ICP analysis with version 5 software.docx
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ICP analysis with version 5 software.docx
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ICPanalysiswithversion5software
HOWTOREALIZEANANALYSIS
INICPWITHVERSION5SOFTWARE.
CONTENTS
1Introduction5
2Enteringthesoftware5
3Lightingtheplasma5
4Methodcreation7
5Methodoptimization10
6Standardpreparation.15
6.1Standards15
6.2Re-slope16
6.3Concentrationrange18
7Calibration18
8Analysis20
Analysisreport20
SCREENS
Screen1:
Plasmacontrol5
Screen2:
Useridentification6
Screen3:
Softwarepresentation6
Screen4:
Newmethod7
Screen5:
Choiceoftheelements7
Screen6:
Concentrationrange8
Screen7:
Linescharacteristics8
Screen8:
Methodparameters9
Screen9:
Operatingconditions9
Screen10:
Standards10
Screen11:
Concentrationrange10
Screen12:
Sequence11
Screen13:
Sequence11
Screen14:
Listofsequence12
Screen15:
Runningsequence12
Screen16:
Modificationofmethods13
Screen17:
Superpositionofprofiles13
Screen18:
Tab"Standard"15
Screen19:
Manualcreationofthestandards15
Screen20:
Standardcreation.16
Screen21:
Tab«Standard».16
Screen22:
Re-slope17
Screen23:
Listofthestandardofthemethod.17
Screen24:
Tab"Calibration"18
Screen25:
Tab"Calibration"inmodification18
Screen26:
Selectionofcalculationfunction19
Screen27:
Choiceofweightedcoefficient19
Screen28:
Tab"Point"20
Screen29:
Selecttheanalysisreport.20
Screen30:
Report"Lines-fast"21
Screen31:
Analysisreport"Table(Conc/unit/RSD)”21
Screen32:
Choiceofexportformat22
Screen33:
Export:
choiceofthedestination.22
1Introduction
Thisdocumentdescribesaproceduretocreateamethodandanalyzesamples.Thisprocedureisintentionallyshort.Formoreexplanation,pleasereferstotheusermanualreference31088469.
Wetaketheexampleoftheanalysisofamineralwater,whichhaselementsandtheirtypicalconcentrationsareindicatedbelow.
Element
Typicalconcentration(mg/l)
Element
Typicalconcentration(mg/l)
Element
Typicalconcentration(mg/l)
Na
20
Fe
<1
As
<0,100
K
10
Cu
<1
Se
<0,100
Ca
100
Zn
<1
Pb
<0,100
Mg
50
Sr
<1
Cd
<0,100
P
10
Cr
<1
S
10
Ni
<1
Tosimplifytheexplanations,wewilltakeonlytheelementsCa,FeandPb.
2Enteringthesoftware
ToenterthesoftwareofICPspectrometermanagement,doubleclickontheicon"Pv5.exe"or« ICPJYV5.0 ».
3Lightingtheplasma
Thescreenforplasmalightingappearsiftheplasmaisautomaticallycontrolled.Thedefaultparameterscorrespondstoanusualanalysisinaqueousmedium.
Screen1:
Plasmacontrol
Fortheothermedium,modifytheparameterswiththetypicalvaluesgiveninthefollowingtable
Medium
Generatorpower
Peristalticpumpspeed
Plasmagasflowrate
Auxiliarygasflowrate
Sheathgasflowrate
Aqueousverylowsaltcontent
900W
20
PL1=12
0
0.2
Aqueous
1000W
20
PL1=12
0
0.2
Aqueouslowsaltcontent
1100W
20
PL1=12
0
0.3
Organic
1200W
10
PL2=14*
1.2
0.3
Veryvolatilesolvent
1400W
5
PL2=16*
1.2
0.3
*tobeadjusted
Clickon«Start»tostarttheplasma.Whentheplasmaisalight,clickon“-“toreducetheapplication.Neverclosetheapplication,otherwisetheplasmawillshutdown.
Thescreen“Useridentification”appears.
Enter3,3(valuesbydefault,canbemodifiedinparagraph17oftheusermanual)thenclickon
Screen2:
Useridentification
Themeanscreenappears.Itrepresentsallthefunctionsoftheversion.
Screen3:
Softwarepresentation
4Methodcreation
Tocreateamethodclickon
Thelastmodifiedmethodappears(dependsontheuser).
Tocreateanewmethod,clickon“New”.
Enterthemethodname:
“TRAINING”
Screen4:
Newmethod
Clickon“Next”.
Createthemethod“Fromtheelements”forapersonalizedchoice.Onecanalsocreateamethod“fromanexistingmethod”andthenmodifythemethodor“fromamatrix”wheretheappropriatewavelengtharegiven,withnointerference,dependingonthematrix.Choosetheunitofmeasureandclickon“Next”.
Screen5:
Choiceoftheelements
Selecttheelementsbyclickingontheirsymbols:
Ca,FeandPb.
Clickon“Next”.
Screen6:
Concentrationrange
Keeptheconcentrationrangeindicatedbydefault“0-10”.(ifthemeasuredvaluesaresuperiortothehighvaluetheywillbeinbracketsonprintingandinyellowonthescreen).
Whenthestandardsaredefinedyoucanputthehighvalueofthestandardforthemaxvalue.
Clickon“Next”.
Screen7:
Linescharacteristics
Theselectedwavelengthsaregenerallythemostsensitivelines.Ifyouwanttochange,seeparagraphoftheusermanual.Ifyoudon’tknowthewavelengthtouse,takeseveralwavelengths.Youwillthendoprofilestochoosethebestwavelengthoryouwillconsultatableofwavelength.
