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Version3.2
TABLEOFCONTENTS
Page#
Section1.0
ABCsofPracticalWorkwithIonChromatographs
Section2.0
InstrumentFlowPaths
2.1
GeneralizedICFlowPath
2.2
DosinoRegenerationofMSM
10
2.3
PeristalticRegenerationofMSM
11
Section3.0
SolutionPreparation
13
3.1
Eluentpreparation
13
3.2
Suppressorsolutions
14
3.3
Calibrationstandards
14
Section4.0
Operation
17
4.1
PurgingtheICpump
17
4.2
Systemstartup
19
4.3
Preparingamethodforcalibration
21
4.4
Startingasinglesampledetermination
23
4.5
Creatingandrunningadeterminationseries
25
4.5.1
29
4.6
Calibration
4.6.1
Calibration:Processstandards
Invialdilutionsystemuserguide(MiVDT3.02._DualDosinoUF)
33
33
4.6.2
Calibrations:Integrationofpeaks
34
4.6.3
Calibration:Updatecomponentretentiontimes
37
4.6.4
Calibration:Updatestandardconcentrations
38
4.6.5
Calibration:Reprocessingintwostages
40
4.6.6
Calibration:Applythecalibrationfromastandardtosampledeterminations
4.7
Databases
4.7.1
Databases:Quickfilter
45
47
4.7.2
Databases:Specialfilter
47
4.7.3
Databases:Batches
49
43
Page#
4.8
Reports
4.8.1
51
Reports:Printingondemand
51
4.8.2
Reports:Automaticprinting
52
Reports:Customizingreporttemplates
53
4.8.3
4.9
EmailingchromatogramsfromMagICNet
59
4.10
Creatingandusingcontrolcharts
63
4.11
Creatingandusingdataexporttemplates
67
4.12
ExportingandImportingMethodsinMagICNet
73
4.13
Addinguserdefinedresultstothedatabaseview
77
RoutineMaintenanceGuide
81
Section5.0
SECTION1.0
ABCsofPracticalWorkwithIonChromatographs
(fromMetrohm2011ICColumnCatalog)
Bacterialgrowth
Bacterialgrowthhasasignificantnegativeeffectonchromatographyanddestroystheanalyticalcolumns.Alarge
numberofchromatographicproblemscanbetracedbacktothegrowthofalgae,bacteria,andmolds.Inorderto
prevent bacterial growth, eluents, rinsing, and regeneration solutions should always be prepared fresh and not
reusedafterprolongedperiods.WerecommendthatallvesselsbethoroughlyrinsedwithultrapureandUVtreated
waterandthenrinsedwithmethanol/wateroracetone/waterandfinallyagainwithwaterbeforebeingrefilled.If
bacteriaoralgaeshouldformdespitethistreatment,then5%methanoloracetonecanbeaddedtotheeluent.This
isnotpossiblewhenusingmembranesuppressors,becausethesecouldbedestroyedbyorganicsolvents.The"MSM
II","MSMHC",and"MSMLC"MetrohmSuppressorModulesare100%solventresistant.Methanolshouldnotbe
usedwithsomecationcolumns.
Cationanalyses
Forallanalyseswerecommendthatthesamplesbeacidifiedwithnitricacid(approximately100L2mol/LHNO3
per100mLofsample)(pH2.53.5),becauseotherwisenoreproducibleresultswillbeobtainedforthedivalent
cations.
CO2
Becausethecarbonate/hydrogencarbonateequilibriumintheeluentisinfluencedbycarbondioxideintheair(the
eluentbecomesweakerovertime)theeluentbottleshouldalwaysbefurnishedwithaCO2adsorbermaterial("soda
lime").EluentswithaweakbuffercapacitymustalsobeprotectedagainstCO2.
Degassingtheeluent
Inordertopreventbubbleformation,werecommendedthattheeluentsproducedbedegassedpriortobeingused
intheICsystem.Thisisdonebyapplyingavacuumcreatedbyawaterjetpumporvacuumpumpforapproximately
10minutesorbymeansofanultrasonicbath.Alternatively,workcanbecarriedoutwithanEluentDegasser.
Eluentbottles
Eluentsarepositionedinspecialeluentbottles,usuallydirectlyontheICsystem.Topreventmoistureandcarbon
dioxide from being absorbed by the eluent, the bottles are equipped with a drying tube which normally has a
molecularsieveandisfilledwithsodalime(asaweakCO2adsorbermaterial)forsodiumhydroxideandcarbonate
eluents.
Environmentalprotection
Agreatadvantageofionchromatographyisthatmostworkiscarriedoutwithaqueousmedia.Thechemicalsused
inionchromatographyarethereforeasnontoxicaspossibleanddonotpollutetheenvironment.Nevertheless,
whenworkiscarriedoutwithacids,bases,organicsolvents,orheavymetalstandards,theymustbedisposedof
properlyafteruse.
Filter
If problems occur with IC systems, they are usually due to particles introduced by bacterial growth, unfiltered
eluents,bythesampleorbyrinsingandregenerationsolutions.Thisriskcanbereducedtoanabsoluteminimum
byusinganaspirationfilter(6.2821.090),inlinefilter(6.2821.120),andguardcolumns(startingonpage167).The
filtersarepartofthebasicequipmentoftheMetrohmionchromatographsandareincludedinthescopeofdelivery.
Westronglyrecommendtheiruse.Careshouldbetakentoensurethatthefiltersarereplacedregularly.
Filtrationoftheeluent
Alleluentsshouldbemicrofiltered(0.45m)immediatelybeforebeingused.
Fun
Ionchromatographyshouldbefunandnotgetonyournerves.Metrohmdoeseverythingitcantoensurethatyour
ICsystemsworkreliablywithaminimumofupkeep,maintenance,andcost.Metrosepseparationcolumnsstandfor
quality,longlifetime,andoutstandingresults.
Guardcolumns(precolumns)
Guardcolumns(startingonpage167)areusedtoprotectthevaluableseparationcolumns.Westronglyrecommend
theiruse.Asaruletheycontainthesamestationaryphaseastheseparationcolumn,althoughinaconsiderably
smallerquantitytoavoidinfluencingthechromatography.Guardcolumnseliminatecriticalcontaminationswhich
mightreactwiththecolumnmaterialandtheyeffectivelyeliminateparticlesandbacterialcontamination.Theguard
columnmustbechangedthanwhenthebackpressureinthesystemrisesorwhenthechromatographyworsens.
GuardcolumnsareavailableforallMetrosepseparationcolumns.
Longtermstorageoftheionchromatograph
Iftheionchromatographwillnotbeusedforaprolongedperiod(>1week),thentheseparationcolumnshouldbe
removedandsealedwiththestoppersprovided.Theionchromatographshouldberinsedwithmethanol/water
(1:4).Careshouldbetakentoensurethatallthreechambersofthesuppressorarerinsedduringthisprocess.The
separationcolumnshouldbestoredinthemediumlistedonthecolumndatasheet,optimallybetween4and8C.
Whentheinstrumentisrestarted,rinsethesystemwithfresheluentbeforeinstallingtheseparationcolumnand
bringituptoroomtemperature.
Particles
Allsolutions,samples,regenerationsolutions,thewaterandtheeluentsshouldbefreeofparticlesbecausethey
may clog the separation columns over time (increase in column pressure). This must be taken into account
particularlywheneluentsarebeingproduced,becauseeluentsflowcontinuouslythroughthecolumn(500to1000
mLperworkingdayincontrasttoapproximately0.5mLofsamplesolution).Thesamplecanbefilteredordialyzed
fullyautomaticallywiththe"MISP"MetrohmInlineSamplePreparationsystems.
Pulsationabsorber
Werecommendtheuseofapulsationabsorber(6.2620.150),whichisalreadyinstalledinICinstrumentsfrom
Metrohm.Inparticular,polymethacrylateandpolyvinylalcoholcolumnsshouldbeprotectedagainstbriefpressure
surgeswhichinevitablyoccurwhenthevalvesareswitched.Thisprotectionisensuredwhenapulsationabsorber
isused.
Qualityofchemicals
All chemicals should be at least of p.a. or puriss. quality. The standards must be specially suited to ion
chromatography.Alinktothewebsiteofamanufacturerwithasummaryofthechemicalsmostfrequentlyused
andrecommendedforionchromatographycanbefoundontheInternetatwww.metrohm.com.
Regenerationofseparationcolumns
Asarule,ifseparationcolumnsareoperatedwithcleaneluentsandchargedwithparticlefreesamples,thenavery
longlifetimeisguaranteed.Aregenerationofthecolumnisthennotnecessaryandisalsonolongerpossibleafter
alargenumberofinjections.Nevertheless,ifthepressureinthecolumnshouldriseunexpectedlyortheseparating
efficiencydecrease,thentheregenerationstepswhichareindicatedforeachseparationcolumncanbecarriedout.
In general, it must be noted that the regeneration takes place outside the analytical line. This means that the
separation column is connected directly to the pump and the regeneration solution feeds through the column
directlyintothewastevessel.Beforetheseparationcolumnisreinstalled,itshouldberinsedsufficientlyfor30
minutesatstandardflowwithfresheluent.
Samplepreparationcartridges
Samplepreparationcartridgesareusedforthepreparationofcriticalsampleswhichcannotbeplaceddirectlyon
the separation columns. Thus, for example, samplepreparation cartridges remove organic contamination or
neutralizestronglyalkalineoracidicsamples.Samplepreparationcartridgesareconsumablematerialswhich,asa
rule,cannotberegenerated.Theydonotreplacetheguardcolumn(precolumn),whichshouldalwaysbeusedwith
eachseparationcolumn."MISP"(MetrohmInlineSamplePreparation)offersanalternativetosamplecartridges,
e.g.forthefullyautomatedneutralizationofalkalinesamples.
Waterquality
Ionchromatographyprimarilyinvolvesworkinaqueousmedia.Waterqualityisthereforeofdecisiveimportancefor
obtaining good chromatographic results. If the water quality is unsatisfactory, then the results will certainly be
unsatisfactoryaswell.Inaddition,thereistheriskofdamaginginstrumentsandseparationcolumns.Theultrapure
water used should have a specific resistance greater than 18 M cm and be particlefree. It is therefore
recommendedthatthewaterbefilteredthrougha0.45mfilterandtreatedwithUV.Modernultrapurewater
plantsforlaboratoryuseguaranteethesestandards.
