03 Measuring Conditions by Element Flame AA岛津原子吸收光谱应用手册火焰分析篇.docx

03 Measuring Conditions by Element Flame AA岛津原子吸收光谱应用手册火焰分析篇.docx

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03MeasuringConditionsbyElementFlameAA岛津原子吸收光谱应用手册火焰分析篇

ATOMICABSORPTIONSPECTROPHOTOMETRYCOOKBOOK

Section3

MeasuringConditionsbyElementofFlameAtomic

AbsorptionSpectrophotometry

AtomicAbsorptionSpectrophotometryCookbook

Section3

CONTENTS

6.MeasuringConditionsbyElementof

FlameAtomicAbsorptionSpectrophotometry1

6.1Measuringconcentration1

6.2Measuringconditions1

6.3Backgroundcorrectionmethodandinterference1

6.4Measuringconditionsbyelement1

1）Silver（Ag）2

2）Aluminum（Al）3

3）Arsenic（As）4

4）Gold（Au）5

5）Boron（B）6

6）Barium（Ba）7

7）Beryllium（Be）8

8）Bismuth（Bi）9

9）Calcium（Ca）I10

10）Calcium（Ca）II11

11）Cadmium（Cd）12

12）Cobalt（Co）13

13）Chromium（Cr）14

14）Cesium（Cs）15

15）Copper（Cu）16

16）Iron（Fe）17

17）Gallium（Ga）18

18）Germanium（Ge）19

19）Potassium（K）20

20）Lithium（Li）21

21）Magnesium（Mg）22

22）Manganese（Mn）23

23）Molybdenum（Mo）24

24）Sodium（Na）25

25）Nickel（Ni）26

26）Lead（Pb）I27

27）Lead（Pb）II28

28）Palladium（Pd）29

29）Platinum（Pt）30

30）Rubidium（Rb）31

31）Rhodium（Rh）32

32）Antimony（Sb）33

33）Selenium（Se）34

34）Silicon（Si）35

35）Tin（Sn）I36

36）Tin（Sn）II37

37）Tin（Sn）III38

38）Tin（Sn）IV39

39）Strontium（Sr）40

40）Tellurium（Te）41

41）Titanium（Ti）42

42）Thallium（Tl）43

43）Vanadium（V）44

44）Zinc（Zn）45

6.MeasuringConditionsbyElementof

FlameAtomicAbsorptionSpectrophotometry

6.1Measuringconcentration

Thesolutionpreparedonthebasisofthestandardsamplepreparationmethodinthecookbooksection2-3isusedtomakethecalibrationcurveinthestandardconcentrationrange.Becauseabsorbanceis0.044to0.3inthecookbooksection2-4,theupperandlowerlimitsofthecalibrationlineareobtainedfromtheabovedatatodeterminethepracticalmeasuringconcentrationrange.

Themeasuringconcentrationrangeofanactualsamplemaydifferfromthedata,duetoaco-existentmatter.Sensitivityofanorganicsolventtypesampleisraisedbytwoorthreetimes.

Tomakeameasurementofhigherconcentrations,theburnermustbetilted（CookbookSection2-4.3）oranotheranalysislinemustbeused.（CookbookSection1-2.1）.

6.2Measuringconditions

IntheAA-6400ortheAA-6500,theanalysisconditionsstoredcanbeused.Becausethereisaslightdifferencebetweeninstruments,itmaybebettertochangethemixingratioofoxidantandfuelgasinaccordancewiththecookbook（section1-2.2）.Thisallowsdataofhighsensitivityandgoodrepeatabilitytobeobtained.

However,theseconditionsareforawatersolutionsample.

Therefore,oxidantflow,fuelgasflow,burnerheightandotherconditionsmustbechangedwhenanorganicsolventtypesampleismeasured.Refertotheoperatinginstructionsoftheatomicabsorptionspectrophotometerforselectionoftheoptimumconditions.

