04MeasuringConditionsbyElementFurnaceAnalysisMetho島津原子吸收光譜應(yīng)用手冊(cè)(石墨爐篇)

ATOMICABSORPTIONSPECTROPHOTOMETRYCOOKBOOK

Section4

MeasuringConditionsbyElementofFurnaceAnalysisMethod

AtomicAbsorptionSpectrophotometryCookbook

Section4

CONTENTS

7.MeasuringConditionsbyElementofFurnaceAnalysisMethod1

7.1Measuringconditions1

7.2Applicationtoactualsamples2

7.3Typesandlifeofgraphitetube2

7.4Interferenceandbackgroundabsorptionandmeasuringcautions3

7.5Measuringconditionsbyelement5

1)Silver(Ag)6

2)Aluminum(Al)8

3)Arsenic(As)10

4)Gold(Au)12

5)Beryllium(Be)14

6)Bismuth(Bi)16

7)Calcium(Ca)18

8)Cadmium(Cd)20

9)Chromium(Cr)22

10)Cobalt(Co)24

11)Copper(Cu)26

12)Iron(Fe)28

13)Potassium(K)30

14)Lithium(Li)32

15)Magnesium(Mg)34

16)Manganese(Mn)36

17)Molybdenum(Mo)38

18)Sodium(Na)40

19)Nickel(Ni)42

20)Lead(Pb)44

21)Platinum(Pt)46

22)Rhodium(Rh)48

23)Antimony(Sb)50

24)Selenium(Se)52

25)Silicon(Si)54

26)Tin(Sn)I56

27)Tin(Sn)II58

28)Strontium(Sr)60

29)Titanium(Ti)62

30)Vanadium(V)64

31)Zinc(Zn)66

Measuringconditionsbyelementoffurnaceanalysismethod7.1Measuringconditions

Thesolutionpreparedonthebasisofthestandardsamplepreparationmethod(cookbooksection2-3)wasusedtomakethecalibrationcurveinthestandardconcentrationrange.AnalysisconditionsstoredinAA-6401or6501weremainlyused.HCL,BGC-D2,andBGC-SRmethodswereusedaccordingtotherespectiveelement.Therelationshipbetweentheashingtemperature,theatomizationtemperature,andsensitivityisalsoshown.However,theyareomittedforsomeelements.

Accordingtothedata,aStepheatingstagecomesaftertheRampheatingstage.BetterrepeatabilitycanbeexpectedbyinsertinganotherRampheatingstageuptotheAshingtemperaturebetweenthetwo.AcleaningstageissetaftertheAtomizationstageitneccessary.

Thehighdensitygraphitetubeorthepyrolyticgraphitetubewasuseddependingonthecharacteristicofeachelementanditsselectioniswrittenineachdata.

Astheatomizationcondition,therearetwomodes:thestandardmode(0.0)andthehighsensitivitymode(0.0H)areavailableandtwotypesofdataareshown.

Thestandardmodeandhighsensitivitymodeareusedasshownbelow.

Standardmode(0.0)

Theabsorbancesensitivityis1/3to1/2ofthatobtainedinthehighsensitivitymode,dependingon

theelement.

However,thismodeiseffectiveforthemeasurementofthesamplewhichissusceptibletoinfluencesfromco-existentsubstances.Backgroundabsorbanceisalsosmall.

Highsensitivitymode(0.0H)

Thehighestsensitivitycanbeobtainedinthismodebut,atthesametime,backgroundishigher.

Thisisparticularlyeffectiveforthemeasurementoftraceelementsincitywater,ultra-purewaterandothersampleswhichcontainsmallco-existentsubstances.

However,thestandardmodeisbetterformeasurementofthesamplewhicheasilycausesbackgroundabsorption.

Thisdataismeasuredattheinnergasflowof0l/minintheatomizationmode.Absorbancesensitivitycanbecontrolledbyflowingtheinnergas(0to1.5l/min)inthisstep.Whentheinnergasflowis1.5l/min,absorbancesensitivitydropstoabout1/5andthehighconcentrationcalibrationcurvecanbeprepared.

7.2Applicationtoactualsamples

Thetemperatureprogramofthisdataisdesignedforthestandardsolution.Goodresultsmaynotbeobtainedintheheatingconditiondescribedhere,becausematrixcomponents,concentration,andthetypeandconcentrationofco-existentsubstancesaredifferentintheactualsample.

