad such asScotchbrite™ (Thermo Elemental P/N 1026048) or alternatively apply afine abrasive metal polish such as Polaris (Thermo Elemental P/N1041300) made into a paste with de-ionized water. Pay most attentionto the area around the orifice and clean with extreme care. The rear ofthe orifice may be reached using a cotton bud and Polaris. All polish orabrasive fibres must be removed before refitting. Place the cone in 2%nitric acid in an ultrasonic bath for 2 minutes then rinse thoroughly withde-ionized water and finally dry carefully with a non-fibre sheddinglaboratory wipe, or leave to air dry.

7. Inspect the 28 x 1.5 mm “O” ring which sits behind the skimmer conefor damage and replace if necessary (Thermo Elemental P/N1201240).

8. Reassemble the Interface in reverse order. Ensure that the skimmeris seated properly and that the front plate and sample cone seals are inposition and clean. Tighten the sample and skimmer cones finger-tightto give a good thermal and vacuum seal. Move the Torch Box back intoposition and close the Torch Box door.

Warning! Be careful to push the torch box enclosure into posi-tion with the door open to avoid damage to the interlock key.


STEP A8: Replacing the Multiplier

2. Switching to Shutdown Mode

With the X Series in Vacuum Ready mode click on the OFF button.

1. Always wear powder and lint free gloves when handling componentsinside the vacuum system.

Close the lid of the Analyser Chamber whenever you are not activelyworking inside it.

This document details the procedure for replacing the AF214Simultaneous Multiplier used in the X Series ICP-MS. The X Series hasbeen specifically designed by Thermo Electron to enable easy accessand replacement of this part.

Please note that when replacing a multiplier you will be entering thevacuum system of the instrument. In order to maintain the optimumperformance of your X Series, it is important that you follow the simpleprecautions below to ensure that the vacuum system does not getcontaminated during this process:

When prompted, clickon YES

Leave the instrument for 5 minutes to vent fully.


3. Removing the existing Multiplier

Remove the main left handside cover and store care-fully.

Undo the 3 clips holding theAnalyzer Chamber Lid.


Open the lid and remove theexisting multiplier. Closethe lid until you are ready tofit the new multiplier, makingsure that the o-ring sealaround the chamber top islocated fully in its groove.


4. Fitting the new Multiplier

Carefully close the Ana-lyzer Chamber lid, mak-ing sure that the o-ringaround the chamber topis located fully in itsgroove, and secure the 3clips which hold the liddown.

Only unpack the multiplierimmediately before fitting,and install immediately. Donot expose the multiplier toair unnecessarily. Removethe new multiplier from itspackaging and place withcare in the locating slotsprovided in the base of theAnalyzer Chamber.


Replace the main left handside cover.

5. Switching to Vacuum Ready Mode

In PlasmaLab click on On and select YES at the prompt.


Each time the turbo pump is started the user will be prompted to say if anew detector has been fitted.

If no is selected then no further action is taken and all information for theDetector monitoring and Cross Calibration continues to be stored for thecurrent detector. If Yes is selected then the user will be prompted to enterthe serial number for the new detector. The number can be found on theside of the box containing the new detector.

NOTEIT IS HIGHLY RECOMMENDED THAT NEW DETECTORS GO THROUGHTHE BURN-IN PROCEDURE. FAILURE TO DO THIS COULD SERIOUSLYIMPACT THE LIFETIME OF THE NEW DETECTOR.

If No is selected for out gassing the new detector, the old detector data isarchived and new records created for the Detector Monitoring and CrossCalibration. If Yes is chosen for the out-gassing then the new records arecreated and the out-gassing dialog is shown.


This dialog shows the progress of the out-gassing and any events (forexample that the out-gassing has not started because the vacuum has notreached the trip point yet). The dialog can be minimised and PlasmaLabused to process data but while the detector is out-gassing no analysiscan be done. The out-gassing can be aborted or paused and a note willbe made in the event log for that detector. Once the automatic out-gas-sing is complete a message will be shown and analysis can begin.

If the turbo pump has been switched off for more than one hour, when it isrestarted if the user chooses No to the New Detector dialog the followingdialog is presented.

NOTEIT IS HIGHLY RECOMMENDED THAT ALL DETECTORS GO THROUGHTHE BURN-IN PROCEDURES. FAILURE TO DO THIS COULD SERIOUSLYIMPACT THE LIFETIME OF THE NEW DETECTOR.