SECTION2.0
INSTRUMENTFLOWPATHS
GENERALIZEDICFLOWPATH
FIGURE2.1
Component Function
Eluentbottle
Liquidphasethatcarries
samplethroughthesystem;
participatesinseparationof
ions
Eluent
Degasser
Removesmacrobubbles
fromeluent;helpsprevent
vaporlockintheICpump
ICPump
Pusheseluentthrough
systemathighpressure
InlineFilter
0.45m;filtersparticulates
fromeluent;regular
maintenanceitem
Pulsation
Absorber
Protectscolumnfrom
pressureshocksasvalve
switched
Injection
Valve
Fillposition:loadssample;
InjectPosition:sendsitto
column
Sampleinlet
DeliverssampletoInjection
valve
15
14
13
12
7
9
1
6
3
11
10
8
2
5
Sampleloop
Measuredvolume(20L)standard
Samplewasteline
(inmostsystemssampleinletandwastelinescanbeswitched)
10 Guardcolumn
Protectscolumnfromparticulates/contaminantsregularmaintenanceitem
11 Separationcolumn
Solidphaseseparatessampleionsintodistinctbands
12
SequentialSuppression
System
Commoninanionsystems;notusedincationorothernonsuppressedanalysis
13 MSMSuppressor
Reducesbackgroundconductivity,increasingsensitivitybyconvertingreplacingsodium
ionsineluentwithH+
14 MCSCO2Suppressor
Furtherreducesbackgroundconductivityandincreasessensitivitybyremovingcarbonate
asCO2
15 Conductivitydetector
Measuresdifferencesinbacgroundconductivityofeluentvs.analyteionsastheypass
through(UV,ELCDandotherdetectorsmaybeusedinplaceoforinconjunctionwiththe
conductivitydetector)
FIGURE2.2:DOSINOREGENERATIONOFMSM
11
12
8
9
5
3
10
13
1
17
16
15
14
Component
Part#
Function
FEPAspirationtube,M6,
0.25m
6.1829.010
DrawsRegenerationsolutionintoDosingUnit
DosingUnit,2mL
6.3032.120
Burettethataspiratesanddispensestheregenerationsolution
Dosino
1.800.0010
Motorthatdrivestheburette
M6Thread/UNF10/32
Coupling
6.2744.080
AdaptsM6threadofDosinoto10/32compressionfitting
PTFEtubing,0.5mmID
6.1803.030
ConnectiontubingfromDosingUnittofilter
Inlinefilter
6.2821.120
FiltersRegen.Solutionto0.45m
RegenerantlineofMSM
(6.2832.010)
MSMUnit(Metrohm
SuppressionModule)
Reducesbackgroundconductivity,increasingsensitivitybyconverting
replacingsodiumionsineluentwithH+
InlineofMSM
(6.2832.010)
FromcolumnoutlettoPosition1ofMSM(SuppressionPosition)
(6.2832.010)
FromMSMPosition1outtoMCS
Furtherreducesbackgroundconductivitybyremovingcarbonateas
CO2fromtheeluent
12 Detectorinletline
13 Detectoroutletline
DetectoroutletservesasrinselineforMSMonPosition2(Rinse
position)
14 Coupling
6.2744.070
15 RinsingsolutionlineofMSM
(6.2832.010)
16 WastelineofRinsesolution
(6.2832.010)
NormallyconnectedtoWasteCollectorcup
WastelineofRegeneration
solution
(6.2832.010)
NormallyconnectedtoWasteCollectorcup
10 OutlineofMSM
11
17
MCS(MetrohmCarbonate
Suppressor)
10
FIGURE2.3:PERISTALTICREGENERATIONOFMSM
10
2
11
8
4
1
9
3
2
12
13
Component
Function
PTFEtubing,0.97mmID
6.1803.020
TubingfromMSMRinseandRegenerantbottlestopump
Pressurescrew,short
6.2744.070
CouplingnozzleUNF10/32
6.2744.034
Threadsintotheperistaltictubingandallowsconnectionofsupplyline
viaacompressionfitting
Pumptubingconnectorwith
securitylockandfilter
6.2744.180
Connecttooutletofperistaltictubing.Filterssolutionto0.45m.
RegenerantlineofMSM
(6.2832.010)
MSMUnit(Metrohm
SuppressionModule)
6.2821.120
Reducesbackgroundconductivity,increasingsensitivitybyconverting
replacingsodiumionsineluentwithH+
RinsingsolutionlineofMSM
(6.2832.010)
InlineofMSM
(6.2832.010)
FromcolumnoutlettoPosition1ofMSM(SuppressionPosition)
OutlineofMSM
(6.2832.010)
FromMSMPosition1outtoMCS
10
MCS(MetrohmCarbonate
Suppressor)
Furtherreducesbackgroundconductivitybyremovingcarbonateas
CO2fromtheeluent
WastelineofRegeneration
solution
NormallyconnectedtoWasteCollectorcup
13 WastelineofRinsesolution
NormallyconnectedtoWasteCollectorcup
11 Detectorinletline
12
Part#
11
12
SECTION3.0
3.1
ICSOLUTIONPREPARATION
Eluentpreparation
MakingEluentfromSalts
1) Calculatethevolumeofdesiredeluentmodifiersbytheir%compositionintheeluent(ifneeded).
Ex.Eluentwith15%acetone
#mlacetone
=volumeofeluentx%modifier
=2000mLx15%=300mLacetone
Willhave300mLofacetonein1700mlH2O(2000mL300ml).
2) Measureoutdesirequantityofultrapurewater(1or2L)intriplerinsedvolumetricflask.Pourthisinto
thetriplerinsedeluentbottle.Degasthewaterfor1030minuteswhilesonicatingorstirringwitha
magneticstirrer(degassingtimesmayvaryaccordingtotheamountofdissolvedgassesinlocalwater).
Thisremovesmicrogasbubblesinthewater.Filterwaterthrough0.45micronfilter(manywatersystems
havethisinline).
3) Calculatetheamountofsaltneededtomaketheeluent:
(Moles/L)
(g/mol)
(L)
Ex.#gNa2CO3for2Lof3.2mM=0.0032mol/Lx106g/molx2Lx1/0.99=0.678gNa2CO3
4) Zeroaweighingboatontheanalyticalbalance.Addthedesiredmassofsalt.Recordtheactualmass.
5) Pourthesaltintotheeluentbottlecontainingthedegassedultrapurewater(orwashitintothebottle
withaportionoftheUltrapurewateryoudegassed).
6) Thoroughlymixthesolutionbystirringwithmagneticstirringorsonicationuntilsaltsarefullydissolved.
MakingEluentfromaConcentrate
1) Proceedwithstep1asshownabove,thenusetheformula
belowtocalculatetheamountofconcentrateneeded:
V1=C2xV2=(FinalEluentConcentration)x(FinalEluentVolume(ml))=
C1
(ConcentratedEluentConcentration)
VolumeofConcentrate
Needed(ml)
2) Addthisamountofconcentratetoavolumetricflaskofappropriatesize,thendilutewithultrapurewater
tothedesiredvolume.Carefullypourtheeluentintotheeluentbottle.Stirorsonicatewhiledegassing
theeluentfor520minutes(degassingtimesmayvarywitheluentcomposition).
13
3.2
Suppressorsolutions(forsuppressedanionsystems)
DIWaterRinse:Rinse1LbottlewithAcetone,thentriplerinsewithultrapurewater.Fillbottletoapproximately1
LwithultrapureDIwater.
100mMH2SO4RegenerantforPeristalticRegeneration/500mMH2SO4RegenerantforDosinoRegeneration::
Rinse1LbottlewithAcetone,thentriplerinsewithultrapurewater.Fillbottletoabout700mLlinewithultrapure
DIwater.Add5.6mLconcentratedH2SO4tothebottle.Takethelevelofthesolutiontoapproximately1Lwith
ultrapureDIwater.ForDosinoRegenerationofMSMuse28mLofconcentratedH2SO4 toafinalvolumeof1L
(500mMfinalconcentration).
3.3 Calibrationstandards(Gravimetricstandardpreparation)
MakeaCombinedStockStandard
1. ForamultipointcalibrationitiseasiesttofirstmakeaCombinedStockStandardfrom1000ppmindividual
ionconcentrates.Thisstockcanbeusedbothasthehighestcalibrationlevel,andbedilutedtomakethe
otherstandardlevels.Makeenoughofthiscombinedstockstandardtouseforthedilutionsandtorunon
theIC(usuallytwiceormoretheamountoftheotherstandards).CalculatetheamountofIndividualIon
ConcentrateneededforeachcomponentionintheCombinedStockStandard:
M1=C2xM2=(FinalStandardConcentration)x(FinalStandardMass*)=InitialMass*
C1
(IndividualConcentrateConcentration)
ofIndividualIonConcentrateNeeded(g)
Pipette
Example: M1=C2xMz=(10ppmSO42)x(100g)=1gof
1000ppmSO42ConcentrateNeeded
C1 (1000ppmSO42)
for100mLof
20ppmstandard
1.010
Balance
1. Placeclean(preferablynew)plasticbottleofappropriatesize
onthebalance.Zerobalance.
14
3.
BackcalculatetheactualconcentrationsofallionsintheCombinedStockStandardusingthisformula(or
usinganExcelSpreadsheet):
C2=C1xM1=(Indv.ConcentrateConcentration)x(StockStandardAdded)=
ActualIon
M2
(FinalStandardMass)
ConcentrationinStock
MakeOtherStandardLevelsbySerialDilutions
4. CalculatetheamountofCombinedStockStandardneededto
Pipette
maketheotherdilutedstandardlevels:
M1=C2xM2=(FinalStandardConcentration)x(FinalStandardMass)=InitialMassof
C1
(StockStandardConcentration)StockNeeded(g)
SampleBottle
15.00
Balance
7.
Ex.M1=C2xM2=(5ppm)x(30g)=
15gCombinedStockStandard
C1
(10ppm)
Neededfor5ppmdiluted
standard(Level4)
7.5gCombinedStockStandard
M1=C2xM2=(2.5ppm)x(30g)=
C1(10ppm)
Neededfor5ppmDil.Std.(Level3)
3.0gCombinedStockStandard
M1=C2xM2=(1.0ppm)x(30g)=
C1(10ppm)
Neededfor2.5ppmDil.Std.(Level2)
1.5gCombinedStockStandard
M1=C2xM2=(0.5ppm)x(30g)=
C1(10ppm)
Neededfor1ppmDil.Std.(Level1)
30.020
6. AddcalculatedInitialMassofStockNeededforthisstandardlevelto
the bottle. Record the actual mass added to the limit of decimal places
displayedbythebalance.Thisvolumeofstockcontainsallcomponentions
desiredintheappropriateratios.
NowaddenoughUltrapure,ICgradewater(18Mpreferred)todilutethestandarduptotheappropriate
FinalStandardMass,andrecordthismass.Labelbottlewithstandardlevel.Repeatthisprocedureforall
standardlevels.
Ex.
Standard
Level
4
3
2
1
Amt.Stock
Added(g)
15.005
7.510
3.015
1.511
FinalStd.
Mass(g)
30.020
30.040
30.056
30.005
15
8.
Backcalculatetheactualconcentrationofeachcomponentioninthestockanddilutedstandardsusingthe
following formula (or with the Standard Concentrations Calculator Excel Spreadsheet, which is much
faster):
C2=C1xM1=(StockStandardConcentration)x(StockStandardAdded)=
M2
(FinalStandardMass)
ActualIonConcentrationinStandard
Ex.
IndividualIonConcentrationsofCombinedStockStandard
Standardor
sample
Ion
Stock
Chloride
Sulfate
Concentrationof
Indiv.Ion
Concentrate(C1)
(1000ppm
(1000ppm
Mass
added(M1)
X
X
1.025)
1.010)
/
/
Totalmass
ofstandard
(M2)
100.050
100.050
IonConcentration(C2)
=
=
10.199ppm
10.095ppm
IonConcentration(C2)
=
=
=
=
=
=
=
=
5.098ppm
5.046ppm
2.550ppm
2.524ppm
1.023ppm
1.013ppm
0.514ppm
0.508ppm
IndividualIonConcentrationofDilutedStandard(s)
Standardor
sample
Ion
L4
L3
L2
L1
Chloride
Sulfate
Chloride
Sulfate
Chloride
Sulfate
Chloride
Sulfate
Concentrationof
CombinedStock
Std.(C1)
(10.199ppm
(10.095ppm
(10.199ppm
(10.095ppm
(10.199ppm
(10.095ppm
(10.199ppm
(10.095ppm
Mass
added(M1)
X
X
X
X
X
X
X
X
15.005g)
15.005g)
7.510g)
7.510g)
3.015g)
3.015g)
1.511g)
1.511g)
/
/
/
/
/
/
/
/
Totalmass
ofstandard
(M2)
30.020g
30.020g
30.040g
30.040g
30.056g
30.056g
30.005g
30.005g
9.
EntertheconcentrationvaluescalculatedforeachstandardlevelintothemethodasdescribedinSection
3.2PreparingaMethodforCalibration.
10. RunthestandardsontheIC.
16
SECTION4.0
4.1
OPERATION
PURGINGTHEICPUMP
TheICpumpshouldbepurgedwhenneweluentisputonthesystem,whenairisobservedinthelines
andpressureislow,orwhenmaintenancehasbeendoneontheICpump.
1.
OpenthedoortotheIC,thenturnthepurgevalveknobturn
counterclockwisetoopenit.
Purgevalve
2.
Ifthesoftwareisnotalreadyopen,openitbydoubleleftclickingontheMagIC
Neticon.
3.
ClickontheManualiconatthebottomleftoftheMagICNetscreen.AManual
controlwindowwillopen,displayingthecomponentsoftheIC.
4.
UnderDevice
SelectionchooseAll
Devices,
5.
ClickontheICinthe
deviceslist.
