MagIC Net User Guide

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:

#gSalt=Desired Concentrationx FormulaWt.xVolumeDesiredx(1/%compositionforsomesalts)

(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

* Note: Because the specific gravity of water= 1g/ml, in these

calculationsyouwillbeweighingout(ingrams)theInitialMassof
Sample
Stock Standard Needed and Final Standard Mass rather than
measuringoutvolume.
Be sure to use new pipette tip for each Individual Ion
Concentrate to avoid cross-contamination of standards.

1.010

Balance

1. Placeclean(preferablynew)plasticbottleofappropriatesize
onthebalance.Zerobalance.

2. Add calculated Initial Mass of Individual Ion Concentrate

Neededforaparticularcomponentiontothebottle.Recordthe
actualmassaddedtothelimitofdecimalplacesdisplayedbythe
balance. Repeat this procedure for each component ion,
recordingtheactualmassofeachionadded(donotzerobalance
inbetweenadditionsofcomponentionskeeparunningtotalof
mass).(Ex.1.010gof1000ppmSO42addedto100mLbottle)Add
100.051
enoughUltrapure,ICgradewater(16Morbetter)tobringthe
massofsolutionuptothedesiredFinalStandardMass.Record
the final mass achieved (to the limit of decimal places on the balance). Mark the appropriate
concentration(s)onthestandardbottle.(Ex.Standarddilutedto100.051g)

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)

5. Place clean(preferably new)plastic bottleof appropriate size on the

balance(usesmallerbottleEx.30mL).Zerobalance.

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).

, and then choose the

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

3. To Increment the numbering of the

Ident, Sample type and Position,
highlight the first standard line, click
ontheIncrementbutton ,thenleft
click and hold on the Ident field for
line2(Standard1)draghorizontallyto
cover the Sample type and Position
columns, and down to encompass
thesefieldsonlines36.Thenrelease
themousebutton.
4. TheIdent,SampletypeandPosition
linesshouldallincrementby1
numberwhenthemousebuttonis
released.
5. Edittheremainingsampletableinformationasneeded.Herearesometipsonusingthe
shortcutsintheEditmenuoftheSampletable:

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)

When new eluent is made (slight changes in eluent

concentrationfrombatchtobatchcancauseslightshifting
of peak retention times and potential mislabeling of
peaks).

2)

When a major change is made to the system (PM

maintenance is done on the IC pump, a new column or
guardcolumnis put on, or autosampler peristaltic pump
tubingischanged).

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.

Reprocess the standards first so you can

makeallthechangesneeded.
(Inalaterstepyouwillreprocessthehighest
standard with all other determinations to
saveonprocessingtime.)
6.

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.

Use the settings on the Peak detection tab to finetune

integration(ifneeded):
MinimumheightandMinimumarea:Usetosetthresholdfor
peakrecognition:decreasetheminimumvaluetoallowsmaller
peakstobeintegrated;increasetoexcludebaselinenoisefrom
beingintegratedaspeaks.
Integrationstart:Timewhensoftwarebeginsintegratingpeaks;
setjustafterinjectionvoid.
Polarity:(+)foranionsandmostotheranalysis;()forcations

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.

10. ChoosetheTexttool ,thendrag

acrosstheareayouwishthetextboxto
beon.
11. ThePropertiesTextfieldwindowwill
appear.Enterthetextinthefieldbelow
(Ex.DilutionFactor).TheFontand
justificationcanbealteredasneeded.

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

General Overview of Consumable Parts

Ascarite in
drying tube
(6 months)

Peristaltic
pump tubing
(monthly)

Eluent
aspiration filter
(quarterly)
Peristaltic
pump tubing
(monthly)

H20 and CO2

Scrubber
Cartridges
(varies)

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.

Check operating pressure of IC pump after running for

30 minutes. Record in operational log and compare to
pressure from previous weeks. This will allow you to note
unusual increases in pressure that may necessitate RP
guard disk or guard column change, or other maintenance.
Check H2O and CO2 Scrubber cartridges on CO2
Suppressor
At end of week run 1+ DI water blanks to flush out sample
flow path

82

Changing the ultra-filtration membrane (slide 1)

1. Remove screws
and disassemble
the ultra-filtration
cell.

2. Using tweezers
provided remove
the old filtration
membrane.

3. Rinse cell with ultrapure water. Clean with soft brush

if necessary. NOTE: Use only ultrapure water or
ethanol to clean the cell. Other solvents (i.e.
acetone) will damage it. Make sure no discolorations
or residue remain in the cell or cell grooves.