Therefore,whenamatrixcomponentiscontainedortheconcentrationsofco-existentsubstancesarehigh,thesuitableconditionsfortheactualsampleshouldbesetbythemethodoftheanalysisconditioninthecookbooksection2-2-2FurnaceAnalysisMethod,onthebasisoftheheatingconditionofthisdata.

7.3Typesandlifeofgraphitetube

Thefollowingthreetypesofgraphitetubesaresupplied,anduseddependingontheelementtobemeasuredandtheinterferencelevel.

Highdensitygraphitetube

Thiscanbeusedforthemeasurementofmostelementsandcanobtainexcellentresultsin

repeatabilityoftheabsorptionsignal.However,withB,Ca,Moandothermetalswhicheasilyreactoncarbon,thetargetcomponentdoesnotvolatilizecompletelyduringatomizationandmemoryeffectoccurs.Withanorganicsolventtypesample,penetrationintothegraphitetubeincreasesandsensitivitymaydropsharplyormemoryeffectmayoccur.

Pyrolyticgraphitetube

Asurfacetreatmentisdoneonthehighdensitygraphitetubetomakeapyrolytictube.Because

samplepenetrationintothetubeissmall,excellentresultscanbeobtainedwithanorganicsolventtypesample.ThememoryeffecthardlyoccurswithB,Ca,Mo,etc.mentionedabove.

Itsabsorbancesensitivityistwotothreetimeshigherthanthatofthehighdensitygraphitetubewith

AlandSiand4b,5b,6b,7b,8groups(Ti,V,Cr,Mo,Fe,Co,Ni,Cu,etc.)andlanthanoidsintheperiodictableofelements.

Itsrepeatabilityoftheabsorptionsignalmaybeworsethanthatofthehighdensitygraphitetube.

Platformtypegraphitetube

Agraphiteplateof1mmthicknessandseveralmm2sizeissetinthegraphitetubetomaketheplatformtypegraphitetube.Becausethistubeheatsthesampleindirectlyandevenly,interferenceofco-existentsubstancesandbackgroundabsorptiondecrease.Thisiseffectivefortheanalysisofmetalsamplescontainingmatrixcomponentsandelementsandinbloodorseawater;particularlyforanalysisofCd,Pbandothermetalswhichhavelowboilingpoints.

Thegraphitetubecanbeuseduntilitisbroken,unlessasensitivityorrepeatabilitydropoccurs.Thislifevarieswidelydependingonliquidpropertiesofthesampletobemeasured.Itcanbeused2000timeswiththesamplewhichhardlycontainsanyacidorco-existentsubstances.

However,itsusemaybelimitedto300timeswiththesamplewhichhashighacidconcentrationoralotofco-existentsubstances.

Therefore,itisrecommendedtocountservicetimesofthegraphitetubeinmeasurementandcheckthetubelifeforthesampleinadvance.TheAA-6401or6501hastheprogramtocountservicetimesofthetube,sothiscanbeusedtoknowthetimewhenthetubeshouldbechanged.

7.4Interference,backgroundabsorption,andmeasuringcautions

Cautionsformeasuringeachelementandinterferenceareenumeratedbelow.

Somesamplesmaynotbemeasuredproperlysimplybydevisingtheheatingprogram.Insuchcase,goodresultsmaybeobtainedifthematrixmodifierisaddedinaccordancewiththecookbooksection2-5.3(Chemicalinterferenceanditscorrectionmethod).

Whenbackgroundabsorptioncorrectionisdone,asensitivitydropoccursintheBGC-SRmethod,ascomparedwithBGC-D2methodfortheprinciplereason.Iftheelementbeinganalyzedisatthe430nmorlongerwavelengthrange,theBGC-SRmethodshouldbeusedforbettercorrectionaccuracy.

Al

Argasisusedasthegas.WhenNgasexists,strongmonocyanideisproduced.

2

As

SensitivityslightlyincreasesbyusingN2ratherthanArasthesheathgas.Theashingtemperature

canbeincreasedbyaddingMg(NO)

2

orNi(NO).

3

32

Ca

Becausethegraphitetubeproducesacarbide,useofthepyrolytic

graphitetubeispreferable.

Attentionmustbegiventotheambientatmosphere,theregent,anddistilledwaterbeingusedfor

microchemicalanalysis.

Cd

Ashingtemperaturecanbeincreasedbyaddingabout1%(NH)

HPO.

42

4

Co

Interferenceoccursifahalogenideco-exists.

3

2

2)

Thesensitizationeffectcanbeexpectedbyadding0.5%Fe(NO).

Cr

Argasispreferableasthesheathgas.