Inourexampletake:
Pb220.353nm
Fe259.940nm
Ca317.933nm
SuppresstheCa393.366nmlinebyclickingon“Delete”thenbymarkingthecorrespondinglineandbyclickingon«OK».
Clickon“Lineaddition”andmarkedinthelinedatabasethewantedwavelength.Ifitdoesn’texist,additfromthelinedatabase.(cf.paragraph14.3oftheusermanual).
Clickon“Next”.
Theparametersofthemethodappeared,keepthedefaultoneatthatpoint.
Screen8:
Methodparameters
Iftheinstrumentisautomaticallycontrolled,clickon“Conditions”,thecontrolparametersappears.Adjustthevaluesinfunctionofthesampletype(seeparagraph3).
Screen9:
Operatingconditions
Clickon«OK»toreturnonscreen8,thenclickon«Next».
Screen10:
Standards
Donotselectstandardsatthepresenttime.
Clickon« Finish ».
Screen11:
Concentrationrange
Clickon“Save”forsafeguardingthemethodcreated.
5Methodoptimization
Gointhesequencepartbyclickingon
Clickon“New”.
Clickonareatoselectthemethod« Training ».
Screen12:
Sequence
Makeapeaksearch,threeprofiles(forexample:
water,sample5ppm,unknownsample).
Selectthetask«peaksearch»,then«profile»threetimes.Enterthenameofeachtask(correspondingtothesamples).
N.B.:
itisimportanttogivedifferentnametotheprofiles,inordertodiffereciatethemwhenvisualizingtheminthemethod.(ifyougivethesamename,theoldprofilewillbecrushed.
Giveanametothesequenceafterhavingclickingon«Save»;Byexample” Methodnameprepa”(inourcase« Trainingpreparation »).Clickon«OK».
Screen13:
Sequence
Screen14:
Listofsequence
Startthesequencebyclickingon.Clicktwiceon«Close»whenthesolutionisreadyforanalyze.
Screen15:
Runningsequence
Variouscasescanappearduringapeaksearch:
1.Thesoftwarerecognizethepeak,abluedotedlinemarksthechosenposition.
2.Thesoftwaredoesn’trecognizeapeak.Doubleclickinorderthattheverticallinecorrespondstothemiddleofthepeakatmidheight.
3.Nopeakappearsinthesearchwindow,changetheparametersofthepeaksearchinthemethod(cf.Paragraphoftheusermanual).
4.Severalpeaksappears.Re-dothepeaksearchwithamono-elementarysolution.Takecare,thesoftwarecanchoosethewrongpeak.
5.Ifthepeakfoundistoosmalltobeselectedautomaticallybythesoftware.Zoombymarkingarectanglewiththemouse.Anddoubleclickontherightposition.Togobacktotheinitialscaleclickonthemagnifier.
Oncethesequenceisended,clickon«Close»(screen15)thenclickagainon“Close”(screen13).
Returntomethodtovisualizetheprofiles:
clickonthe“Line”tab,selectthelines(withthehelpofthemouse,underlinethelinesinblue),clickon«Modify»onthebottomofthescreen(selectpreviouslythefunction«Modify»ontherightofthescreen).
Screen16:
Modificationofmethods
Thenclickon«Background»andselecttheprofilestosuperpose.
Screen17:
Superpositionofprofiles
Evaluateroughlytheconcentrationsofthesamplestoanalyze.Determinethentheslitstheanalysismode,theintegrationtimeconsideringthefollowingtables.
ForaJYULTIMA,JY238,JY38.
Concentration
Analysismode
Integrationtime(s)
Incrementbetweentwomeasuredpoints(nm)
Slits
>20mg/l
Max(1/1)
2
0,002for<310nm
0,003for>310nm
0,004forNa,Li,K
20/80
Mean(3/3)
0,5
0,002for<310nm
0,003for>310nm
0,004forNa,Li,K
20/80
Gauss(9/5)
0,3
0,002for<310nm
0,003for>310nm
0,004forNa,Li,K
20/15
0,5 Gauss(9/5) 0,5 0,002for<310nm 0,003for>310nm 0,004forNa,Li,K 20/15 0,1 Max(5/1) 0,5 0,002for<310nm 0,003for>310nm 0,004forNa,Li,K 20/15 <0,1 Max(5/1) 1 0,002for<310nm 0,003for>310nm 0,004forNa,Li,K 20/15 LQ Mean(3/3) 2 0,001for<310nm 0,002for>310nm 0,003forNa,Li,K 20/15 ForaJY2000,JY24,JY124. Concentration Analysismode Integrationtime(s) Incrementbetweentwomeasuredpoints(nm) Slits >20mg/l Max(1/1) 2 0,003for<310nm 0,004for>310nm 0,005forNa,Li,K 20/80 Mean(3/3) 0,5 0,003for<310nm 0,004for>310nm 0,005forNa,Li,K 20/80 Gauss(9/5) 0,3 0,003for<310nm 0,004for>310nm 0,005forNa,Li,K 20/15 0,5 Gauss(9/5) 0,5 0,003for<310nm 0,004for>310nm 0,005forNa,Li,K 20/15 0,1 Max(5/1) 0,5 0,003for<310nm 0,004for>310nm 0,005forNa,Li,K 20/15 <0,1 Max(5/1) 1 0,003for<310nm 0,004for>310nm 0,005forNa,Li,K 20/15 LQ Mean(3/3) 2 0,002for<310nm 0,003for>310nm 0,004forNa,Li,K 20/15 With Conc: concentrationoftheelement LQ: limitofquantification Max: Modemaximum Mean: Modemean Gauss: Modegaussien Takecare,beforeusingtheslits20/80,verifyonpro
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