Changing the ultra-filtration membrane (slide 2)

Cardboard
separator
Wax paper
separator
Filtration
membrane

4. Locate replacement filtration membrane

(6.2414.020 or 6.2414.030). Do not
confuse it with the thick, white cardboard
or blue wax paper separators. Handle
membrane with tweezers to avoid
contamination.

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

Check operating pressure (weekly)- in MagIC Net software

4.
1. Click on the
Workplace Button.
2. Select the desired
method.

3. Click the Start HW

button.

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.

Check H2O and CO2 Scrubber Cartridges (weekly)

H2O Scrubber
Cartridge
(6.2837.010)

CO2 Scrubber
Cartridge
(6.2837.000)

Check H2O Scrubber Cartridge

(Lifespan varies according to ambient conditions)

Check the color of the orange or purple beads in the H2O

scrubber cartridge. If the majority have become pale or
translucent (lost their color), they are expended and need
to be regenerated. Regeneration is accomplished by
removing the end-cap from the cartridge, pouring the
beads into a watch glass or other flat glass container, and
heating the beads in an oven at 1000 C for 24 hours. An
extra H2O scrubber cartridge is provided to be in use while
the beads from the exhausted cartridge are being
regenerated.

Check CO2 Scrubber Cartridge

(Approx. lifespan 4-6 months)
One can tell that the CO2 scrubber cartridge is exhausted in
one of several ways:
1) Baseline conductivity increases to 12-20 S/cm.
2) The brown layer of the cartridge starts to clump or look wet
(water scrubber was not changed often enough).
The CO3 scrubber cartridge cannot be regenerated. It is a
good idea to have an extra one on-hand at all times.

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.

Checking flow from autosampler peristaltic tubing (slide 2)

For MagIC Net Software

2.

Click on the Manual Icon in

MagIC Net.
3.

Select the Tower tab on the

autosampler (in version 2.0+ ) or the
Rack tab (in version1.0-1.1) , select one
of the Special beakers, and hit Start.

4.

Set the lift position to the Work position

and hit start (in version 1.0-1.1 select the
Tower before doing this).

5.

Click on the peristaltic tab of the

autosampler. Press the Start button and
time the length of the pump time with a
stopwatch, collecting the flow out of the
peristaltic tubing with a graduated
cylinder or test tube. Press Stop when
done. Divide the volume of liquid
collected by the number of minutes
timed to get the flow rate in mL/min.

3.
4.

85

Checking flow from autosampler peristaltic tubing (slide 3)

PERISTALTIC TUBING AND APPROXIAMTE DELIVERY RATES
Order No.

Description

Inner Diameter

Delivery

Use

OLDER TUBING STYLES (733, 752, 753, 766, 788, 790, 791, 793, 833, 838, 861)
6.1826.010

Pump tubing with 2 white-white bands

(PVC- Tygon ST)

1.02 mm 0.05mm

1.41 mL/min. (20rpm) 1.69

mL/min. (24 rpm)

On autosampler- standard delivery for direct injections

6.1826.030

Pump tubing with 2 orange-yellow bands

(PVC- Tygon ST)

0.51 mm 0.05mm

0.40 mL/min. (20rpm) 0.48

mL/min. (24 rpm)

Can be used for suppressor solutions; not compatible with organic

solvents

6.1826.040

Pump tubing with 2 black-black bands

(PVC- Tygon ST)

0.76 mm 0.05mm

0.75 mL/min. (20rpm) 0.90

mL/min. (24 rpm)

Sample delivery- common with ultra-filtration; pulls from outlet

(top) of filtration cell

6.1826.060

Pump tubing with 2 orange-yellow bands

(PP-PharMed)

0.51 mm 0.05mm

0.47 mL/min. (20rpm) 0.56

mL/min. (24 rpm)

Most common suppressor solution tubing; can handle up to 5%

organic solvents

6.1826.070

Pump tubing with 2 yellow-yellow bands

(PVC- Tygon ST)

1.42 mm 0.05mm

2.55 mL/min. (20rpm) 3.06

mL/min. (24 rpm)

Sample delivery- common with ultra-filtration; delivers to inlet

(bottom) of filtration cell

6.1826.110

Long-life Pump tubing with 2 yellow-orange

bands (PVC-Tygon LFL)

0.51 mm 0.05mm

0.44 mL/min. (20rpm) 0.53

mL/min. (24 rpm)

6.1826.120

Long-life Pump tubing with 2 orange-white

bands (PVC-Tygon LFL)

0.59 mm 0.05mm

0.44 mL/min. (20rpm) 0.53

mL/min. (24 rpm)

6.1826.130

Long-life Pump tubing with 2 white-white bands

(PVC-Tygon LFL)