Ifahalogenideco-exists,usethepyrolytic

graphitetube.Chromiumvolatilizesevenatlow

temperaturesettings.ItbecomesCrCl3undertheco-existenceofNaCl.

Cu

Fe

Ga

K

3)

Interferenceoccursifahalogenideco-exists.Itispreferabletodecomposeitbywetashing,oraddnitricacid,beforethedryingorashingconditionisset.

Itisrelativelyinsusceptibletointerferencesfromotherelements.However,attentionmustbegiventoFeimpuritiesinthegraphitetubeandambientatmosphereduringmicrochemicalanalysis.

ItisrecommendedtouseHNO3totreatastandardorunknownsample.ThedoublesensitizationeffectcanbeexpectedwiththemixedsolutionofHNO3+H2O2.1)

Attentionmustbegiventodistilledwaterandtheambientatmosphereduringmicrochemicalanalysis.

Itisdesirabletonarrowtheslitwidthformeasurement,becauseemissionfromthegraphitetubeisstronginthiswavelengthrange.

Mg

Mn

Mo

Na

Ni

Pb

Se

Si

Sn

Ti

V

Zn

Argasispreferableasthesheathgas.Attentionmustbegiventodistilledwaterandimpuritiesinthereagent.

Itissusceptibletointerferenceifahologenideco-exist.Itisexpectedthattheashingtemperature

o

canbeincreasedfrom1100to1150CbyaddingHNO3.

Carbideisproducedbycarbonfromthegraphitetubeorthesample,andsensitivitydrops.

Therefore,usingthepyrolyticgraphitetubeisrecommended.

Attentionmustbegiventotheambientatmosphere,anddistilledwaterduringmicrochemicalanalysis.

o

Volatizationissmallevenifashingtemperatureissetfrom900to1000C.

o

Volatizationincreaseswhenashingtemperatureissetfrom600to650Corhigher.

o

Itisdesiredthattheashingtemperatureis300Corlower.Itisexpectedthattheashingtemperature

o

isincreasedfrom1000to1100CbyaddingCu,NiandMo.

TheuseofN2gasispreferabletoArasthesheathgas.

Usingthepyrolyticgraphitetubeisrecommended.

Arispreferableasthesheathgas,andhighersensitivitycanbeobtainedwithasmallerflow.

o

Sensitivityislowandtheatomizationtemperatureis2700to3000C.Thepyrolyticgraphitetubeisused.

o

Volatizationissmalleveniftheashingtemperatureissetat700C.Theuseofthepyrolyticgraphitetubeispreferable.

Attentionmustbegiventotheatmosphereanddistilledwaterduringmicrochemicalanalysis.ThesensitizationeffectcanbeobtainedbyaddingAl(NO3)2.4)

Reference

R.D.Ediger,At.Absorpt.Newsl.,14,127-130(1975)

AAnalysiswiththeGraphiteFurnaceUsingMatrixModification”.

R.B.CruzandJ.C.VanLoon,Anal.Chim.Acta,72,231-243(1974)

.CriticalstudyofGraphiteFurnaceNon-FlamlAAStotheDeterminationofTraceBaseMetalsin

ComplexHeavyMatrixSampleSolutions”.

W.J.Price,SpectrochemicalAnalysisbyAtomicAbsorption,HEYDEN.

F.J.M.Maesen,J.BalkeandR.Massee,Spectrochim.Acta,33B,311-324(1978)

on-SpectralInterferencesinFlamelessAASUsingGraphiteMiniTube-Furnaces”.

7.5Measuringconditionsbyelement

Silver(Ag)

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection3-3forthestandardsolutionpreparationmethod

Measuringconditionsandcalibrationcurve

Lightingconditions

Current

;10mA/0mA

;10mA/400mA

Wavelength

;328.1nm

;328.1nm

Slitwidth

;

0.5nm

;

0.5nm

Lightingmode

;

BGC-D2

;

BGC-SR

Graphitefurnacetemperatureprogram(Highsensitivitymode0.0H),Highdensitygraphitetube

STAGE#

TEMP.(oC)

TIME(sec)

GAS

(l/min)

HEAT

SAMPLING

PreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

400

10

#1

1.0

STEP

OFF

4

400

3

#1

0.0H

STEP

OFF

5

1500

3

#1

0.0H

STEP

ON

2

CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)328.1nm

10.00000.0039

22.00000.2014

36.00000.5895

410.00000.9301

[ABS]=K2*[C]2+K1*[C]+K0r2=0.9999

K0=0.0016,K1=0.1043,K2=–0.0011

CalibrationcurveinBGC-SRmode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)328.1nm