Inthecasesofcalcium,lead,andtinasthetargetelements,twoormoreflameconditionsandanalysiswavelengthsareindicatedbyaI,II,III,orIV.

6.3Backgroundcorrectionmethodandinterference

Concerningelementsforwhichtheself-reversalhollowcathodelampisavailable,backgroundcorrectionisdonebytheD2lampmethodandtheself-reversalmethod.TheirresultsareshownrespectivelyasBGD-D2modeandBGC-SRmode.IncaseofBGC-SR,sensitivitydropoccursduetoitsprinciplereason.TheBGC-D2isrecommendedasarulewhenbackgroundcorrectionisdone.

But,inthecaseofasamplewhichhasthebackgroundabsorptionabove0.5Absorhasanyspectralinterface,orinthecaseitsanalysislineisinalongerwavelengthrangeforwhichtheD2lampcannotbeused,BGC-SRmodeisdesirable.

Datainthissectionshowsinformationoninterference.

Inmeasuringanactualsample,confirmationofinterferenceisnecessary.Refertothecookbooksection2-5forinterferenceintheatomicabsorptionmethod.

6.4Measuringconditionsbyelement

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection2-3fortheStandardsolutionpreparationmethod

MeasuringconditionsandCalibrationcurve

Measuringconditions

Current;10mA/0mA;10mA/400mABurnerheight;7mm

Wavelength;328.1nm;328.1nmBurnerangle;0deg

Slitwidth;0.5nm;0.5nmFuelgasflow;2.2l/min

Lightingmode;BGC-D2;BGC-SRTypeofoxidant;air

CalibrationcurveinBGCD2mode

STD.CONC.ABS.

No.（ppm）328.1nm

10.50000.0967

21.00000.1892

32.00000.3716

43.00000.5470

54.00000.7179

[ABS]=K2*[C]2+K1*[C]+K0

K0=0.0000,K1=0.1923,K2=0.0032

CalibrationcurveinBGC-SRmode

STD.CONC.ABS.

No.（ppm）328.1nm

10.50000.0645

21.00000.1297

32.00000.2596

43.00000.3903

54.00000.5215

[ABS]=K2*[C]2+K1*[C]+K0

K0=0.0000,K1=0.1293,K2=0.0003

Interference

Chemicalinterferencehardlyexists.

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection2-3fortheStandardsolutionpreparationmethod

MeasuringconditionsandCalibrationcurve

Measuringconditions

Current;10mA/0mA;10mA/600mABurnerheight;17mm

Wavelength;309.3nm;309.3nmBurnerangle;0deg

Slitwidth;0.5nm;0.5nmFuelgasflow;7.0l/min

Lightingmode;BGC-D2;BGC-SRTypeofoxidant;N2O

CalibrationcurveinBGCD2mode

STD.CONC.ABS.

No.（ppm）309.3nm

15.00000.0585

210.00000.1183

320.00000.2243

[ABS]=K1*[C]+K0

K0=0.0000,K1=0.0114

CalibrationcurveinBGC-SRmode

STD.CONC.ABS.

No.（ppm）309.3nm

15.00000.0330

210.00000.0638

320.00000.1288

[ABS]=K1*[C]+K0

K0=0.0000,K1=0.0064

Interference

Alisionized10to15%byN2O-C2H2flame.0.1%lanthanumchlorideorpotassiumisaddedtothestandardorunknownsampleasionizationrestrainer.

About10%positiveinterferenceisgivenifTiandFecoexistswithAlin10to50-foldconcentration.

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection2-3fortheStandardsolutionpreparationmethod

MeasuringconditionsandCalibrationcurve

Measuringconditions

Current;14mA/0mA;14mA/500mABurnerheight;15mm

Wavelength;193.7nm;193.7nmBurnerangle;0deg

Slitwidth;0.2nm;0.2nmFuelgasflow;3.7l/min

Lightingmode;BGC-D2;BGC-SRTypeofoxidant;air

CalibrationcurveinBGCD2mode

STD.CONC.ABS.