1.02 mm
0.0127mm

1.41 mL/min. (20rpm) 1.69

mL/min. (24 rpm)

Sample delivery- commonly used with preconcentration

6.1826.140

Long-life Pump tubing with 2 grey-grey bands

(PVC-Tygon LFL)

1.25 mm
0.0127mm

2.18 mL/min. (20rpm) 9.7

mL/min. (stage 15)

Sample delivery- can be used to deliver sample to ultrafiltration

cell (instead of yellow-yellow tubing)

NEW TUBING (850, 858, 863, 881, 882)

6.1826.310

Pump tubing LFL 3 orange-green bands (PVCTygon LFL)

0.38 mm

~0.4 mL/min. (Rate=3)

Pump tubing for Bromate application using triiodide method

6.1826.320

Pump tubing LFL 3 orange-white bands (PVCTygon LFL)

0.48 mm

0.4-0.5 mL/min. (Rate=3)

For suppressor solutions and acceptor solutions for dialysis

6.1826.330

Pump tubing LFL 3 orange-green bands (PVCTygon LFL)

0.64 mm

~0.7 mL/min. (Rate=3)

No special applications

6.1826.340

Pump tubing LFL 3 black-black bands (PVCTygon LFL)

0.76 mm

0.75-0.9 mL/min. (Rate=3)

Used with ultrafiltration- delivery of filtrate to IC

6.1826.360

Pump tubing LFL 3 white-white bands (PVCTygon LFL)

1.02 mm

1.2-1.4 mL/min. (Rate=3)

General sample delivery

6.1826.380

Pump tubing LFL 3 gray-gray (PVC-Tygon LFL)

1.25 mm

~ 2 mL/min. (Rate=3)

May be used to deliver sample from needle to Ultra-filtration Cell

1.37 mm

2.5-3.0 mL/min. (Rate=3)

May be used to deliver sample from needle to Ultra-filtration Cell

1.25-1.5 mL/min. (Rate=3)

Autosampler tubing for Ethanol producers

6.1826.316
M.1826.040

Pump tubing LFL 3 yellow-yellow bands (PVCTygon LFL)

Peristaltic Pump Tubing (Solvent Resistant)

Checking flow from suppressor acid and water waste lines

Waste
bundle

1. Locate the suppressor waste

tubing; remove it from the 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.

Changing peristaltic pump tubing (monthly or more frequently if needed)

Tubing cartridge
Snap action lever
(loosens here)

Contact
pressure levers
Peristaltic tubing

1.

(full tension position)

Push down contact pressure levers to

loosen them completely.

2.

Push bottom right of snap action lever to

release the cartridge (hinges at left).
Remove tubing cartridges from IC.

Push
orange/
yellow tubing
to at least
third barb on
fitting

3.

Disconnect lines at inlet and

outlet of peristaltic pump
tubing. Remove peristaltic
tubing from IC. Remove barb
fittings from end of tubing.
Insert them into new
peristaltic tubing of same
kind.

4.

Thread new peristaltic

tubing through center
groove of tubing
cartridge. Stoppers
should fit in a matching
indentation in cartridge.

5.

Replace tubing and

cartridges in IC. Carefully
reconnect lines. Ensure
contact pressure lever is at
450 angle from the corner
of the cartridge for proper
tension.

87

Changing RP2 guard disk and filter (monthly or more frequently if needed)

1.

Loosen RP2 holder carefully

with two wrenches.

3.

Remove old RP2 guard

disk.

6.

Insert new paper frit using

triple-rinsed tweezers and
gently push edges of frit
into holder rim.

2.

Place holder with long

portion facing up.

3.

Unscrew and remove

upper housing.

4.

Remove paper frit by

carefully pushing a small
wire or paper clip through
the back of the holder.

5.

Replace with new paper

frit and RP2 guard disk
(6.1011.130 (10 Pk. Replacement)handle with gloves to avoid
contamination).

8.
7.

Insert new RP Guard

disk.

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

Changing In-line Filters

(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.

Loosen holder carefully

with two wrenches.

Paper filter

4.
2.

Remove filter using end

of PEEK tubing (scrape out,
but avoid scratching holder).

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.

Insert new filter using

PEEK tubing to gently
push edges of filter into
holder rim.
Reassemble holder.
Tighten by hand, then
turn with wrench (do not
over-tighten).

Change Eluent Filter (quarterly- if used)

1. Prepare the eluent filter by pushing ethanol or

methanol through it with a syringe, then flush
with DI water.
2. Handle the filter with gloves to avoid
contamination.
3. Screw new filter onto fitting at the end of the
eluent line.