10.00000.0057

22.00000.0868

36.00000.2843

410.00000.4801

Silver(Ag)

[ABS]=K1*[C]+K0r2=0.9991

K0=0.0012,K1=0.0479

Graphitefurnacetemperatureprogram(Standardmode0.0),Highdensitygraphitetube

STAGE#

TEMP.(oC)

TIME(sec)

GAS

(l/min)

HEAT

SAMPLING

PreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

400

10

#1

1.0

STEP

OFF

4

400

3

#1

0.0

STEP

OFF

5

1500

3

#1

0.0

STEP

ON

2

CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)328.1nm

10.00000.0033

22.00000.1217

36.00000.3734

410.00000.6077

[ABS]=K2*[C]2+K1*[C]+K0r2=0.9999

K0=0.0010,K1=0.0629,K2=–0.0002

CalibrationcurveinBGC-SRmode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)328.1nm

10.00000.0062

22.00000.0572

36.00000.1828

410.00000.3060

[ABS]=K1*[C]+K0r2=0.9991

K0=0.0018,K1=0.0303

Ashingtemperature,atomizationtemperatureandsensitivity(Solution:HNO3,AgNO3)

AshingconditionAtomizationcondition

Aluminum(Al)

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection3-3forthestandardsolutionpreparationmethod

Measuringconditionsandcalibrationcurve

Lightingconditions

Current

;8mA/0mA

;10mA/600mA

Wavelength

;309.3nm

;309.3nm

Slitwidth

;

0.5nm

;

0.5nm

Lightingmode

;

BGC-D2

;

BGC-SR

Graphitefurnacetemperatureprogram(Highsensitivitymode0.0H),Pyrolyticgraphitetube

STAGE#

TEMP.(oC)

TIME(sec)

GAS

(l/min)

HEAT

SAMPLING

PreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

700

10

#1

1.0

STEP

OFF

4

700

3

#1

0.0H

STEP

OFF

5

2400

3

#1

0.0H

STEP

ON

2

CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)309.3nm

10.00000.0035

24.00000.0896

312.00000.2846

420.00000.4353

[ABS]=K2*[C]2+K1*[C]+K0r2=0.9989

K0=0.0010,K1=0.0255,K2=–0.0002

CalibrationcurveinBGC-SRmode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)309.3nm

10.00000.0028

24.00000.0381

312.00000.1298

420.00000.1950

[ABS]=K1*[C]+K0r2=0.9949

K0=0.0030,K1=0.0098

Graphitefurnacetemperatureprogram(Standardmode0.0),pyrolyticgraphitetube

STAGE#TEMP.(oC)TIME(sec)GAS(l/min)HEATSAMPLINGPreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

700

10

#1

1.0

STEP

OFF

4

700

3

#1

0.0

STEP

OFF

5

2400

3

#1

0.0

STEP

ON

2

?CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.

CONC.

ABS.

No.

(ppb)

309.3nm

1

0.0000

0.0035

2

4.0000

0.0497

3

12.0000

0.1653

4

20.0000

0.2914

[ABS]=K1*[C]+K0r2=0.9975

K0=–0.0030,K1=0.0145

CalibrationcurveinBGC-SRmode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)309.3nm

10.00000.0037

24.00000.0219

312.00000.0802

420.00000.1399

[ABS]=K1*[C]+K0r2=0.9953

K0=0.0010,K1=0.0069

Ashingtemperature,atomizationtemperatureandsensitivity(Solution:HClMetal)

AshingconditionAtomizationcondition

Arsenic(As)

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection3-3forthestandardsolutionpreparationmethod

Measuringconditionsandcalibrationcurve

Measuringconditions

Current

;12mA/0mA

;12mA/500mA

Wavelength

;193.7nm

;193.7nm

Slitwidth

;

0.5nm

;

2.0nm

Lightingmode

;

BGC-D2

;

BGC-SR

Graphitefurnacetemperatureprogram(Highsensitivitymode0.0H),highdensitygraphitetube,Pd10

ppmadded

STAGE#

TEMP.(oC)

TIME(sec)

GAS

(l/min)

HEAT

SAMPLING

PreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

600

10

#1

1.0

STEP

OFF

4

600

3

#1

0.0H

STEP

OFF

5

2200

3

#1

0.0H

STEP

ON

2

CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)193.7nm

10.00000.0113

24.00000.0996

312.00000.2456

420.00000.3922

[ABS]=K1*[C]+K0r2=0.9989

K0=0.0174,K1=0.0189

CalibrationcurveinBGC-SRmode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)193.7nm

10.00000.0085

24.00000.0366

312.00000.0838

420.00000.1219

[ABS]=K1*[C]+K0r2=0.9945

K0=0.0119,K1=0.0056

?