6.
SelectthePumptab
(orclickontheicon
fortheICpump).
7.
Makesurethepump
isshutdown(the
Stopbuttonis
grayedout).
8.
ChangetheFlow
Inputto2mL/min.
andthePMinto0.0
MPa.
9.
ClicktheApply
button.
4.
5.
6.
8.
7.
9.
17
10. ConnectasyringewithaLuerconnectiontothepurge
lineoftheICpump.
Purgeline
11. Pullonthesyringewiththepurgevalveopenandthe
pumpoffuntilyouseeafewdropsofliquidbeginning
toenterthesyringe.Thispurgesairoutoftheeluent
lineandbeginsagravityfedeluentflow.
12. TurnontheICpumpbyclickingtheStartbuttoninthe
Manualcontrolwindow.
13. WiththeICpumpnowrunning,pullthesyringe
plungerbacktodraweluentintothesyringe.Holdthe
pressureontheplungeruntilyoucanseethatliquidis
beingsteadilydeliveredintothesyringe.
14. Releasethepressureonthesyringeplungerandallow
ittoequalize.Turnthesyringeupsidedown(plunger
facingupwards,needletipfacingdownwards).The
liquidfillingthesyringeshouldbepushingtheplunger
outwardsatanobservablerate.
15. Tapthefrontofthepumpheadlightlyoneithersideof
divisionlinewhilethepumpisrunning.Observe
whetherornotairbubblesarepassingintothesyringe.
Iftheydo,continuelightlytappingthefrontofthe
pumpheadandtheeluentlineuntilairbubblesareno
longerpassingintothesyringe.
16. Oncefluidisobservedflowingfreelyintothesyringe
andnoairbubblesareobserved,clickStoponthe
manualcontrolwindow.
17. Turnthepurgevalveknobclockwiseuntilitissnug
(fingertightonly).
18. CloseoutoftheManualcontrolwindowandproceed
toequilibratetheinstrument(seethenextsectionof
thisdocumentforinstructions).
18
4.2 SYSTEMSTARTUP
1. Ifthesoftwareisnotalreadyopen,openitbydoubleleftclickingontheMagICNet
icon.
Themainprogramwindow
willopenandwilldisplaya
messageindicatingthatthe
programanddevicesare
beinginitialized.Ifan
autosamplerisconnectedto
thesystemitwillmake
severalaudiblebeepsand
theneedleandrackwillgo
throughaninitialization
process.Ifanydevices
designatedinthemethod
arenotdetected,awarning
messagetothiseffectwillbe
displayed.Priortostarting
thehardware,clickonthe
Configurationbutton.
ThiswilltakeyoutotheConfigurationwindow.IntheDevicessubwindowlookattheStatusofall
devices.Wheninitializing,ICsandautosamplerswillhaveanorangeflagandStatusofNotok.Wait
untilthedeviceStatusislistedasOKandisflaggedgreenbeforeStartingthehardware.
19
INSTRUMENTSTARTUP
1. ClicktheWorkplacebutton
2. Select the Method in the Run window by clicking the selector button
appropriatemethodoutofthelistgiven(Ex.Chloride_SulfateAnalysis).
3. Press the
button to start the instrument hardware and allow it to warmup. The
instrumentneedstowarmupforabout40minutesbeforeanalysesarerun.
4.
SuppressedAnionAnalysis:AfterthistimethebaselineConductivityreadingintheWatchwindowshould
bebetween0.83S/cm(dependingoneluentcomposition)andthebaselineshouldbeflatatascalingof
about0.2S/cmbetweeneachdividinglineontheyaxisofthegraph.
A dip in the baseline will be observed approx. every 10
minutes as the MSM suppressor steps (rotates). The
baseline after each MSM step should be about the same
conductivity.Once3goodMSMstepshavebeenobserved
thesampletablecanbestarted.
Other Analyses: Look for a stable, relatively noisefree
baseline, then begin the sample table (generally 30 min.
equilibration;foraUVdetectorallow1hr.equilibrationfor
baselinetocompletelystabilize).
20
4.3
PREPARINGAMETHODFORCALIBRATION
1.
ClicktheMethodbuttontoentertheMethodviewofMagICNet.
2.
Clickonthe
icontoopenamethod(ifoneisnotalreadyopeninthisview).
3. IntheMethoddirectoryselectthesystemfileyounormally
useforanalysis(unlessyouconductextensiveapplication
development,therewilllikelyonlybeoneorafewmethodsin
thisfolder).Thenclick.
UpdateStandardConcentrations
4. IntheEvaluationsectionoftheMethod,clickontheStandardsbutton.
5. Checktomakesurethatallstandardconcentrationslistedmatchthecurrentcalibrationlevels
youarerunning.Ifnotyouwillneedtoupdatetheconcentrationsforeachlevel.
6. Updatetheconcentrationsfora
levelbyrightclickingonthatlevel
andselectingEdit.
7. Entertheappropriate
concentrationsintheEditStandard
window.ClickOKwhenfinished.
8.
UpdatetheconcentrationsfortheCheckstandards
21
9.
UpdatetheconcentrationoftheSpikingsolution(ifused).Enter
thevolumeofSampleandSpikingsolutioninthematrixspike.
ThesevalueswillbeusedtocalculatetheSpikerecovery.
10. TosavethechangestothemethodselectFileSave.
22
4.4
STARTINGASINGLESAMPLEDETERMINATION
Note:IntelligentDilutionsystemsshouldnotberunwithSingledeterminationmode.
Ifdesiringasinglerun,makeaDeterminationSerieswithjustoneline.
1.
ClickontheWorkplaceicontotheleftoftheMagICNetscreen.
2.
3.
3.
4.
8.
5.
6.
7.
4.
SelecttheSingledeterminationtabinthe
Runwindow.
EntersampleidentificationintheIdent
blank.
SelecttheSampletypefromthepulldown
menu(Ex.Blank)
5.
Position:Theautosamplerrackpostion
thesampleisin;whennotusingan
autosamplerentera1inthisfield.
6.
Volume:Thesampleloopsize(Ex.20uL)
7.
Dilutionfactor:Thedilutionfactorofthe
sample;forexample100wouldbeentered
fora1:100dilution.Entera1forno
dilution.
8.
Sampleamount:Entera1;for
automaticcalculationofthedilutionenter
theamountofsamplebeforedilutionin
thisfieldandthefinalmassafterdilution
intheDilutionfactorfield.Thesample
amountfieldcanalsobeusedtoenterthe
Densityofthesampletocorrectfor
differencescomparedtothewater
standards.
9.
ClickStart.
10. ThetimeProgramfortheinstrumentwill
nowbegin.
23
11. Afteryouhearthesoundofthevalveswitching,
insertthesamplelineintothesamplebottleand
pullbackonthesyringeplungertoaboutthe2mL
marker.
12. Holdthesyringeinthispositionuntilnearly2mL
hasbeenaspiratedintothesyringe.Slowlythe
releasetheplungerandallowthepressureinthe
syringetoequilibrateandthefluidtostopflowing.
13. ClicktheContinuebuttononthewindowthatpops
up.Ensurethatthesamplelineisnotremoved
fromthebottleuntilthevalvehasgoneto
injection,otherwiseairmaybeintroducedintothe
sampleloop,givinganincompleteinjection.
Thechromatogramwillnowrunfortheallottedtime.
24
4.5 CREATINGANDRUNNINGADETERMINATIONSERIES
NOTESABOUTSAMPLETABLES
SystemswithautosamplerscanbemosteffectivelyusedforanalysisbyrunningaDetermination
SeriesratherthanSingleDeterminations.
IntelligentDilutionmethodscanonlyruninDeterminationSeries,notSingleDeterminations,
becauseofthepredictivedilutionprogrammingtheyutilize.Torunjustoneanalysiswiththese
methods,makeaDeterminationSerieswithasingleline.
UserswithanInVialDilutionsystemshouldrefertoSection4.5.1beforepreparingaSampleTable.
1. NavigatetotheWorkplaceviewinMagICNet.IntheRunwindowclickonthe
Determinationseriestab.
LOADINGANEXISTINGSERIES
2
1
1.
Normallyitiseasiesttocreateasampletableisfroman
existingtable.TodososelectSampletableLoadand
selectthenameofasavedsampletabletoload.Thebenefit
tousinganexistingtableisthemethodwillbepreloaded,as
wellanyspecialfieldsaddedtothetablethatarenotdefault
fields.
2.
Tocreateanewsampletable,selectSampletableNew.
NotethatyoumayneedtoeditthePropertiesofthesample
tabletomakesurethatallofthefieldsneededforthemethod
torunarepresent.
3.
Withanexistingtable,resettheSampletablebyselecting
SampletableReset.ThiswillchangetheStatusofa
FINISHEDsamplelinetoREADY.
25
4. ToeditanexistinglineofdataintheSampleTableselectEditEditline.
Thefollowinginformationcanbechangedinthiswindow:
Method:Choosetheappropriatemethod.Usethe
andmethodoutofthoseavailable.
Ident:TheIdentificationofthesample(samplenameorID).
Sampletype:Sampleforanythingyouwishtobeevaluatedagainstthecalibrationcurve
(includingblanksyouwantquantified);Standard1forcalibrationstandards;Check
standard1forcheckstandards;Blankuseonlyforblanksubtractions(peakswillnotbe
integratedorquantified);Spiking1useformatrixspikes
Position:thepositionofthesamplevialontherack
Injections:1forasingleinjection,higherforreplicates.Checktoseehowmuchsample
volumeisusedforanalysisprogrammingmultipleinjectionsoutofonevial.Systemswith
ultrafiltrationcandoatmost2injectionspervial.
Volume:20isstandard;thisisthevolumeofthesampleloopusedtocalculatefinal
concentrations
Dilution:1ifnomanualdilutionwasperformed;otherwisethedenominatorofthemanual
dilutionfactor(e.g.100for1/100)
Sampleamount:1ifthereisnodensitycorrectionfactorneeded;otherwiseenterthe
densityifsampledensityisdifferentfromthestandards.
Info1:Anyspecialinformationornotesaboutthesample
butontochoosethemethodgroup
5. Use toadvancedtothenextlineandincrementinformation;useApplytoapplythecurrent
linesinfotothetable
26
DuplicateRows
1. Tomakemultiplecopiesofanexistingrowonasampletable,highlighttherow,thenselectEdit
Duplicate.Thisisusefulformakingmultiplecopiesofastandardlinetofillintheinformation
fortherestofthecalibrationstandards.
2. EntertheNumberofduplicaterowsyouwant
made,thenclickOK.
Increment
Insertnewline:Addsablanklinetothetable(nomethodspecified).
Cutlines:Cutsthecurrentlyhighlightedlinesoutofthesampletable(canbePasted
intoanotherlocation).
Pastelines:PasteslinesthathavebeenCutoutofthetableintothelocationcurrently
highlightedonthesampletable.
Deletelines:Deletesallcurrentlyhighlightedlines
Increment:Seeabove
Filling:Afterselecting,cursorbecomesanF;click,dragandreleaseoveraselectionto
makeallthesameasfirstcellhighlighted.
Duplicate:Seeabove
Marklines:Canmarklineswitharedflag;allowscertainactionstobedonewhenthese
linesarerun(e.g.Pausethequeueandshowamessage;stopthedetermination).
Unmarklines:Removetheabovementionedflag
Setlinesinexecutable:Crossesoutthelineitwillbeskipped;thisisusefultoeliminate
certainlinesfromfrequentlyruntableswithoutdeletingthem.
Setlinesexecutable:Removesstrikethroughandallowslinetoberun.
27
SavingtheSampleTable
6. Aftermakingchangestothesampletableitisbesttosaveit.ManyuserswillperformaSaveas
andgivethetableanamecorrespondingtothedatethetableisrun.
RunningaSampleTableTest
7.
PriortostartingaSampletableselectSampletableSampletabletest.
8.
Thiswilllookforanymissingorincompatibleinformationinthetable(like
missingdilutionfactorsorvialpositions)andwilldisplayitinamessage
box(asshownbelow)withthelineandspecificsofthemissingor
incompatibleinformation.