89

Cleaning peristaltic pump rollers (quarterly)

(style with disk holding them in place)
Tubing cartridges

1.

Remove tubing
cartridges (see
instructions for
changing peristaltic
pump tubing).

4.

Remove rollers from

mechanism.

2.

5.

Remove screws holding

bar in place.

3.

Remove screws holding

disk in place; gently pull
disk off of roller
mechanism.

Rinse rollers with Deionized water. Dry and

replace on roller
mechanism.
Reassemble pump.

Cleaning peristaltic pump rollers (quarterly)

(style with clips holding them in place)
2.

1.

Use a small flat-tip

screwdriver to carefully
remove the circlips
holding the rollers in
place. Use caution as
they can fly out of your
grip very easily.
Should any of the rollers or circlips be damaged, their part
numbers for re-order are as follows:

Remove tubing
cartridges (see
instructions for changing
peristaltic pump tubing).

Roller: 4.850.4460

4.
3.

Remove rollers from

mechanism.

Rinse rollers with Deionized water. Dry and

replace on roller
mechanism.

Circlip: v.110.0040

5.

Carefully use the

screwdriver to push the
circlips back into place.
Reassemble the pump.

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)

Replace sample and waste lines (as

needed).
Replace CO2 scrubbing agent in drying
tube on eluent bottle (if used)

Pump maintenance (semi-annual for high-usage instruments- run 24/7; annual for
instruments with lesser usage)

Replace outlet check valve (6.2841.160)

Remove the outlet valve
1. Unscrew the connection capillary to the outlet check
valve.
2.
Use an adjustable wrench to carefully loosen the check
valve cover. Hold the pump head while loosening with
the wrench to avoid causing damage to it.
3.
Remove the outlet check valve from the valve holder.

Re-insert outlet valve into pump head

1. Re-insert a new check valve into the check valve cover.
2. Carefully thread the cover into the pump head (avoid
cross-threading) and tighten with a wrench until pressure
with only 2 fingers on the wrench no longer allows
movement (avoid over-tightening).
(To clean check valves see section on this topic in the IC
instrument manual),

91

Pump maintenance (semi-annual for high-usage instruments- run 24/7; annual for
instruments with lesser usage)

Replace inlet check valve (6.2841.170)

Remove the inlet valve
1. Unscrew the connection capillary to the inlet check valve.
Use a column plug to cap the eluent line coupling so it
does not leak.
2. Use an adjustable wrench to carefully loosen the check
valve cover. Hold the pump head while loosening with the
wrench to avoid causing damage to it.
3. Remove the inlet check valve from the valve holder.

Re-insert inlet valve into pump head

1. Re-insert a new check valve into the check valve cover.
2. Carefully thread the cover into the pump head (avoid
cross-threading) and tighten with a wrench until pressure
with only 2 fingers on the wrench no longer allows
movement (avoid over-tightening).
(To clean check valves see section on this topic in the IC
instrument manual),

Pump maintenance (semi-annual for high-usage instruments- run 24/7; annual for
instruments with lesser usage)

Removing the Pump Head (prior to servicing pistons)

92

Pump maintenance (semi-annual for high-usage instruments- run 24/7; annual for
instruments with lesser usage)

Removing the Piston Cartridges

Remove piston cartridge from pump
head
1. Flip pump head so that the back end
of the pistons are facing down.
2. Loosen the piston cartridge with an
adjustable wrench, then unscrew it
from the pump head by hand.
3. If the steel backup ring (3) remains
within the pump head when the piston
cartridge (9) is removed, shake the
pump head carefully until the backup
ring falls out.
4. Occasionally the piston seal will
remain on the end of the piston. If this
is the case carefully remove it from
the piston and replace the seal with
the steps to follow.
5. Remove both piston cartridges from
the pump head.

Pump maintenance (semi-annual for high-usage instruments- run 24/7; annual for
instruments with lesser usage)

Removing the Piston Seals (Piston Gaskets; 6.2741.020)

Remove the piston seals
1. Place the pump head face-down on a table or
other stable surface so that the openings of the
piston chambers are facing up toward you.
2. Insert the threaded end of the piston seal
removal tool (1) into the piston seal (3) and
twist the tool to thread it lightly into the seal. Take
care not to thread past the seal and into the pump
head as this could damage it.
3. Wiggle the piston seal tool lightly side to side to
loosen the seal in the pump head, then pull
upward to remove the seal completely.
4. Remove both piston seals in this manner.
Note: Once the tool had been threaded into a seal,
that seal is ruined and cannot be re-used. Do this
procedure only when replacing old piston seals.