At this point the Detector Monitoring page will begin showing the informa-tion for the new detector. The various parameters can be displayed usingthe options on the right of the page.

This data will show every voltage change made on the detector whetherautomatically by the instrument calibration software or manually from thetune page. Monitoring data for older detectors can be viewed by using thedrop down dialog box at the top of the page. It is possible to export themonitoring data to a file using the export button.

NOTEWHENEVER A NEW DETECTOR IS FITTED, PLEASE EXPORT THEMONITORING DATA FOR YOUR OLD DETECTOR AND E-MAIL IT [email protected]. THIS WILL HELP THERMOELECTRON IMPROVE THE LIFETIME OF DETECTORS GOING FORWARDBY ANALYSING THE DATA FOR THE PARAMETERS THAT EFFECTDETECTOR PERFORMANCE.

To view parts of the data in more detail the zoom tools can be used.

To highlight any events that occurred in the zoomed region of the graph,the highlighting tools can be used to show the information in the tablebelow the graph.

On this page it is possible to view the changes that have taken place onthe instrument during the lifetime of the detector. The main purpose is fordiagnostic reasons allowing any problems that may contribute to thelifetime of the detector to be tracked.

6. Detector Monitoring


Routine Maintenance Checklist

DailyInspect and clean cones if necessary (if performance is notacceptable)Complete instrument log

WeeklyPrepare fresh performance monitoring solutionReplace sample and drain peristaltic pump tubingExchange ICP glassware (optional)Clean removed glassware ready for next exchange (optional)Clean spray chamber drain plugClean nebuliserCheck air filters and clean if necessaryCheck multiplier voltages and do a cross calibration

MonthlyReplace sample uptake tubingCheck rotary pump oilCheck oil mist filtersCheck chiller water level in reservoir

Note: 6 / 12 monthly should be carried out by a qualifiedservice engineer.

Six Monthly (Thermo Elemental engineer servicing)Examine lens system and clean if necessaryExamine penning gauge and clean if necessaryChange rotary pump oil

AnnuallyReplace any worn 0-rings



This section will help you to diagnose a particular problem, and willrecommend remedial action. Many problems in high performanceinstrumentation are the result of trivial concerns, usually after someroutine maintenance, or if another operator has left the instrument in anon-standard configuration.

The two rules of diagnosing potential problems are to:- Examine the recent history of use of the instrument- Consider the simple causes first (sample introduction is more likelythan quadrupole failure!)

The single most useful ‘tool’ for probing analytical concerns and hard-ware problems is the daily instrument log. Once a day (when in use)following the routine tuning procedure, the lens, gas and RF settingsshould be documented, and a short term stability test and a scan,performed. Hard copies of settings, stabilities and once a week spec-tra should be put into the log book.

If you have any doubts about the performance of your instrument trainedThermo Technical Support personnel are always available to assist you,however trivial you think the problem may be.

Step B1 – Instrument will not go from Vacuum Ready to Operatemode

If the instrument does not respond to any command check that theinstrument and data system are communicating via the PlasmaLabservice icon. If required, stop and restart the service.

When Plasmalab fails to start the instrument successfully a fault mes-sage is placed in the Technician / Event Log. You should view thismessage first as it is the quickest and easiest way to pinpoint theproblem. (Note: The Technician icon changes from yellow to red if aproblem is detected).

One of the most common causes of the instrument not starting is failureto light the plasma. The Flowchart shows a simple step-by-step guidewhich covers the most frequent causes of this failure.


Plasma will not light

Check that all the Plasma interlocks are satisfied on the Advanced page of PlasmaLab

Check all gas lines are securely connected, free from kinks and not trapped.

Check the PlasmaTorch is in good condition with no cracked or melted areas

Check the Nebulizer is fitted securely and the black nebulizer readback arrow on the Minor Tune page goes to 0 during ignition

Check the ignition Power in the Advanced page of PlasmaLab is set to 800W or greater and the Post ignisition power is set to 1200W

Check the condition of the Cooling water. Contamination of the water increases the conductivity of the

NO

If individual interlock is not satisfied check the following

Hood Closed - Check that the Faraday Cage door is closed and firmly secured

Coil Water - Check that external water supply is switched on and filter on rear of X Series is not blocked

Expansion Temp -Check temperature of sample interface. If hot check temperature of chiller water. If cold sensor is faulty.