28
4.5.1 INVIALDILUTIONSYSTEMUSERGUIDE(MiVDT3.0.2_DualDosinoUF)
Overview:Aninvialdilutionsystemperformsdilutionsandautocalibrationrunsinemptyvialsthat
havebeenpreparedatspecificlocationsonthesamplerack.Empty,cappedvialsmustbereadyin
thesepositionsforthesystemtoperformproperly.
Setup
1. ClickontheConfigurationbuttonattheleftsideoftheMagICNetscreentoenterthe
Configurationview.IntheCommonVariablessectionupdatethefollowingcommon
variables:
(01)FirstEmptyVial_Anions:Normallyposition74
(02)LastEmptyVial_Anions:Normallypostion111.
Concentration(HighStd):Changeallofthecommonvariables
withadesignationsimilartothisonetothevalueofyour
highestcalibrationstandardforthation.Thesevalueswill
allowthesystemtodeterminewhenasampleisoutofthe
calibrationrangeandhowmuchitneedstobedilutedtofitthe
calibration.
29
SampleTableSetup
1. Dilution:Dilutionfactorformanuallydilutedsamples(dilutedpriortoplacingthemonthesystem)
2. SampleAmount:Ifthesystemisperforminganinitialdilutiontobringthesampleuptoavolumethatcan
befiltered(lessthan5mLofrawsamplepresent),thentheAmountfieldrepresentstheamount(inmL)of
sampleaddedtothevial.Ifmorethan5mLofsampleispresent,leavethisvalueat1.
3. Value1:ThisistheInstrumentDilutionFactortheamountofdilutionyouwishtheinstrumentto
perform.Ex:Fora1:100dilutionenter100intothisfield.Foradirectinjection(nodilution)entera1into
thisfield.(Maximumof100)
4.
Value2:Emptyvialpositionusedfordilutions.Fillvials74148withEmptyvialsfordilutionsandspikes.
EmptyVials74148arefortheAnionMethod.Enterthefirstvialpositiononline1ofthesampletable,
thenIncrementdownthelist.ThelastValue2inthetablecannotexceed11forAnionsand148for
Cations,asthesearealloftheavailableEmptyVialPositions.
5.
Info1:Usethepulldownmenutoselectthefollowingoptions(orselectnoneofthem):
6.
Noselection=noeffectonanalysis
(01)ResettoFirstEmpty
Vial_Anions:
ResetstheautovialpositiontotheCommonVariableEmpty
VialPosition_Anion_First.Usethisafterreloadingallofthe
emptysamplevials;alsorestartstheSampleCount.
(02)Restartsampleprep
Useifanerroroccursduringtheprevioussamplerun;willcause
thesampledilutiontobepreparedagaininanewvial.
(03)InitialRinse:
Rinseofsampleflowpathbeforeanyanalysisisconducted.Use
whencontaminationfromahighsampleissuspected.
Info2:UsethepulldownmenutoselectfromthefollowingoptionsonSampleanalyses
Note:Ifnoselectionismadethesamplewillbeevaluatedfori
DilutionbyComparingalltheionstotheHighestStandard
(01)iDilution_CompareAllAnions EvaluatessampleforiDilutionbycomparingallionsinthe
sampletotheconcentrationofthehigheststandard;dilutes
basedonionmostabovecalibration
(02)NoiDilution
SampleisnotevaluatedforiDilution
30
7. OnceallinformationintheDeterminationSerieshasbeenupdated,
clicktheSampletablebutton,andselectSaveAs,givingthetablea
uniquename.
6.
8. ThenselectSampletableSampletabletesttomakesurethere
arenoerrorsormissingvaluesinthetable.
7.
9. TobeginthesampleseriesclickStart.
ClickPausetofinishthecurrentrunandnotadvance
tothenextlineofthetable.
ClickStoptostopthecurrentsamplerun,andkeep
thesampletablefromadvancing.Iftherunis
stoppedafterthesampleinjection,thefullduration
oftherunwillneedtoelapsebeforeallofthe
samplepeakseluteoffofthecolumnandanewrun
canbeinitiated.
10.
BesuretochecktheStophardwarewhensample
tableisfinishedboxtohavethesystemshutsdown
whenthetablefinishes.
Examplesampletable:
31
BEAKERPOSITIONS:
Ontheautosamplerrackthethreerinse
positionsaresetupasfollows:
149: CCB(ContinuingCalibrationBlank)
150: CCV_Anions(ContinuingCalibration
Verification)
151: Extrabeaker
149
150
151
EMPTYVIALPOSITIONSFORDILUTION:
74
148
FirstEmptyVialPosition_Anion:74
LastEmptyVialPosition_Anion:148
Setasidethevialpositionsfrom74148forcapped,emptyvialsinwhichthedilutionswillbeperformed.
32
4.6
CALIBRATION
SUMMARYOFCALIBRATIONBY
BATCHREPROCESSING:
4.6.1
ProcessStandards
4.6.2
IntegrationofPeaks
4.6.3
UpdateComponent
Retentiontimes
4.6.4
UpdateStandard
Concentrations
4.6.5
Reprocessin2Steps
Frequencyofcalibration:Herearesomegeneral
guidelinesforwhenrecalibrationisrecommended:
1)
2)
3)
Whenacheckstandard(usuallyfromthelowmidendof
thecalibrationrange)fallsoutside10%oftheexpected
concentrationvalue.
4)
Whennewanalyteionsareaddedtotheanalysis.
4.6.1 CALIBRATION:PROCESSSTANDARDS
1. EquilibratetheinstrumentasdetailedinSection4.2Systemstartup.
2. Whiletheinstrumentisequilibrating,updatethestandardcomponentsandconcentrationsinthe
methodasdetailedinSection4.3Preparingamethodforcalibration.
3. Once the instrument is equilibrated, create and run the series of standards as detailed in
Section4.5Startingasampleseries.
4. Afterthecalibrationstandardshavecompletedrunning(ortheentiresampleseriesis
complete),clickontheDatabaseiconontheleftsideoftheMagICNetscreen.
5.
IntheDeterminationoverviewhighlightall
ofthestandardsandthenrightclickonthe
selectedstandardsandselect
inthepopupmenu.
IntheReprocessingtableselectthelowest
standard. Keep this line highlighted while
makingallchangesduringthefirststepsof
reprocessing.Thosechangeswillbeapplied
to all chromatograms in the reprocessing
table.
33
4.6.2 CALIBRATION:INTEGRATIONOFPEAKS
1. LeftclickoncewiththemouseontheChromatogramfortheloweststandard,thenusetheup
arrowkeyonthePCkeyboardtozoominonthebaselinesofallthepeaksandchecktheir
integration.
2. ClickontheIntegrationbuttonoftheEvaluationparameterswindowandselecttheSettingstab.
TheBasicsettingforSmoothingandSensitivityintegratesmostpeakswell.Onlyonoccasionwill
youhavetomodifythesesettingstooptimizeintegration.ClicktheUpdatebuttontoseethe
changesonthechromatogram.
Settings
Smoothing:Increasetodrawabroaderbaselineunderall
peaks;decreasetonarrowit.
Sensitivity:Increasetohavesmallerpeaksintegrated,decrease
tonotintegratethesesmallerpeaks.
Tipsforintegratingpeaks
Maketheminimumamountofchangesneededtoproperlyevaluatetheareaofthepeaks.Thebasic
settingsworkformostchromatograms.
UsetheIntegrationSettingstocreateastandardsetofintegrationparametersthatwillworkformost
of your chromatograms and can be applied automatically. Use Manual Peak Integration only for
samplespeaksthatdonotconformtothesenormalsettingsanddocumentthesemanualchanges.
GoalofIntegratingPeaks:Ensureallanalytepeaksarerecognizedandeachpeaksareaisevaluatedas
fullyaspossible.Establishthebestintegrationtoproduceagoodcalibration:aregularprogressionof
areaastheconcentrationofstandardsincreases.Ifyoudonothaveappropriatepeakintegration,you
willlikelyhavepoorcalibrationcurves.
34
PeakDetection
3.
Filter(optional):Themeasuringpointslistusedtocreatethedisplayedchromatogram
isfilteredusingtheSavitzkyGolayalgorithmutilizingtheFilterlengthspecified.This
featureisnormallyusedwithlowlevelUVanalysistofilterbaselinenoiseandenhance
peakrecognitionandintegration.
Negativepeaks(optional):Softwarewillevaluatenegativepeaks.Notnecessaryfor
mostanalysis.
Subtractblank(optional):IfenabledthelastdeterminationlabeledassampletypeBlankwillhaveits
measuringpointslistsubtractedfromallsubsequentchromatogramsrunbythemethod.Thisisacontinuous
processwheneverthechromatogramisrecorded.Theblankwillnothaveanypeaksevaluated.Thisoption
canbeusedintracelevelanalysiswhenbaselinecontaminationcannotbeeliminatedandwillbefactored
outmathematically.Itisnotnecessaryformostanalysis.
Standard
Blank
StandardwithBlankSubtracted
Driftcompensation(optional):Ifenabledthedriftiscalculatedforthebaselineandthensubtractedfrom
themeasuringpointlistofthechromatogram.Thismeasuringpointlististhenintegratedandevaluated.
Notneededformostanalysis.
NoDriftcompensation
WithDriftcompensation
IgnoreOverflow(optional):Whenenabledwillcausepeaksthatoverloadthedetector(flattoppeaks)tostill
beevaluated.Notneededformostanalysis.
35
Events
Integrationeventsareneededwhencustomintegrationorpeakrecognitionpatternsareneeded,or
whenbaselineeffects,contaminationpeaksorsystempeaksmakeintegrationofanalytepeaksdifficult
withthestandardSettings.
Avoidusingexcessiveintegrationevents
4. SelectEditNewtocreate
anewIntegrationevent.
5. SelecttheStartandEnd
timesfortheeventonthe
chromatogram.
Deactivatepeakdetection:Thepeakdetectionisdeactivatedinthisinterval
Peakstart:Thestartpointofthepeakissettothisvalue.TheeventPeakstartisignoredifthesetvalueis
beforetheendofthepreviouspeakorafterthefirstturningpointofthepeakinquestion.
Peakend:Theendpointofthepeakissettothisvalue.TheeventPeakendisignoredifthesetvalueisafter
thestartofthefollowingpeakorbeforethesecondturningpointofthepeakinquestion.
ValleyValley:Peaksthatarenotseparatedbythebaselineareeachgiventheirownbaseline.
Commonbaseline:Peaksthatarenotseparatedbythebaselinearegivenacommonbaseline.
Riderpeak:Peaksthatarenotseparatedbythebaselineareinterpretedsuchthatthesmallerpeaksare
evaluatedasridersonthehighestpeak.
Horizontalbaseline:Thebaselineisdrawnhorizontallyfromlefttorightfromthestartpointofthepeak.
Theintersectionpointwiththecurveortheendoftheeventistheendpoint.
Horizontalbaselineback:Thebaselineisdrawnhorizontallyfromlefttorightfromtheendpointofthepeak.
Theintersectionpointwiththecurveorthestartvalueoftheeventisthestartpoint.
Smoothing:Newvalueforthesmoothing
Minimumheight:Newvaluefortheminimumheight
Minimumarea:Newvalueforminimumarea.
36
4.6.3 CALIBRATION:UPDATECOMPONENTRETENTIONTIMES
1.
2.
6.
3.
4.
Peakswhoseretentiontimeshaveshiftedslightlyorarenotlabeledatall:
1. UpdatetheretentiontimesfortheComponentionsbyhighlightingtherowfortheioninthe
Componenttable.
2. ThenleftclickonthepeakforthationontheChromatogram.Thepeakwillbecomehighlighted
inlightblue.
3. ClicktheUpdateretentiontimebuttontoupdatetheretentiontimeinthetablewiththetimeof
thepeakdisplayed.
4. ToseethechangeonthechromatogramclicktheUpdatebuttonatthebottomofthe
Reprocessingwindow.
5. Repeatsteps14forallionsinthetable.
Peaksthataremislabeled:
6. Ifapeakiscompletelymislabeled(likeSulfateintheexampleabove),doubleleftclickontherow
oftheComponenttableforthationtoeditit.