Graphitefurnacetemperatureprogram(Standardmode0.0),Highdensitygraphitetube,Pd10ppmadded

STAGE#

TEMP.(oC)

TIME(sec)

GAS

(l/min)

HEAT

SAMPLING

PreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

600

10

#1

1.0

STEP

OFF

4

600

3

#1

0.0

STEP

OFF

5

2200

3

#1

0.0

STEP

ON

2

CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)93.7nm

10.00000.0158

24.00000.0569

312.00000.1534

420.00000.2412

[ABS]=K1*[C]+K0r2=0.9994

K0=0.0114,K1=0.0114

CalibrationcurveinBGC-SRmode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)193.7nm

10.00000.0120

24.00000.0243

312.00000.0476

420.00000.0750

[ABS]=K1*[C]+K0r2=0.9987

K0=0.0116,K1=0.0031

Ashingtemperature,atomizationtemperatureandsensitivity(Solution:NaOH,As2O3)

AshingconditionAtomizationcondition

Gold(Au)

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection3-3forthestandardsolutionpreparationmethod

Measuringconditionsandcalibrationcurve

Lightingconditions

Current

;12mA/0mA

;10mA/400mA

Wavelength

;242.8nm

;242.8nm

Slitwidth

;

0.5nm

;

0.5nm

Lightingmode

;

BGC-D2

;

BGC-SR

Graphitefurnacetemperatureprogram(Highsensitivitymode0.0H),Highdensitygraphitetube

STAGE#

TEMP.(oC)

TIME(sec)

GAS

(l/min)

HEAT

SAMPLING

PreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

500

10

#1

1.0

STEP

OFF

4

500

3

#1

0.0H

STEP

OFF

5

1700

3

#1

0.0H

STEP

ON

2

CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)242.8nm

10.00000.0023

210.00000.1088

330.00000.3908

450.00000.6341

[ABS]=K2*[C]2+K1*[C]+K0r2=0.9984

K0=–0.0056,K1=0.0129,K2=–0.0000

CalibrationcurveinBGC-SRmode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)242.8nm

10.00000.0061

210.00000.0796

330.00000.2228

450.00000.3609

[ABS]=K2*[C]2+K1*[C]+KOr2=1.0000

K0=0.0061,K1=0.0074,K2=–0.0000

Graphitefurnacetemperatureprogram(Standardmode0.0),Highdensitygraphitetube

STAGE#TEMP.(oC)TIME(sec)GAS(l/min)HEATSAMPLINGPreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

500

10

#1

1.0

STEP

OFF

4

500

3

#1

0.0

STEP

OFF

5

1700

3

#1

0.0

STEP

ON

2

?CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.

CONC.

ABS.

No.

(ppb)

242.8nm

1

0.0000

0.0029

2

10.0000

0.0922

3

30.0000

0.2784

4

50.0000

0.4494

[ABS]=K2*[C]2+K1*[C]+K0r2=0.9999

K0=0.0013,K1=0.0095,K2=–0.0000

CalibrationcurveinBGC-SRmode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)242.8nm

10.00000.0073

210.00000.0600

330.00000.1820

450.00000.2959

[ABS]=K2*[C]2+K1*[C]+K0r2=0.9996

K0=0.0055,K1=0.0058,K2=0.000

Ashingtemperature,atomizationtemperatureandsensitivity(Solution:AquaRegia,Metal)

AshingconditionAtomizationcondition

Beryllium(Be)

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection3-3forthestandardsolutionpreparationmethod

Measuringconditionsandcalibrationcurve

Lightingconditions

Current

;16mA/0mA

Wavelength

;234.9nm

Slitwidth

;

0.5nm

Lightingmode

;

BGC-D2

Graphitefurnacetemperatureprogram(Highsensitivitymode0.0H),Pyrolyticgraphitetube

STAGE#

TEMP.(oC)

TIME(sec)

GAS

(l/min)

HEAT

SAMPLING

PreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

600

10

#1

1.0

STEP

OFF

4

600

3

#1

0.0H

STEP

OFF

5

2600

3

#1

0.0H

STEP

ON

2

?CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.

CONC.

ABS.

No.