93

Pump maintenance (semi-annual for high-usage instruments- run 24/7; annual for
instruments with lesser usage)

Replacing the Piston Seals (Piston Gaskets; 6.2741.020)

1.

Insert new piston seals

2.

Up

3.

1.

Insert a new piston seal (3) into the recessed sleeve

end of the piston tool guide sleeve(2). The springside of the seal should be facing upward.

2.

Hold the pump head facing upward (piston chambers

facing down) and insert the guide sleeve(2) into the
pump head.

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.

Use the back (non-threaded) end of the piston

removal tool (1) as a plunger to push the piston seal
into place. Tap the seal lightly several times to ensure
that it has clicked firmly into place.

5.

Repeat process for other piston seal.

(1)
4.

NOTE: If the piston seal is inserted into the pump head at

an angle, it could cause the piston to lock up in the pump
head and potentially damage or break it.

Pump maintenance (semi-annual for high-usage instruments- run 24/7; annual for
instruments with lesser usage)

Reseating pistons in pump head

Reseat pistons in pump head.
1. Hold the pump head with the face up and the
piston chamber openings facing down.
2. Carefully reinsert the piston assembly (9) into
the pump head and hand-tighten it.
3. Be careful not to cross-thread the pump head as
the piston cartridge threads are steel and the
pump head is PEEK and will be damaged in the
process.

94

Pump maintenance (semi-annual for high-usage instruments- run 24/7; annual for
instruments with lesser usage)

Mounting the pump head

Mount the pump head onto the IC
1. Push the pump head carefully onto the four
fastening bolts of the IC.
2. Push the pump head carefully back onto the chip
reader and hold it in place.
3. Tighten the four fastening screws using a hex key
in an alternating, cross-wise pattern, beginning
with the screw in the top left corner.
4. Once this screws threads catch, it will then be
possible to alternate tightening the other screws
to mount the pump head in an even manner.
Note: If the pump head is mounted improperly or with
excessive force the chip reader could be damaged. It
is recommended to have a qualified Metrohm service
representative perform pump maintenance for you.

Replace sample and waste lines (semi-annually)

Sample in

Sample waste

Replace sample and waste lines with equivalent lengths of PTFE

or PEEK tubing (PTFE: 6.1803.030, 0.5mm ID; PEEK: 6.1831.0).

95

Replace CO2 Absorbing Agent in Drying Tube(quarterly)

(For anion systems using bottled eluent)

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

Annual pump maintenance

Replace piston check valves and piston seals as

mentioned in the Semi-annual maintenance section.
Replace zirconium oxide pistons and springs (as
described in the instructions to follow).
Reseat pistons and mount pump head as described in
the semi-annual maintenance section.

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Pump maintenance
Replacing piston rods and springs #1

Disassembling the piston cartridge.

1.
2.

3.

4.

5.

6.

Slide the backup ring (8) off of the end of

the piston.
Use one adjustable wrench to hold the
piston cartridge (7) in place by affixing it to
the hexagonal ring at the end of the
cartridge.
Use a second adjustable wrench to slightly
loosen the piston cartridge screw (1). Be
careful- the piston cartridge screw can
suddenly pop loose. Loosen the screw
manually to better prevent it from flying
loose.
Remove the zirconium oxide piston (3)
from the cartridge with the inner plastic
sleeve (6), spring (5), spring retainer (4),
retainer washer (2), and piston screw (1).
Replace the zirconium oxide piston (3) and
the spring (5). Retain the other parts for
later reassembly.
Clean the inside of the piston cartridge (7)
and piston screw (1) with methanol and DI
water using a cotton swab, then dry
thoroughly.

Pump maintenance
Replacing piston rods and springs #2

Reassembling the piston cartridge.

1.

2.
3.

4.
5.

6.

Clip the retaining washer (2) onto the

notched metal portion of the new zirconium
oxide piston (3).
Slide the spring retainer (4) onto the piston.
Use a very tiny amount of vacuum grease or
paraffin grease to lightly lubricate the outside
of the new spring (5). Wipe off the excess
with a tissue or paper towel.
Slide the spring (5) onto the piston, then
place the inner plastic sleeve (6) over it.
Carefully insert this entire assembly into the
piston cartridge (7), hold it horizontally and
tighten it until the first few threads of the
screw catch. The completely hand-tighten
the screw into the cartridge.
Turn the piston assembly vertical and place
the backup ring on the end of the piston
that protrudes from the piston cartridge.

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For more information on a Performance Maintenance or Total Care Service

Package, please contact your local Metrohm service or sales representative,
or contact Customer Support at the number listed below.

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