7. EntertheRetentiontimeoftheproperpeakas
displayedabovethepeakorwhenthecursorhovers
overthepeakandtheTooltipappears(14.44inthis
case).
8. IfneededtheNameoftheComponentioncanalsobe
changedinthiswindow.
9. ClickOKwhendoneediting.ThenhittheUpdatebuttonatthebottomoftheReprocessing
windowtoupdatethechromatogramview.
10. Themislabeledpeak(Phosphateinthiscaseat12.28min)canthenbeupdatedusingsteps14
above.
37
4.6.4
CALIBRATION:UPDATESTANDARDCONCENTRATIONS
2.
3.
4.
1.
EditingStandardConcentrations
1. Toedittheconcentrationsofastandard,eitherhighlightitonthetableandselectEditEdit,or
doubleleftclickonthatstandardinthetable.EitherapproachopenstheEditStandardwindow.
2. Foruserspreparingcalibrationstandardsgravimetricallyitisrecommendedtoenterthe
concentrationscalculatedbymasseachtimethestandardsaremadetogetthemostaccurate
calibrationcurve.Userswhopreparetheirstandardsvolumetricallywillnotneedtochangethe
concentrationvaluesforthestandardsunlesstheyalterhowtheymakethem.Consistent
techniqueandClassA,calibratedvolumetricpipettesandvesselsareneededtoestablishan
accuratecalibrationcurvewithvolumetricallypreparedstandards,asthevaluesenteredintothe
methodareessentiallyanestimatebasedontheidealvaluepipetted(seeSection3.3Calibration
Standardsformoredetailsonthistopic).
3. Note:Whentheconcentrationvaluesarethesameforeachioninastandard(e.g.10ppmofall
ions)itispossibletoenterthefirstconcentrationvalue,thenclickFillingtofillthisvalueintoall
theotherconcentrationfieldsforthatlevel.
4. Oncedoneentertheconcentrationvaluesforalevel,clickOK.Repeatforallstandardlevels.
Otherfunctions
New:Createnewstandardlevels(thenumbervaluewillbeincrementedby1foreachadded)
Copy:Copythehighlightedstandardlevel.Canthenbepastedasanotherlevel(forreplicate
standards),pastedintoanothermethod,orpastedintotheCheckstandardstab.
Insert:Insertscopiedorcutstandards.
Cut:Cutsoutthehighlightedlevelbutallowsittobepastedelsewhere.
Delete:Removesthehighlightedstandard.
38
CHECKSTANDARDS(UpdatingConcentrations)
1. UpdatetheCheckstandardconcentrationsinthesame
mannerasdescribedforstandards.
2. Whenacheckstandardleveliscreatedandsavedinthe
method,amatchingSampletypewillbeavailableinthe
Sampletable.
2.
3. WhenaSampletypeofCheckstandard
ischosen,thatdeterminationcanbe
evaluatedforcheckstandardRecovery,
comparingtheresultconcentrationsof
thechromatogram.
39
4.6.5 CALIBRATION:REPROCESSINTWOSTAGES
STAGE1:BUILDTHECALIBRATIONCURVEFROMTHESTANDARDSINTHETABLE
1.
1. Allthechangesthathavebeenmade
toIntegration,Componentlabeling
andRetentiontimes,andStandard
Concentrationsshouldbemadewhile
keepingjustonestandardofthe
reprocessingtablehighlighted.Thisis
normallyStandard1.
2. Onceallofthechangeshavebeen
made,clicktheUpdatebutton.
4.
3. ThenclicktheReprocessingbutton.
5.
3.
2.
4. IntheReprocesswindow,choosethe
optiontoReprocess
5. ClickOK.Thisoptionsdoesseveralthings:
a)
Appliesallmethodparameters:Integration,ComponentlabelingandRetentiontimes,
StandardConcentrations,andMethodProgrammingfromthehighlighteddeterminationto
alloftheothersintheseries.
b)
Erasesthepreviouscalibrationpoints.
c)
BuildsanewcalibrationcurvepointbypointfromtheStandardsinthereprocessingtable
(anythingwithaSampletypeofStandard).Thismeansthateachstandardisevaluatedwith
onlyitsowncalibrationpointandtheonesbeforeitinthetable.Thelaststandardonthe
tablethereforehasallofthecalibrationpoints.
Std.1=1Cal.Point
Std.3=3Cal.Points
6. Keepmanualintegration:Ifcheckedthisoptionpreservesmanual
integrationchanges;ifuncheckedpriortoreprocessingitwilloverwrite
manualchangeswiththesettingsintheIntegrationparameters.
Std.7=7Cal.Points
40
STAGE2:APPLYTHEFULLCALIBRATIONFROMTHELASTSTANDARDTOWHOLETABLE
7.
7.
Highlightthelaststandardofthe
Reprocessingtable.
8.
ClicktheReprocessingbutton.
9.
Reprocess
10. ClickOKtoinitiatethereprocess.
11. Thisstepwillapplythefullcalibrationto
allofthestandards(samplesandcheck
standards)intheReprocessingwindow;
theywillthenbeevaluatedwillallthe
pointsinthecurve.
9.
10.
8.
Evaluatingthecalibrationgraph
12. OnceyouhaveperformedtheReprocessfromtheselecteddetermination,applyingthefullcurveto
allofthestandards,lookattheChromatogramwindowoftheReprocessingwindowandclickon
theCalibrationcurvebutton.
13. TheComponentpulldown
menuallowsyoutochangethe
viewbetweenthedifferent
calibrationcurves.
13.
12.
14.
15.
14. Relativestandarddeviation:
Generally<5%ispreferred
16.
17.
15. CorrelationCoefficient:0.99+
preferred
18.
16. Curvetype:Canbechangedin
theEvaluationparameters
Calibrationsection.A
quadraticcurvetypemaybe
mostapplicableforsuppressed
anioncalibrationrangesat2+
ordersofmagnitude.
17. Weighting:CanalsobesetintheEvaluationparametersCalibrationsection.Weightingof
1/Concentrationor1/Areamaybeneededwhenabroadcalibrationrangeiscausingthelow
calibrationpointsinthecurvetobeevaluatedwithtoohighaconcentration(USEPAMethod218.7
forHexavalentChromiumusesthisfeature).
18. Pointsatthetoporbottomofacalibrationcurvecanbeeliminatedbyrightclickingonthatlineof
thetableandselectingOff.Notethatdroppingpointsfromthetoporbottomofacalibrationcurve
meanthatonecannolongerreportatthatconcentration.
41
20.
19. Aftermakingchangestothecalibrationgraph(s),toseetheir
19.
effectonthatgraph,clicktheUpdatebutton
bottomoftheReprocessingwindow.
atthe
20. Ifchangesweremade,toapplythesechangestoallofthe
standardsintheReprocessingwindow,clicktheReprocessing
button,choose
,andthenclickOK.
21. Ifnochangesweremadetothecalibrationgraphsafter
evaluatingthem,thenskipsteps1920.
SavingthereprocessedcalibrationtotheMethod
Thenormalgoalofreprocessingacalibrationistosaveit
tothemethod.Onceitissavedtothemethod,every
determinationrunwiththatmethodwillhavetheproper
calibrationappliedtoitautomatically.
23.
22. Tosavethereprocessedcalibrationtothemethod
selectMethodSaveas
23. IntheSavemethodwindowoncecaneithergivethe
methodanewname(manycustomersusethedate
inthatnametoshowwhenthesystemwaslast
calibrated)orselectthecurrentmethodnameand
overwriteitwithanewversion.
24.
24. Ifyouchosetosavethemethodwiththesame
nameyouwillneedconfirmmessage013113Save
method?byclickingtheYesbutton.
25.
26.
25. TosaveallthechangesmadeintheReprocessing
window(includingthecalibration)totheDatabase,
simplyclicktheOKbuttonatthebottomrightofthe
Reprocessingwindow.Thiswillalsoclosethe
Reprocessingwindowandtheprogressbaratthe
bottomofthescreenwillshowthechangesbeing
saved.
27.
27.
26. IfyouclickCancelmessage015156Recalculation
willbeshown.IfyouclickNothechangedyoumade
willbelost.
42
4.6.6
CALIBRATION:APPLYTHECALIBRATIONFROMASTANDARDTOSAMPLE
DETERMINATIONS
1. Oncethecalibrationcurvehasbeenreprocessedand
appliedtoallcalibrationstandards,thecurvesavedin
astandarddeterminationcanbeappliedtosample
determinations,checkstandards,blanks,etc.that
wererun.
2.
Todothishighlightoneofthecalibrationstandards
run(Ex.ManualStd8)andthenallofthe
determinationsthatwillbereprocessedwithit.If
thedeterminationsareseparatedbysomelinesin
thedatabasewhicharenottobeincludedinthe
reprocess,dooneofthefollowing:
HolddowntheCtrlkey(Control),thenclickoneach
determinationlinetohighlightit.Clickingonita
secondtimewhileholdingCtrlwilldeselectit.
Makeabatch(Section4.7.2),appendthestandards
toit,thenalldeterminationstobereprocessedwith
thosestandards.Filterforthisbatch,thenreprocess
asmentionedbelow.
3.
ClicktheReprocessingbutton.
4.
Reprocess
5.
ClickOKtoinitiatethereprocess.
6. Afterthereprocess
completes,checktheresults
ofsamplestoensurethat
peakswereidentifiedand
integratedproperly,check
standardspassed,etc.
7. Oncedoneevaluatingthe
data,clicktheOKbuttonto
savethereprocessed
changestothedatabase.
43
44
4.7
DATABASES
1. WhenalineoftheDeterminationoverviewishighlighted,theassociatedchromatogramwill
appearintheCurveswindow,theResulttablewillappearintheResultswindow,andthe
Informationwindowhasahostoftabswithdetailedinformationabouttheanalysis,devices,
method,etc.
DATABASESHORTCUTICONS:
Openanexistingdatabase
Applyquickfilter
Closecurrentdatabase
Definespecialfilter
Opendatabasemanager
Removeappliedfilter
Logoutuserandopenloginwindow
Signselecteddeterminationonlevel1
Copy
Signselecteddeterminationonlevel2
Updatedeterminationoverviewtable
Changelayoutandcontent
Loadpreviouslysavedviewsettings
Makecurrentselecteddetermination
Savecurrentviewsettings
Showdetailoverviewforselecteddeterminations
Viewtwowindowssidebyside
Overlaycurvesoftheselecteddeterminations
Viewtwowindowsonebelowtheother
Reprocessselecteddeterminations
Unsplitwindow
Deleteselecteddeterminations
Entercommentondetermination
Openexistingreporttemplate
Search
OpenMagICNetHelp
Applylastfilter
Showmethodofthefocuseddetermination
Showhistoryforfocuseddetermination
45
Databasepages
Scrollthrough
currentPageof
Database
Numberof
records
GotoNext
Pageof
database
LastPageof
database
1. UsetheVerticalScrollBartonavigatethroughallofthedeterminationsontheCurrentPageof
theDatabase.Thereareamaximumof200determinationsperpageofthedatabase.
2. Usethe
buttontogototheNextPageofthedatabase(next200determinations).
3. Usethe
buttontogototheLastPageofthedatabase.
Sortingthedatabasebycolumn
Sortedbydate:latestdeterminationattop
Sortedbydate:earliestdeterminationattop
1. ClickthetopofacolumninthedatabaseviewtoSortthedatabasebythatcriteriain
ascendingordescendingorder.
2. AnexampleofthisissortingthedatabasebyDeterminationstart.Whenthearrowpoints
downitissortedindescendingorderlatestdeterminationruntoearliest.Whenthe
arrowpointsupthedatabaseissortedinnascendingorderearliestdeterminationat
thetopandthelatestatthebottom.Whenexportingblocksofchromatogramstoa.csv
filethisisoftenthebestformattohavethedatabaseindescendingorderasthisplacesthe
lowestconcentrationsstandardatthetopofthetable(Std1)andthiswillbemostlogicalin
tabularpresentations.Whensearchingthedatabasefordeterminationsjustcompleted,itis
oftenconvenienttohaveitsortedindescendingDeterminationstartasthiswillputthelast
determinationsrunatthetopoftheview.