(ppb)

234.9nm

1

0.0000

0.0041

2

0.2000

0.1367

3

0.6000

0.4307

4

1.0000

0.7463

[ABS]=K1*[C]+K0r2=0.9991

K0=0.0054,K1=0.7441

Beryllium(Be)

Graphitefurnacetemperatureprogram(Standardmode0.0),Pyrolyticgraphitetube

STAGE#

TEMP.(oC)

TIME(sec)

GAS

(l/min)

HEAT

SAMPLING

PreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

600

10

#1

1.0

STEP

OFF

4

600

3

#1

0.0H

STEP

OFF

5

2600

3

#1

0.0H

STEP

ON

2

CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)234.9nm

10.00000.0041

20.20000.0412

30.60000.1389

41.00000.2434

[ABS]=K1*[C]+K0r2=0.9973

K0=0.0019K1=0.2416

Bismuth(Bi)

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection3-3forthestandardsolutionpreparationmethod

Measuringconditionsandcalibrationcurve

Lightingconditions

Current

;10mA/0mA

;10mA/300mA

Wavelength

;223.1nm

;223.1nm

Slitwidth

;

0.5nm

;

0.5nm

Lightingmode

;

BGC-D2

;

BGC-SR

Graphitefurnacetemperatureprogram(Highsensitivitymode0.0H),Highdensitygraphitetube

STAGE#

TEMP.(oC)

TIME(sec)

GAS

(l/min)

HEAT

SAMPLING

PreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

450

10

#1

1.0

STEP

OFF

4

450

3

#1

0.0H

STEP

OFF

5

1700

3

#1

0.0H

STEP

ON

2

CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)223.1nm

10.00000.0069

210.00000.1326

330.00000.4847

450.00000.7950

[ABS]=K1*[C]+K0r2=0.9981

K0=–0.0065,K1=0.0161

CalibrationcurveinBGC-SRmode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)223.1nm

10.00000.0072

210.00000.0624

330.00000.2143

450.00000.3764

[ABS]=K1*[C]+K0r2=0.9967

K0=0.0030,K1=0.0075

Graphitefurnacetemperatureprogram(Standardmode0.0),Highdensitygraphitetube

STAGE#TEMP.(oC)TIME(sec)GAS(l/min)HEATSAMPLINGPreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

450

10

#1

1.0

STEP

OFF

4

450

3

#1

0.0

STEP

OFF

5

1700

3

#1

0.0

STEP

ON

2

CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)223.1nm

10.00000.0080

210.00000.0358

330.00000.1334

450.00000.2464

[ABS]=K1*[C]+K0r2=0.9901

K0=–0.0032,K1=0.0048

CalibrationcurveinBGC-SRmode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)223.1nm

10.00000.0071

210.00000.0205

330.00000.0637

450.00000.1107

[ABS]=K1*[C]+K0r2=0.9938

K0=0.0031,K1=0.0021

Ashingtemperature,atomizationtemperatureandsensitivity(Solution:HNO3,Metal)

AshingconditionAtomizationcondition

Calcium(Ca)

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection3-3forthestandardsolutionpreparationmethod

Measuringconditionsandcalibrationcurve

Lightingconditions

Current

;10mA/0mA

Wavelength

;422.7nm

Slitwidth

;

0.5nm

Lightingmode

;

BGC-D2

Graphitefurnacetemperatureprogram(Highsensitivitymode0.0H),Pyrolyticgraphitetube

STAGE#

TEMP.(oC)

TIME(sec)

GAS

(l/min)

HEAT

SAMPLING

PreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

700

10

#1

1.0

STEP

OFF

4

700

3

#1

0.0H

STEP

OFF

5

2500

3

#1

0.0H

STEP

ON

2

CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)422.7nm

10.00000.0438

20.40000.2778

31.20000.6807

42.00001.0625

[ABS]=K2*[C]2+K1*[C]+K0r2=0.9998

K0=0.0477,K1=0.5690,K2=–0.0312

Calcium(Ca)

Graphitefurnacetemperatureprogram(Standardmode0.0),Pyrolyticgraphitetube

STAGE#

TEMP.(oC)

TIME(sec)

GAS

(l/min)

HEAT

SAMPLING

PreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

700

10

#1

1.0

STEP

OFF

4

700

3

#1

0.0

STEP

OFF

5

2500

3

#1

0.0

STEP

ON

2

CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)422.7nm

10.00000.0302

20.40000.2305

31.20000.5795

42.00000.9083

[ABS]=K2*[C]2+K1*[C]+K0r2=0.9999

K0=0.0331,K1=0.4904,K2=–0.0267

Ashingtemperature,atomizationtemperatureandsensitivity(Solution:HCl,CaCO3)