No.（ppm）193.7nm

10.00000.0042

210.00000.1965

330.00000.4890

450.00000.7096

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

K0=0.0002,K1=0.0200,K2=0.0001

CalibrationcurveinBGC-SRmode

STD.CONC.ABS.

No.（ppm）193.7nm

10.00000.0007

210.00000.1163

330.00000.2878

450.00000.4280

[ABS]=K2*[C]2+K1*[C]+K0r2=0.9995

K0=0.0036,K1=0.0113,K2=0.0000

Interference

ThegreatestinterferenceisdiffusionandabsorptionbyAir-C2H2flame.

ThemeasuringmethodsendingarsinegasdirectlytoAr-H2flameorheatedquartzshellisrecommendedforsensitivityandinterference.

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection2-3fortheStandardsolutionpreparationmethod

MeasuringconditionsandCalibrationcurve

Measuringconditions

Current;12mA/0mA;10mA/400mABurnerheight;7mm

Wavelength;242.8nm;242.8nmBurnerangle;0deg

Slitwidth;0.5nm;0.5nmFuelgasflow;1.8l/min

Lightingmode;BGC-D2;BGC-SRTypeofoxidant;air

CalibrationcurveinBGCD2mode

STD.CONC.ABS.

No.（ppm）242.8nm

10.00000.0000

24.00000.1683

312.00000.4794

420.00000.7673

[ABS]=K2*[C]2+K1*[C]+K0r2=1.0000

K0=0.0000,K1=0.0424,K2=0.0002

CalibrationcurveinBGC-SRmode

STD.CONC.ABS.

No.（ppm）242.8nm

10.00000.0009

24.00000.1124

312.00000.3362

420.00000.5392

[ABS]=K2*[C]2+K1*[C]+K0r2=1.0000

K0=0.0019,K1=0.0296,K2=0.0001

Interference

IfFe,CuandCacoexistinlargequantities,negativeinterferenceisgiven.However,chemicalinterferenceisgenerallysmall.

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection2-3fortheStandardsolutionpreparationmethod

MeasuringconditionsandCalibrationcurve

Measuringconditions

Current;16mA/0mABurnerheight;17mm

Wavelength;249.7nmBurnerangle;0deg

Slitwidth;0.2nmFuelgasflow;7.7l/min

Lightingmode;BGC-D2Typeofoxidant;N2O

CalibrationcurveinBGCD2mode

STD.CONC.ABS.

No.（ppm）249.7nm

10.00000.0025

2200.00000.1254

3600.00000.3494

41000.00000.5219

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

K0=0.0012,K1=0.0007,K2=0.0000

Interference

IfNacoexistsinlargequantities,positiveinterferenceisgiven.InterferencecanbedecreasedbychangingtheC2H2quantityoftheN2O-C2H2flameorburnerheight;butsensitivityalsodrops.

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection2-3fortheStandardsolutionpreparationmethod

MeasuringconditionsandCalibrationcurve

Measuringconditions

Current;16mA/0mABurnerheight;17mm

Wavelength;553.6nmBurnerangle;0deg

Slitwidth;0.2nmFuelgasflow;6.7l/min

Lightingmode;HCLTypeofoxidant;N2O

CalibrationcurveinHCLmode

STD.CONC.ABS.

No.（ppm）553.6nm

12.00000.0568

24.00000.1035

38.00000.2171

[ABS]=K1*[C]+K0

K0=0.0000,K1=0.0270

Interference

Standardsubstanceandstandardsolutionpreparationmethod

RefertoSection2-3fortheStandardsolutionpreparationmethod

MeasuringconditionsandCalibrationcurve

Measuringconditions

Current;16mA/0mABurnerheight;17mm

Wavelength;234.9nmBurnerangle;