3. Thedatabasecanalsobesortedbyothercriteria:byUser(shortname)willgroup
everythingrunbyaparticularoperator,byMethodgroupseverythingrunwiththat
particularmethod,etc.
46
4.7.1 DATABASES:QUICKFILTER
1. Tofilterthedatabaseforoneofthecriteriathatmakeupthecolumnsofthe
DeterminationoverviewfirstclicktheQuickfiltericon
1.
Onceyoudothis,whateverfieldyouplace
thecursoroverwillbehighlighted.Ifyou
doubleleftclickthisfielditwillbecome
theQuickfiltercriteria.
2.
InthisexampletheDeterminationstartis
thefiltercriteria.Oncethisfieldis
selecteditwillfilterthedatabaseforall
Determinationsrunonthatday.
3.
Toremoveafilterandgobacktoviewing
Alldeterminationseitherclickthe
Removeappliedfilterbutton ,orselect
Alldeterminationsfromthepulldown
Filtermenu.
4.
OtherusefulquickfiltersarebySample
type(wouldallowonetofilterforallofa
particularcheckstandardrun),byIdent(to
seeeverychromatogramofaparticular
sampleID).
4.
4.7.2 DATABASES:SPECIALFILTER
1.
TocreateamorespecificfilterclickontheDefinespecialfilterbutton.Thiswillopen
theSpecialfilterwindow,wherethesefilterscanbecreated,editedandactivated.
2. ClicktheEditbuttonandEditlineto
begineditingafilter.
47
SelectallfieldsontheEdit
filtercriterionwindow.
3. Linkbetweenthe
differentlinesofthefilter
criteria.Selections
available:AND,OR
4. Fieldcompared;havea
pulldownmenuofwhat
hasbeenusedpreviously,
orcanclicktheMore
buttontosearchthe
foldersforallthecriteria
available(seeFilterField
Selectionimagebelow.
Forthisexample
Determinationstartwas
chosen).
5. Typeofdata(text,
number,date,etc.)will
bedisplayedafterthe
Fieldisselected.
6. Operator:theoperatorforthecomparisonofthedata:[Field]=[Comparativevalue],
[Field]>[Comparativevalue],[Field]<[Comparativevalue],etc.
7. Comparativevalue:ValueagainstwhichthedataFieldiscompared.Inthisexampleitisthe
dateoftheDeterminationstart.
8. ForsomeComparativevaluesselectionsbecomeavailabletoMatchcaseandUseasterisk(*)as
wildcard.Itispossibletoaddmultiplelines
toafilter.PleaseseebelowforaFilterby
month:
Thisfilterwillshowdeterminationswitha
date>01/01/2014and<01/31/2014.
9.
ClickSavefiltertokeepitandgiveitfor
lateruseandgiveitaspecificname.
10. ClickApplyfiltertoseeitsimmediate
results.
11. Onceafilterhasbeencreateditcanbe
selectedfromtheFiltermenuatthetop
oftheDeterminationoverviewwindow.
48
4.7.3 DATABASES:BATCHES
Creatingabatch
1. Onewaytofilterdeterminationsinthedatabaseintogroupingsbasedonacurrentrun,orthe
datafallingunderaparticularcalibration,iswithaBatch.Thisisespeciallyusefulfor
reprocessingdeterminationsthatareondifferentpagesofadatabase.Onecancreatethe
batch,appendthecalibrationchromatogramstoit,thennavigatetothepagewiththedata,add
thistothebatch,andthenfilterthedatabasesoitonlyshowstheitemsinthatbatch.Itisthen
mucheasiertoreprocessthefiltereddata.Thestepsthatfollowwilldetailhowtodothis.
2.
TocreateaBatchnavigatetothe
Determinationsmenuofthe
DatabaseandselectBatchNew
batch.
3.
Namethebatchasdesired.
3.
2.
Appendingdeterminationstoabatch
4.
4.
Highlightthedeterminationstobe
includedinthebatch(inthis
exampleitisthecalibration
standards).
5.
Rightclickontheselectionandthen
chooseBatchAppendtobatch
6.
Choosethebatchthe
determinationsaretobeaddedto,
thenclickOK.
7.
Navigatetotherestofthedatayou
wishtobeaddedtothebatchand
performsteps46again.
8.
IntheBatchmenuofthe
Determinationoverviewselectthe
appropriateBatchtofilterthe
databaseforonlyDeterminationsin
thisbatch.
9.
Thebatchdisplayedisnotmuch
moremanageable.
5.
6.
8.
9.
10. Toseeallofthedeterminations
againselectfromtheBatchmenu
Nobatchselected.
10.
49
50
4.8 REPORTS
4.8.1 REPORTS:PRINTINGREPORTSONDEMAND
1. Selectoneormoredeterminationstobe
printedbyhighlightingtheminthe
Determinationovervieworbyapplyingafilter.
2. Toprintthereportforaparticular
determinationordeterminations,highlightitin
theDeterminationoverviewandthengoto
FilePrintReport.
3.
4.
3. ChoosetheSelectiontobeprinted(Selected
determinationsiftheywerehighlighted;All
filtereddeterminationsifyouranafilterfirst
andareprintingtheresultsofthefilter.
5.
6.
7.
4. SelectReporttype:
a. Originalreport(s):Ifareporttemplatewasalreadysetinthemethod.
b. Reporttemplate:Iftherewasnoneinthemethod;choosetheoneyouwishtousenow(the
followingarethedefaultreportsforthesoftware;customreportscanbegenerated):
i.
Result:Singlepagereportforeachdetermination:sampledata;chromatogram;results
table.
ii.
ResultandCalibration:SameastheResulttemplate,plusallthecalibrationdata2
graphsperpage.Everydeterminationprintswithallcalibrationgraphsmaynotwantto
usethisforallreportsjusttoshowcalibrationgraphsonhigheststandard.
iii.
SummaryReport,Anion3perpage:Basicsampledata,smallchromatogramandaresult
table;3oftheseperpageofreport.
5. SelecttheOutputtarget(theprintertobeused).
6. Ifdesired,selectthePDFoption,andthenpressthe
andfilenameandclickSave.
buttontodesignatethefiledestination
7. ClickOKontheReportoutputwindowtosendthereportstoprintand/orPDF.
51
4.8.2 REPORTS:AUTOMATICREPORTPRINTING(aftereverydetermination)
1. ChecktomakesurethatthereisadefaultprinterinMicrosoftWindowsforyour
computer.
2. ClickontheMethodbuttontoopentheMethodview.
3.
GotoFileOpentoopenthedesiredmethod.
4.
ClickontheResultsbuttonintheEvaluation
sectionofthemethod.
5.
ClickontheReporttab.
6.
Selecttheexistingreporttemplateandthepress
theEditbuttonandselectEdit,orifnoreport
templateispresent,selectEditandthenNew.
7.
SelecttheappropriateReporttemplate(see
previoussectionforadescriptionofthereport
types).
5.
6.
4.
a. Result
7.
b. ResultandCalibration
8.
9.
10.
c. SummaryReport,Anion3perpage
8.
UndertheReportoutput,checkthePrinterbox
andselectthePrinterdesiredoutoftheones
availableinthepulldownmenu.
9.
IfaPDFreportisdesiredselectthetarget
directoryandbasefilename(asdescribedin
previoussection).
10. Indicateifanemailreportisdesiredandwhat
Emailtemplatetouse(seesection_._onEmail
Templates).
11. ClickOKandthensavethesechangestothe
method.
52
4.8.3 REPORTS:CUSTOMIZINGREPORTTEMPLATES
2.
1.
GototheDatabaseview.
2.
Ifyouchosetomakeareporttemplatefroma
blanktemplate,selectToolsReporttemplates
Newtheoptionsarethe:
a.
b.
3.
3.
Itisofteneasiertocreateitfromanexisting
template.Thisisthepathwewillfollowinthis
tutorial.Todothis,selectfromtheToolsmenu
ReporttemplateManager
4.
IntheReporttemplatemanagerhighlightthe
reporttypeyouwishtomodify,rightclickonit
andthenselectCopy.
5.
RightclickontheCopyofthistemplateandselect
Rename
6.
Givetheappropriatenametothecustom
template.
4.
5.
Formreport:Oneormoredeterminationsperpage
Tabularreport:Reportmultipledeterminationsonone
table)
6.
7.
7.
ToOpenandbegineditingthereporttemplate
selectToolsReporttemplatesOpen
8.
8.
SelectthetemplateyourenamedandclickOpen.
53
PartsoftheReportTemplate(Result)
Selecttool
Gridlines
Snaptogridlines
Textbox
Header
Data
Date
Time
Pagenumber
#ofPages
Fixedreport
Group
Data
fields
Text
boxes
Fixedreport
Curve+resulttable
Resulttable
Singleresult
Curve+resulttable
Image
Line
Rectangle
Curve
Calibrationcurve
Spectrum+
maximatable
Cyclovoltamogram
54
Movingaportionofthereport
9.
9.
ClickontheSelecttool ,thenclicka
portionofthereport(e.g.Fixedreport:
AnalysisInfo).Itcanthenbedraggedto
anotherlocationonthereport(i.e.to
makeroomforadditionalfields).
Addatextfield
10.
12.
11.
Displaymultiplelines
Fillfieldwithdots
13.
12. ClicktheFillfieldwithdotsicon
to
matchtheformattingoftheotherText
fields.
13. ClickOKwhendone.
Addadatafield
14. ChoosetheDatatool
,thendrag
acrosstheareayouwishtheDatafield
tobein.APropertiesDatafield
windowwillappear.
14.
16.
15.
15. ClicktheSelectdatafieldbutton
.
Expandthefolderstolocatethedata
youwishtoaddtothisfield(Ex.Anion
DilutionFactorfromtheResults
categorythisisaUserDefinedResult
setupupinIntelligentDilutionsystems
andwillnotbepresentinallsystems).
16. ClicktheRightalignedbutton
18.
17.
,and
thentheFillfieldwithdotsicon
to
maketheformattingmatchthelookof
theotherDatafieldsthatalreadyexist
inthetemplate.
17. ClickOKtoclosetheSelectdatafield
windowwhendone.
18. ClickOKtoclosethePropertiesData
fieldwindow.
55
Editingthe<Curve+resulttable>field
19. ClickontheSelecttool
then
selectthe<Curve+resulttable>field.
20.
20. Rightclickonthefieldandchoose
Propertiesfromthepopupmenu.
21. TheCurveviewinthereportcanbe
editedbyselectingtheUserdefined
radiobutton.Onecanthenchange
thefollowing:
21.
a. Axes:Setuserdefinedvaluesfor
theseratherthanautoscaling
b. Curve:ChangethePeaklabel,
CurveandBaselineproperties
c. Display:ChangetheColorsand
LinethicknessoftheCurve,
ReferencecurveandGraphthat
aredisplayedonthereport.
22. EdittheResulttabledisplayedonthe
report.
23.
22.
25.
26.
27.
23. ChoosetheAnalysisthesevalues
applyto(incaseofhavingmorethan
onedatarecorderinamethod).
24. ChooseanyAvailableresultstobe
addedtotheDisplayedresults.
24.
28.
25. HighlighttheresultintheAvailable
results,thenclickthe
buttontomoveittotheendofthe
Displayedresults.
26. Usethe arrowstomovetheresult
addedtoorderyouwishittobe
displayedontheResulttable.
27. Usethe
toremoveany
resultsdesiredfromtheDisplayed
results.
28. ClickOKwhendoneeditingthe
<Curve+resulttablefield>.
56
Reportpreview
29. Oncedoneeditingthereporttemplate,ortocheckonhowlooksonceyou
havemadeachange,clickthePagepreviewicon
30. Editthereporttemplateagainto
correctanyissuesseeninthe
preview.
31. OncedoneeditingtheReport
template,gotoFileSave.
32. Closethetemplate.
57
58
4.9 EmailingChromatogramsfromMagICNet
Onacomputerwithanaccessibleemailprogramdothefollowing:
1. HighlightaseriesofchromatograminDeterminationoverviewoftheDatabase.
2.