AshingconditionAtomizationcondition

Cadmium(Cd)

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection3-3forthestandardsolutionpreparationmethod

Measuringconditionsandcalibrationcurve

Lightingconditions

Current

;8mA/0mA

;8mA/300mA

Wavelength

;228.8nm

;228.8nm

Slitwidth

;

0.5nm

;

0.5nm

Lightingmode

;

BGC-D2

;

BGC-SR

Graphitefurnacetemperatureprogram(Highsensitivitymode0.0H),Highdensitygraphitetube

STAGE#

TEMP.(oC)

TIME(sec)

GAS

(l/min)

HEAT

SAMPLING

PreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

300

10

#1

1.0

STEP

OFF

4

300

3

#1

0.0H

STEP

OFF

5

1500

3

#1

0.0H

STEP

ON

2

?CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.

CONC.

ABS.

No.

(ppb)

228.8nm

1

0.0000

0.0129

2

0.1000

0.0751

3

0.3000

0.1971

4

0.5000

0.3340

[ABS]=K1*[C]+K0r2=0.9992

K0=–0.0109,K1=0.6395

CalibrationcurveinBGC-SRmode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)228.8nm

10.00000.0047

20.10000.0363

30.30000.1005

40.50000.1577

[ABS]=K1*[C]+K0r2=0.9993

K0=0.0057,K1=0.3072

Cadmium(Cd)

Graphitefurnacetemperatureprogram(Standardmode0.0),Highdensitygraphitetube

STAGE#

TEMP.(oC)

TIME(sec)

GAS

(l/min)

HEAT

SAMPLING

PreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

300

10

#1

1.0

STEP

OFF

4

300

3

#1

0.0

STEP

OFF

5

1500

3

#1

0.0

STEP

ON

2

CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)228.8nm

10.00000.0138

20.10000.0453

30.30000.1224

40.50000.1894

[ABS]=K1*[C]+K0r2=0.9989

K0=–0.0127,K1=0.3558

CalibrationcurveinBGC-SRmode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)228.8nm

10.00000.0060

20.10000.0211

30.30000.0568

40.50000.0951

[ABS]=K1*[C]+K0r2=0.9985

K0=0.0045,K1=0.1791

Ashingtemperature,atomizationtemperatureandsensitivity(Solution:HNO3,Metal)

AshingconditionAtomizationcondition

Chromium(Cr)

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection3-3forthestandardsolutionpreparationmethod

Measuringconditionsandcalibrationcurve

Lightingconditions

Current

;10mA/0mA

;10mA/600mA

Wavelength

;357.9nm

;357.9nm

Slitwidth

;

0.5nm

;

0.5nm

Lightingmode

;

BGC-D2

;

BGC-SR

Graphitefurnacetemperatureprogram(Highsensitivitymode0.0H),Pyrolyticgraphitetube

STAGE#

TEMP.(oC)

TIME(sec)

GAS

(l/min)

HEAT

SAMPLING

PreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

700

10

#1

1.0

STEP

OFF

4

700

3

#1

0.0H

STEP

OFF

5

2500

3

#1

0.0H

STEP

ON

2

CalibrationcurveinBGC-D2mode(Sampleinjectionvolume10l)

STD.CONC.ABS.

No.(ppb)357.9nm

10.00000.0108

21.00000.0807

33.00000.2158

45.00000.3478

[ABS]=K1*[C]+K0r2=0.9999

K0=0.0123,K1=0.0673

CalibrationcurveinBGC-SRmode(Sampleinjectionvolume10l)

STD.CONC.ABS.

No.(ppb)357.9nm

10.00000.0043

21.00000.0444

33.00000.1268

45.00000.2121

[ABS]=K1*[C]+K0r2=0.9999

K0=0.0034,K1=0.0416

Graphitefurnacetemperatureprogram(Standardmode0.0),Pyrolyticgraphitetube

STAGE#TEMP.(oC)TIME(sec)GAS(l/min)HEATSAMPLINGPreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

700

10

#1

1.0

STEP

OFF

4

700

3

#1

0.0

STEP

OFF

5

2500

3

#1

0.0

STEP

ON

2

CalibrationcurveinBGC-D2mode(Sampleinjectionvolume10l)

STD.CONC.ABS.

No.(ppb)357.9nm

10.00000.0124

21.00000.0389

33.00000.1078

45.00000.1661

[ABS]=K1*[C]+K0r2=0.9983

K0=–0.0110,K1=0.0313

CalibrationcurveinBGC-SRmode(Sampleinjectionvolume10l)

STD.CONC.ABS.