Ar OK (Gas Control Module) - Check that Argon supply is switched on and can supply 80psi


STEP B2: Sensitivity Problems

The majority of concerns over performance surround an aspect of signalsensitivity. In most cases, the problems are trivial, caused by a recentchange in the sample introduction system or tuning, and can be ad-dressed with ease; only occasionally are they caused by failure of acritical component.

The daily log of instrument performance is most useful, you should checkthe previous days log and make sure that none of the instrument param-eters have changed significantly. Use the guide below to help diagnosethe problem.


No or Low Sensitivity

No

Check Detector voltages are set correctly and readback are correct.

Check solution concentration

Check Nebuliser pressure is >1bar and stable. Check you can see aspirated sample in the spray chamber

Check instrument is in Operate mode and slide valve is open

Check that the Detector is switched on in the Advanced page of PlasmaLab and the HT readbacks are correct

Check that the cables from the Detector PCB to the embedded PC are securely connected

No signal

Poor sensitivity

No PC signal

Yes

Check Pulse Count for a known analyte peak. If necessary check mass 56. Can you see a peak?

Check Analogue signal on mass 56. Can you see a peak?

No

Check Cool and Auxiliary Gas flow read backs are correct and stable

Check that Torch translation optimizes in the Horizontal and Vertical. If necessary use mass 56.

Check the expansion pressure is approx. 2mbar and the cones and sample cone gasket are in good condition

Monitor the Lens slider readbacks and check they are stable and match the setpoints

Call for Service Support


STEP B3: Signal Drifts with Time

The usual cause of signal drift is deposition of matrix on the sample andskimmer cones. As material builds up, the sampling and skimmer ori-fices become smaller, and the total ion beam is reduced. Removal andcleaning of the cones will resolve this problem.

If however, you suspect an instrumental drift, perform a short term stabilitytest and examine the %RSD’s obtained. Use the guide below to diag-nose the problem

1. Ensure that the total dissolved solids level of the solution being aspi-rated is below the recommended levels (i.e. < 0.2% m/v).

2. Check that the laboratory temperature is stable.

3. Check that the temperature of the coolant water being supplied to theinstrument is stable.

4. Monitor the temperature of the Peltier control (where fitted) and checkit is stable.

5. Monitor the Nebulizer Slider Control read back and check that it isstable and matches the Nebulizer Slider set-point.

6. Monitor the Nebulizer Pressure value. It should be stable and consis-tent with values previously recorded for the same nebulizer/flow condi-tions.

7. Inspect the sample introduction system and ensure all components arecorrectly fitted and all connections are secure.

8. Check that the tension on the peristaltic pump tubing is correct and thepump tube is in good condition.

9. Monitor the Lens Slider Control read backs and check they are stable.Set the Real Time Display to monitor a low, mid and high mass peak(e.g. Be, In, U). Check that the mass calibration is accurate.


STEP B4: Poor Stability

Stability is interpreted as the ability of the instrument to produce good%RSD values on repeats of the same sample (sometimes defined as theinternal precision). Poor stability is often the reason behind a set of databeing discarded. Sample matrix can have an effect on stability, especiallyif the nebulizer cannot form a stable aerosol. System related stabilityproblems will occur if when running a standard tune solution, short termstability test %RSD’s worse than 2 to 3% are obtained.

1. Ensure that the total dissolved solids level of the solution being aspi-rated is below the recommended levels (i.e. < 0.2% m/v).

2. Check that the laboratory temperature is stable.

3. Check that the temperature of the coolant water being supplied to theinstrument is stable.

4. Monitor the temperature of the Peltier control (where fitted) and check itis stable.

5. Monitor the Nebulizer Slider Control read back and check that it isstable and matches the Nebulizer Slider set-point.

6. Monitor the Nebulizer Pressure value. It should be stable and consis-tent with values previously recorded for the same nebulizer/flow condi-tions.

7. Inspect the sample introduction system and ensure all components arecorrectly fitted and all connections are secure.

8. Check that the tension on the peristaltic pump tubing is correct and thepump tube is in good condition.

9. Monitor the Lens Slider Control read backs and check they are stable.Set the Real Time Display to monitor a low, mid and high mass peak (e.g.Be, In, U). Check that the mass calibration is accurate.

Documents

X Series Getting Started Guide