IntheDeterminationsmenuselectSend
to
3. SelecttheFilenameforthechromatograms.DeterminationIDcanbeused,butSample
identificationisthemostrecognizable.
4. TheclickOK.Theprogressoftheexportwillbedetailedinabaratthebottomrightofthe
screen.
5. Amessagewillautomaticallybeopenedinyouremailprogramwiththeselectedchromatogram
filesasattachments.
59
OnacomputerwhichdoesnotanaccessibleemailprogramitwillbenecessarytocreateanExport
Templatesothatfilescanbeexportedtosomekindofremovablemedia(e.g.aUSBFlashDriveora
CDROM)andemailedfromanothercomputer.
Creatinganemailexporttemplate
1.
IntheDatabasewindowgototheToolsdirectoryandselect
Templates>Exporttemplates.
2. IntheExportTemplates
windowclickontheNew
button.
3. NamethetemplateEmail
chromatogramsorsomething
similar.
4. LeavetheFiletypesetto
*.idet(MagICNetformat).
5. Clickonthe buttontoselect
theTargetdirectorythetemplate
willsendthefilesto.
60
6. ClicktheNewdirectorybuttonto
createadistinctdatadirectoryforthe
exportedfilestogoto.
7.
Givethedirectoryadistinctnamethatyouwilleasily
remember(Ex.ICDataforExport),thenclickOK.
8.
Thenewdirectorywillnowshowup
inthedirectorytree.
9.
ClickOKtofinalizeselectionofthe
directorypath.
10. ClickOKtocompletecreationofthenew
exporttemplate.
61
11. ClickClosetoexitoutofthe
Exporttemplatewindow.
Exportingchromatogramstoemailthem
1. IntheDatabasewindow
highlightallthe
chromatogramsyouwish
toemail,thenselect
Determination>Export.
2.
IntheExportdeterminationswindowchoosethe
selectionAllselecteddatarecordsandthenuse
thepulldownmenutoselecttheappropriateexport
template(inthiscaseEmailchromatograms).
3.
ClicktheOKbuttonontheExportdeterminations
windowtosendthedatatotheExportfolder
designatedinthetemplate.
4.
Inyouremailprogram,gotothefeaturethatallows
youtoattachfilestoanemailmessage,navigateto
theExportdirectorywedesignatedintheExport
templateandselectalltheappropriate
chromatogramsyouwishtoemail.
62
4.10 CreatingandUsingControlCharts
Creatingacontrolcharttemplate
1.
ClickontheDatabasebuttontoentertheDatabaseview.
2. GototheToolsmenuandselectTemplatesandControl
charttemplates.
3.
IntheControlcharttemplateswindow,clickontheNew
button.
4.
FromthePropertiesControlcharttemplate
windowselectEditNew.
5. WithintheControlchartresultproperties
window,clickontheselectorbuttonto
selecttheresulttomonitor.
6.
Toselecttheresulttomonitor:
Clickonthemagnifyingglass
nexttotheResultsfield
toexpandtheresultsavailable.
Clickonthe
nexttoexpandanalysisfolder(Anionsin
theexample).
Click
toexpandthefolderforaparticularion(Chlorideinthisexample).
63
7.
Fromthelistofparametersavailableundertheionsfolder,choosethe
oneyoudesiretomonitorforinstanceCONC(concentration).Then
clicktheOKbutton.
8.
IntheControlchartresultproperties
window,selecttheLimitstab.Enteran
upperorlowerWarninglimit,and/oran
upperorlowerInterventionlimitforthe
parameter.
9.
LabeltheParameterbeingmonitored(Ex.
ChlorideConcentration).
10. ClicktheStatisticstabtoeditmonitoring
statisticsfortheparameter.
11.
NametheControlcharttemplate(Ex.
ChlorideConcentration)andclickOKto
savethetemplate.
12.
CreateanyadditionalControlchart
templatesneededbyrepeatingsteps311
foreachtemplate.
13.
OncefinishedclicktheClosebuttontoexit
theControlcharttemplateswindow.
64
USINGCONTROLCHARTS
1. IntheDeterminationoverviewoftheDatabase
window,highlightallthedeterminationsyouwishto
sendtoaControlchartbyleftclickingwithyour
mouseanddraggingoverthem.
2. ThenselecttheDeterminationsmenuandDetail
overview.
3. IntheOpendetailoverviewwindow,choose
SelecteddeterminationsandclickOK.
1. IntheDetailoverviewthatopens,selecttheresultyouwishtoview(Ex.Concentration).
2. Clickonthetabfortheionyouwishtoview(Ex.Chloride).
3. ClickontheControlchartbutton.
4.
SelecttheTemplatetouse(Ex.
ChlorideConcentration).Theplot
showstheconcentrationsofthe
selectedion.Anydeterminations
meetingorexceedingthewarning
limitwillhaveayellowpoint
displayedonthegraph,whichwillbe
onoraboveayellowline.Any
determinationsmeetingorexceeding
theinterventionlimitsetwillbeonor
abovearedlineandwillshowupasa
redpointonthegraph.Thetable
belowthegraphwilldisplaythe
concentrationsoftheselectedionin
eachdetermination.Thosewithinthe
limitswillshowagreenconcentrationnumberonthetable.Usethescrollbarattherightorthe
tabletoseealldeterminationsinthetable.
5. TheControlchartcanbeprintedusingthePrint(PDF)button.
65
66
4.11 CreatingandUsingDataExportTemplates
CREATINGANEXCELEXPORTTEMPLATE(.CSVTEMPLATE)
1.
ClickontheDatabaseiconattheleftsideof
theMagICNetwindowtogototheDatabase
view.
2.
IntheDatabasewindownavigatetotheTools
menuandselectTemplateExport
templates.
3.
IntheExporttemplateswindow,clickonthe
Newbuttontocreateanewtemplate.
4.
Nametheexporttemplate(Ex.csvexport)
5.
UnderFiletypeselect*.csv(Comma
Separated).
6.
Clickontheselectorbutton nexttoTarget
directorytoselectthelocationfileswillbe
exportedto.
7.
Onceyouhavechosentheappropriate
directoryforexport(orcreatedanewone),
clicktheOKbutton.
67
1.
ChosetheFilenameoftheexportfile(s)
producedbythetemplate.Thenamemaybe:
TheDeterminationID(newfileforeachdetermination)
TheSampleidentification(newfileforeach
determination)
Requestedoneachexport(newfileforeach
determination)
AFixedfilename(thedataisappendedoraddedtothis
singlefileasitisexported)
2.
ClicktheSelectfieldsbuttontochoosewhich
datafieldswillbesenttotheexportedfile.
3.
Intheexampleshownabove,theResultsfolderwaschosen,thentheAnionsanalysis,andthe
valuesforChloride.OutofthesetheConcentrationofChloridewasselectedandtheleft
selectorarrowwasclickedtoaddittotheSelectedfieldslist.Repeatthisprocessforthevalues
oneachanalyteionyouwishtobeexported.ClickOKwhenfinished.
68
4.
ClickontheOptionsbuttontoselect
theFieldSeparatorseparatingdatafieldsinthe
.csvfilecreatedandselect,tohaveacomma
betheseparator.ClickOKwhendone.
5.
ClickClosetoexittheExporttemplates
window.
USINGANEXPORTTEMPLATEFORONDEMANDDATAEXPORT
1. ClickontheDatabaseiconattheleftsideoftheMagICNetscreen.
2. Highlightallthechromatogramsinthedatabaseoverviewthatyouwishtoexport(orfilter
thedata)andthengototheDeterminationsmenuandselectExport.
69
3. IntheExportDeterminationswindowchoose:
a. Allselecteddatarecordsforchromatograms
highlightedintheDeterminationoverview
b. Allfiltereddatarecordsifafilterwasusedtoselectthe
data
4. SelecttheExporttemplatetouse(Ex.csvexport).
5. ClickOKtobegintheexport.Aprogressbarwillappearat
thebottomrightoftheMagICNetscreenwithinformation
onhowmanyofthefileshavebeensuccessfullyexported.
Thisdisappearswhentheexportiscompleted.
6. Toseetheexporteddata,
openthefiledirectory
designatedinsteps67of
CreatinganExport
Template.
7. Thedatainthe.csv(orotherfileformat)cannowbeeitherimportedintoaLIMSsystemor
formattedasafinalreport.
70
FORMATTINGFORAFORMALEXCELREPORT
8. Towidenthecolumnssoalldatacanbeseen,doubleleftclickonthegraylineatthetopofthe
columnthiswillautomaticallyexpandittofitthewidthofitscontents.
9. Tokeepchangestotheformatofthereport,savethefilewithauniquefilename(Ex.Calibration
Data100109)intheExcelWorkbookformat(.csvfilesdonotsupportformattingchanges).The
newExcelfileisnowessentiallythefinalreport.Itcanbeedited,butdatacannotbeaddedtoit
onceformatchanges(columnwidth,textadded,etc.).
71
USINGANEXPORTTEMPLATEFORAUTOMATICDATAEXPORT
1. ClickontheMethodiconattheleftsideoftheMagICNetwindowtogototheMethod
view.
2. IntheEvaluationsectionofthemethod,click
ontheResultsbutton.
3.
3. SelecttheDatabasetaboftheResultswindow.
4. IntheAutomaticexportportionofthiswindow
clickontheEditbuttonandselectNew.
2.
4.
5. Choosetheproperexporttemplatefromthepulldownmenuin
theSelectexportsettingswindow(Ex.csvexport).ClickOK.
6. TheexporttemplatewillnowbevisibleintheAutomaticexportwindow.
OR
7. SavethechangestothemethodbyclickingtheSavemethodshortcut
FileSave.
,orbyselecting
8. Anychromatogramsrunonthismethodwillnowbeautomaticallyexportedtothefileformat
anddirectoryyouselectedinthecreationoftheexporttemplate.
72
4.12 ExportingandImportingMethods
ExportingMethodsfromMagICNet
1.
ClickontheMethodicontothefarleftoftheMagICNetmainscreentoenterthe
Methodview
2.
SelectFileMethodmanager.
3. Selectthemethodyouwishtoexport.ClickontheEditbuttonatthebottomoftheMethod
ManagerwindowandselectExport.
4. Selectthelocationwhereyouwanttosavethe
exportedfile.ClicktheSavebutton.
73
ImportingMethodsintoMagICNet
1. ClickontheMethodicontothefarleftoftheMagICNetmainscreentoenterthe
Methodview
2.
SelectFileMethodmanager.
3. IntheMethod
manager
window,
selectEdit
Import.
4. Navigatetothelocationcontainingthe
Methodfilesyouwishtoimport.
5. Selectthemethodfile(s)youwishtoimport
(toselectmultiplefilesholddowntheCtrl
keyonyourkeyboardandthenleftclickwith
yourmouseoneachmethodfile).Clickthe
Openbutton.
6. Theimportedmethod
fileswillnowappearin
theMethodmanager
window.ClickCloseto
exitthemethod
manager.
74
OpenandEditImportedMagICNetMethods
7. OpenanimportedmethodbyselectingFileOpen.
8. SelectthemethoddesiredfromtheOpenmethodwindow
andclicktheOpenbutton.
ClickoneachoftheDevicesinthe
Methodfileandcomparethename
displayedintheyellowbarofthe
Methodwindowtothenameofthe
DeviceslistedintheConfigurationview
ofMagICNet.
(Inthiscasethenameinthe
methodandthenameinthe
configurationdonotmatch:
themethodsaystheICiscalled
IonChromatographthe
Configurationsaysitiscalled
850ProfessionalIC4.
75
9.
IntheMethod,Deviceswindow,rightclickontheiconforadevicethatneedstoberenamed.
SelecttheEditoption.IntheEditdevicewindowthatcomesup,changetheDevicenameto
matchthenamingintheConfigurationwindow.ClickOKtoexit.Thiswillautomaticallychange
thewaythedeviceisnamedintheProgramwindowofthemethod.
10. Changeanyotherdevices(suchasautosamplers)thatneedtoberenamed.
11. Clickonthe
toTestthemethodfor
plausibility.Anyerrorsinthemethodwillbe
notedandcanbecorrected.