No.(ppb)357.9nm

10.00000.0031

21.00000.0236

33.00000.0617

45.00000.1042

[ABS]=K1*[C]+K0r2=0.9994

K0=0.0029,K1=0.0201

Ashingtemperature,atomizationtemperatureandsensitivity(Solution:HCl,Metal)

AshingconditionAtomizationcondition

Cobalt(Co)

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection3-3forthestandardsolutionpreparationmethod

Measuringconditionsandcalibrationcurve

Lightingconditions

Current

;12mA/0mA

;12mA/400mA

Wavelength

;240.7nm

;240.7nm

Slitwidth

;

0.2nm

;

0.2nm

Lightingmode

;

BGC-D2

;

BGC-SR

Graphitefurnacetemperatureprogram(Highsensitivitymode0.0H),Pyrolyticgraphitetube

STAGE#

TEMP.(oC)

TIME(sec)

GAS

(l/min)

HEAT

SAMPLING

PreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

400

10

#1

1.0

STEP

OFF

4

400

3

#1

0.0H

STEP

OFF

5

2500

3

#1

0.0H

STEP

ON

2

CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)240.7nm

10.00000.0169

24.00000.1578

312.00000.4332

420.00000.6482

[ABS]=K2*[C]2+K1*[C]+K0r2=0.9997

K0=0.0138,K1=0.0389,K2=–0.0004

CalibrationcurveinBGC-SRmode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)240.7nm

10.00000.0178

24.00000.1058

312.00000.2953

420.00000.4600

[ABS]=K2*[C]2+K1*[C]+K0r2=0.9997

K0=0.0152,K1=0.0243,K2=–0.0000

Cobalt(Co)

Graphitefurnacetemperatureprogram(Standardmode0.0),Pyrolyticgraphitetube

STAGE#

TEMP.(oC)

TIME(sec)

GAS

(l/min)

HEAT

SAMPLING

PreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

400

10

#1

1.0

STEP

OFF

4

400

3

#1

0.0

STEP

OFF

5

2500

3

#1

0.0

STEP

ON

2

CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)240.7nm

10.00000.0319

24.00000.1063

312.00000.2988

420.00000.4591

[ABS]=K2*[C]2+K1*[C]+K0r2=0.9983

K0=0.0265,K1=0.0227,K2=–0.0000

CalibrationcurveinBGC-SRmode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)240.7nm

10.00000.0154

24.00000.0715

312.00000.2148

420.00000.3384

[ABS]=K2*[C]2+K1*[C]+K0r2=0.9987

K0=0.0117,K1=0.0167,K2=–0.0000

Ashingtemperature,atomizationtemperatureandsensitivity(Solution:HCl,CoCl)

AshingconditionAtomizationcondition

Copper(Cu)

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection3-3forthestandardsolutionpreparationmethod

Measuringconditionsandcalibrationcurve

Lightingconditions

Current

;6mA/0mA

;10mA/500mA

Wavelength

;324.8nm

;324.8nm

Slitwidth

;

0.5nm

;

0.5nm

Lightingmode

;

BGC-D2

;

BGC-SR

Graphitefurnacetemperatureprogram(Highsensitivitymode0.0H),Pyrolyticgraphitetube

STAGE#

TEMP.(oC)

TIME(sec)

GAS

(l/min)

HEAT

SAMPLING

PreTIME

1

120

20

#1

1.0

RAMP

OFF

2

250

10

#1

1.0

RAMP

OFF

3

500

10

#1

1.0

STEP

OFF

4

500

3

#1

0.0H

STEP

OFF

5

2300

3

#1

0.0H

STEP

ON

2

CalibrationcurveinBGC-D2mode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)324.8nm

10.00000.0041

21.00000.1062

33.00000.3052

45.00000.4881

[ABS]=K1*[C]+K0r2=0.9994

K0=0.0079,K1=0.0969

CalibrationcurveinBGC-SRmode(Sampleinjectionvolume20l)

STD.CONC.ABS.

No.(ppb)324.8nm

10.00000.0025

21.00000.0564

33.00000.1937

45.00000.3153

[ABS]=K1*[C]+K0r2=0.9988

K0=–0.0008,K1=0.0635

Graphitefurnacetemperatureprogram(Standardmode0.0),Pyrolyticgraphitetube

STAGE#TEMP.(oC)TIME(sec)GAS(l/min)HEATSAMPLINGPreTIME

1

120