12. Oncealltheappropriatechangeshavebeen
madetothemethod,selectFileSaveto
savethesechanges.
76
4.13 ADDINGUSERDEFINEDRESULTSTOTHEDATABASEVIEW(ExampleisaddingCheckStandard
Recovery)
NavigatetotheMethodview.Opentheparticular
1.
methodyouwishtoedit.
3.
2.
4.
2.
IntheEvaluationsectionofthemethodclickthe
Resultsbutton,theselecttheUserdefinedresults
tab.
3.
TocreateanewUserdefineresultclicktheEdit
buttonandselectNew.
4.
IntheDefineresultwindow,selecttheResulttype
fromthepulldownmenu:
Singleresult:Anindividualcalculationthatwillonly
becalculatedforonce(e.g.foroneComponention).
Componentresult:Thiscalculationwillbe
performedforalloftheComponentions(inthis
exampleaComponentresultwillbecreated).Ifthis
ischosen,theAnalysisinthemethodtowhichit
appliescanalsobeselected.
5.
EntertheResultname.
6.
ThePropertiesfieldiswheretheformulawillbe
entered.Todoso,clicktheFormulaeditorbutton
5.
5.
7.
TheFormulaeditorwindowhastwomainfields
fromwhicheitherVariablesorOperators/Functions
canbechosentowritethelogicoftheequation.
8.
TheMiscellaneousfoldercontainstheveryuseful
Casestatement,whichcanbeusedtosetup
conditionallogicforaformula,essentiallydefining
whenitisusedorforwhattypeofdata.
Thecasestatementiswritteninthisformat:
Case(Condition;True;False[;Error])
10.
TheConditioniswhatyouareevaluatingor
comparingintheformula.ItessentiallystatesIf
thisconditionistrue,then
TheTruestatementfollowsthesemicolon;
afterConditionandisthevaluetheformulaequals
ortheactionperformediftheConditionistrue
TheFalsestatementfollowsthe;aftertheTrue
statementandisthevalueoractionperformedif
theConditionisnotmet
9.
TheErrorstatementisoptionalandifused
comesafterthe;followingtheFalsestatement.Itdetails
whatvalueisreturnedoractionistakenifanerroroccursinthecalculationoftheformula.Acloseparenthesis)
followstheerrorstatementandmarkstheendoftheformula.IfnoErrorstatementisusedthenthis)followsthe
Falsestatement.
9. TousetheCasestatementhighlightCase,thenclicktheAddbutton.
10. SetCondition:selectthevaluefromtheVariablesfieldandclickAdd.Thenentera;afterward.Inthisexamplethe
conditionselectedwasTYPENAMEofthedetermination=Checkstandard.
77
11. SetTruestatement:forcheckstandard
selectundertheVariablesfield,Results
AnionsAC(whichisAllComponents)
REC(whichischeckstandardrecovery).
12. OncetheRECishighlightedclickAddto
insertitintotheformulaafterthe;
followingCheckstandard.
13. ThevaluethatwillappearisRS.(forResults)
Anions(forthenameoftheAnalysis).AC
(Allcomponents).REC(Recovery).
11.
15.
12.
16.
14.
14. SetFalsestatement:Adda;afterthis,
thenenterv(openquotationmark
followedbyaspace,thenaclosedquotation
mark.Thismeansthatnovaluewillbe
displayedwhentheTYPENAMEofthe
determinationisnotaCheckstandard.
13.
15. SetErrorstatement:Adda;thenenter
v.Thismeansnovaluewillbereturned
forCheckstandardrecoveryifanerror
occursinthecalculation.
17.
16. Entera)toclosetheformula.
17. ClickOKwhendoneenteringvaluesintothe
Formulaeditor.
18. EntertheUnitfortheUserdefined
result.Itcanbeselectedfromthepull
downmenuortypedin.%was
enteredforthisexamplecalculation.
19. EntertheDecimalplacestowhichthe
resultwillbedisplayed.
18.
20. EnteraDescriptionofthisresultif
desired(e.g.anexplanationofthe
calculation)ifdesired.
19.
20.
21. ClicktheOKbuttontoacceptthisUser
definedresult.
22. Savethemethodtokeepthischange.
21.
78
AddingUseDefinedResultstotheDatabaseView
23. ToviewtheCheckStd.RecoverycalculationintheResultstableforyourdatabase,navigatetothe
Databaseview,thentheResultswindow.
24. RightclickonthewhitebackgroundoftheResultswindow,theleftclickonthePropertiesResults
buttonthatappears.
25. Scrolltothebottomof
theColumnsavailable,
highlightUserdefined
componentresultsand
thenclickthe
buttontomoveittothe
Columnsdisplayed.
26. ClickOKoncedone
editingtheProperties
resultswindow.
27. AllUserdefined
componentresultsresult
willnowbedisplayedin
theResultswindowof
thedatabase.
79
80
SECTION5.0
ROUTINEMAINTENANCE
81
Ascarite in
drying tube
(6 months)
Peristaltic
pump tubing
(monthly)
Eluent
aspiration filter
(quarterly)
Peristaltic
pump tubing
(monthly)
Guard
columns/ RP2
Guard
(monthly)
Ultrafiltration
cell membrane
(approximately
weekly or
every 200
samples)
In-line filters
(quarterly)
IC Pump Parts
(yearly)
Weekly maintenance
Replace autosampler ultra-filtration membrane (if present):
for standard water samples change once per week or
every 200 samples.
82
1. Remove screws
and disassemble
the ultra-filtration
cell.
2. Using tweezers
provided remove
the old filtration
membrane.
5. Place membrane
in clean beaker
filled with
ultrapure water
and soak for 2
minutes.
7. Reassemble cell
as shown on left
(screws pass
through nonthreaded half of
cell).
6. Use tweezers
to place
membrane in
cell.
8. Carefully
tighten
screws in
star-pattern
to avoid
cracking cell.
83
4.
1. Click on the
Workplace Button.
2. Select the desired
method.
Allow the
system to
run for 30
minutes and
then record
the
operating
pressure in
log book.
Compare to
previous
readings. A
gradual
increase in
pressure by
1+ MPa is a
sign that the
RP2 guard
disk an filter
need to be
changed.
CO2 Scrubber
Cartridge
(6.2837.000)
84
Bi-weekly maintenance
Check flow rate of autosampler peristaltic pump tubing- if it is below 80%
the recommended flow rate, replace the peristaltic pump tubing.
Check the flow rate out of the acid and water waste lines of the chemical
suppressor (MSM)- if it is below 80% the recommended flow rate, replace
the peristaltic pump tubing.
2.
4.
5.
3.
4.
85
Description
Inner Diameter
Delivery
Use
OLDER TUBING STYLES (733, 752, 753, 766, 788, 790, 791, 793, 833, 838, 861)
6.1826.010
1.02 mm 0.05mm
6.1826.030
0.51 mm 0.05mm
6.1826.040
0.76 mm 0.05mm
6.1826.060
0.51 mm 0.05mm
6.1826.070
1.42 mm 0.05mm
6.1826.110
0.51 mm 0.05mm
6.1826.120
0.59 mm 0.05mm
6.1826.130
1.02 mm
0.0127mm
6.1826.140
1.25 mm
0.0127mm
0.38 mm
6.1826.320
0.48 mm
6.1826.330
0.64 mm
No special applications
6.1826.340
0.76 mm
6.1826.360
1.02 mm
6.1826.380
1.25 mm
~ 2 mL/min. (Rate=3)
1.37 mm
6.1826.316
M.1826.040
Waste
bundle
Suppressor
waste tubing
2. Startup hardware/measure
baseline in the software.
3. While the instrument is running,
hold a paper towel or beaker
under the suppressor waste lines
and observe the flow out of the
lines. It should be a drop every
2-3 seconds from each waste line
(about 0.4-0.5 mL/min. if
measured with graduated
cylinder.
86
Monthly maintenance
Replace tubing on peristaltic pump(s).
Replace RP2 guard disk and paper filter
(wear clean gloves while replacing these
parts to avoid contaminating the system).
Triple rinse suppressor regenerant (acid)
and rinse (water) bottles with ultrapure
water.
Tubing cartridge
Snap action lever
(loosens here)
Contact
pressure levers
Peristaltic tubing
1.
2.
Push
orange/
yellow tubing
to at least
third barb on
fitting
3.
4.
5.
87
Changing RP2 guard disk and filter (monthly or more frequently if needed)
1.
3.
6.
2.
3.
4.
5.
8.
7.
Reassemble holder.
Tighten by hand, then
turn with wrench (do not
over-tighten).
Quarterly maintenance
Replace in-line filters*.
Replace eluent filter (if used)*.
Clean peristaltic pump rollers with DI
water.
* Wear clean gloves when replacing these parts to avoid
contaminating the system.
88
(quarterly)
Cation systems have one in-line eluent filter; Anion systems may have 3-4 (eluent, H2O, H2SO4, and filter before
CO2 Suppressor)
(6.2821.120)
1.
Paper filter
4.
2.
3.
Replacement filter
(6.2821.130- 10 Pack)
Connector
6.2744.180 with
built-in filter (for
H2O and H2SO4
lines of MSM)takes same filter
replacement
(6.2128.130) as
eluent in-line filter
5.
89
1.
Remove tubing
cartridges (see
instructions for
changing peristaltic
pump tubing).
4.
2.
5.
3.
1.
Remove tubing
cartridges (see
instructions for changing
peristaltic pump tubing).
Roller: 4.850.4460
4.
3.
Circlip: v.110.0040
5.
90
Semi-annual maintenance
Replace check valves and piston seals on
IC pump (semi-annual replacement on instruments
that run a high sample load; otherwise replace these
parts annually)
Pump maintenance (semi-annual for high-usage instruments- run 24/7; annual for
instruments with lesser usage)
91
Pump maintenance (semi-annual for high-usage instruments- run 24/7; annual for
instruments with lesser usage)
Pump maintenance (semi-annual for high-usage instruments- run 24/7; annual for
instruments with lesser usage)
92
Pump maintenance (semi-annual for high-usage instruments- run 24/7; annual for
instruments with lesser usage)
Pump maintenance (semi-annual for high-usage instruments- run 24/7; annual for
instruments with lesser usage)
93
Pump maintenance (semi-annual for high-usage instruments- run 24/7; annual for
instruments with lesser usage)
2.
Up
3.
1.
2.
3.
Hold the guide sleeve in the pump head and flip the
pump head over, placing it face-down on a table (with
piston chambers and the guide sleeve facing toward
you). Maintain light pressure on the guide sleeve in
this step so that the seal does not insert crookedly into
the pump head.
4.
5.
(1)
4.
Pump maintenance (semi-annual for high-usage instruments- run 24/7; annual for
instruments with lesser usage)
94
Pump maintenance (semi-annual for high-usage instruments- run 24/7; annual for
instruments with lesser usage)
Sample in
Sample waste
95
Annual maintenance
A Metrohm technician or an operator who has
gone through Metrohm maintenance training
performs the following tasks:
Complete overhaul of IC pump (PM)- this includes
replacement of piston seals, piston springs, and piston rods.
Replace all PTFE and PEEK tubing.
PEEK tubing for system flow path (6.1831.010, 0.25mm ID)
PTFE tubing for suppressor rinse and regenerate lines
(6.1803.020, 0.97 mm ID)
96
Parts for IC Pump Rebuild (850, 872, 881, 882, 883, 930, 940,
942)
M.900.073K Metrohm Pump Rebuild Kit for 850,
872, 881, 882, 883, 930, 940,942
(Consumable parts needed for Pump PM)
2
2
2
1
1
X
X
X
X
X
6.2741.020
6.2824.070
6.2824.060
6.2824.160
6.2824.170
Piston Gasket
Zircon Piston
Spring, Auxiliary Piston 44mm
Outlet Check Valve for ProfIC
Inlet Check Valve for ProfIC
97
Pump maintenance
Replacing piston rods and springs #1
3.
4.
5.
6.
Pump maintenance
Replacing piston rods and springs #2
2.
3.
4.
5.
6.
98
99
100