X-Ray Emission Spectroscopy - FHI · X-Ray Emission Spectroscopy Axel Knop-Gericke [email protected]
Emission Spectroscopy
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Transcript of Emission Spectroscopy
![Page 1: Emission Spectroscopy](https://reader033.fdocuments.us/reader033/viewer/2022061111/545463efb1af9fb5468b47f9/html5/thumbnails/1.jpg)
Emission Spectroscopy Based upon Plasma, Arc, and Spark Atomization ArcArc Higher TemperatureHigher Temperature Lower interelement Lower interelement
interferenceinterference Single set of excitation Single set of excitation
conditions can excite conditions can excite multiple elementsmultiple elements
Permit low detection limits Permit low detection limits for refractory complexesfor refractory complexes
Larger linear rangeLarger linear range Can directly measure hard to Can directly measure hard to
measure samplesmeasure samples
FlameFlame Simpler, less Simpler, less
expensive expensive instrumentationinstrumentation
Lower operating costsLower operating costs Greater reproducibilityGreater reproducibility
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Emission Spectroscopies Cont.
Plasma (def.) Electrically conducting Plasma (def.) Electrically conducting gaseous mixture containing significant gaseous mixture containing significant concentrations of cations and electronsconcentrations of cations and electrons
ICP and DCPICP and DCP
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Inductively Coupled Plasma
Inductively coupled Inductively coupled means that the plasma means that the plasma is generated due to is generated due to differences in the differences in the magnetic field and magnetic field and currentscurrents
Temp. very hot (4000-Temp. very hot (4000-8000K)8000K) Good & badGood & bad
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Direct Current Plasma (DCP)
Plasma forms by Plasma forms by bringing graphite and bringing graphite and W electrodes in W electrodes in contact with one contact with one anotheranother
Temp @ core 10,000KTemp @ core 10,000K
in viewing region in viewing region 5000K5000K
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ICP DCP Comparison
DCP is an order of DCP is an order of magnitude less magnitude less sensitive than ICPsensitive than ICP
Similar Similar reproducibilitiesreproducibilities
DCP requires less ArDCP requires less Ar
Auxillary power less Auxillary power less expensive in DCPexpensive in DCP
Graphite electrode Graphite electrode must be replaced every must be replaced every couple of hourscouple of hours
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Comparison of Plasma to Flame Emission Sources Plasma sources offer significantly better Plasma sources offer significantly better
quantitative data than do other flame quantitative data than do other flame emission sourcesemission sources
- High stability- High stability
- Low noise- Low noise
- Low background- Low background
- Freedom from interferences- Freedom from interferences
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Comparison between Atomic Absorption & Emission Techniques
AASAAS AESAES
InstrumentsInstruments Requires HC lamp for each Requires HC lamp for each elementelement
No high quality MC requiredNo high quality MC required
Flame/ sample is sourceFlame/ sample is source
Requires high quality MCRequires high quality MC
Operator SkillOperator Skill
Bkgd.CorrectionBkgd.Correction
Prec. & Prec. & AccuracyAccuracy
InterferencesInterferences
Detection limitDetection limit
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Comparison between Atomic Absorption & Emission Techniques
AASAAS AESAES
InstrumentsInstruments Requires HC lamp for each Requires HC lamp for each elementelement
No high quality MC requiredNo high quality MC required
Flame/ sample is sourceFlame/ sample is source
Requires high quality MCRequires high quality MC
Operator SkillOperator Skill Lower skillLower skill Higher skillHigher skill
Bkgd.CorrectionBkgd.Correction
Prec. & Prec. & AccuracyAccuracy
InterferencesInterferences
Detection limitDetection limit
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Comparison between Atomic Absorption & Emission Techniques
AASAAS AESAES
InstrumentsInstruments Requires HC lamp for each Requires HC lamp for each elementelement
No high quality MC requiredNo high quality MC required
Flame/ sample is sourceFlame/ sample is source
Requires high quality MCRequires high quality MC
Operator SkillOperator Skill Lower skillLower skill Higher skillHigher skill
Bkgd.CorrectionBkgd.Correction Harder to doHarder to do Easier to doEasier to do
Prec. & Prec. & AccuracyAccuracy
InterferencesInterferences
Detection limitDetection limit
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Comparison between Atomic Absorption & Emission Techniques
AASAAS AESAES
InstrumentsInstruments Requires HC lamp for each Requires HC lamp for each elementelement
No high quality MC requiredNo high quality MC required
Flame/ sample is sourceFlame/ sample is source
Requires high quality MCRequires high quality MC
Operator SkillOperator Skill Lower skillLower skill Higher skillHigher skill
Bkgd.CorrectionBkgd.Correction Harder to doHarder to do Easier to doEasier to do
Prec. & Prec. & AccuracyAccuracy
Unskilled betterUnskilled better
Same for skilledSame for skilled
Unskilled worseUnskilled worse
InterferencesInterferences
Detection limitDetection limit
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Comparison between Atomic Absorption & Emission Techniques
AASAAS AESAES
InstrumentsInstruments Requires HC lamp for each Requires HC lamp for each elementelement
No high quality MC requiredNo high quality MC required
Flame/ sample is sourceFlame/ sample is source
Requires high quality MCRequires high quality MC
Operator SkillOperator Skill Lower skillLower skill Higher skillHigher skill
Bkgd.CorrectionBkgd.Correction Harder to doHarder to do Easier to doEasier to do
Prec. & Prec. & AccuracyAccuracy
Unskilled betterUnskilled better
Same for skilledSame for skilled
Unskilled worseUnskilled worse
InterferencesInterferences Spectral interferences corrected Spectral interferences corrected in AESin AES
Chemical interferences Chemical interferences on AE (flame) bad, on AE (flame) bad, plasma eliminatedplasma eliminated
Detection limitDetection limit
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Comparison between Atomic Absorption & Emission Techniques
AASAAS AESAES
InstrumentsInstruments Requires HC lamp for each Requires HC lamp for each elementelement
No high quality MC requiredNo high quality MC required
Flame/ sample is sourceFlame/ sample is source
Requires high quality MCRequires high quality MC
Operator SkillOperator Skill Lower skillLower skill Higher skillHigher skill
Bkgd.CorrectionBkgd.Correction Harder to doHarder to do Easier to doEasier to do
Prec. & Prec. & AccuracyAccuracy
Unskilled betterUnskilled better
Same for skilledSame for skilled
Unskilled worseUnskilled worse
InterferencesInterferences Spectral interferences corrected Spectral interferences corrected in AESin AES
Chemical interferences Chemical interferences on AE (flame) bad, on AE (flame) bad, plasma eliminatedplasma eliminated
Detection limitDetection limit Flame some metals better on Flame some metals better on AA than AESAA than AES
Plasma comparable to Plasma comparable to flame for some metals, flame for some metals, other metals plasma other metals plasma betterbetter
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Comparison of Metal Spectroscopic Techniques
Performance Performance CriteriaCriteria
Flame Flame AAAA
Electrothermal Electrothermal SamplingSampling
Flame Flame AESAES
DCPDCP ICPICP
Dynamic Dynamic rangerange
limitedlimited limitedlimited widewide widewide WideWide
Qualitative Qualitative analysisanalysis
Elemental Elemental rangerange
Trace Trace analysisanalysis
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Comparison of Metal Spectroscopic Techniques
Performance Performance CriteriaCriteria
Flame Flame AAAA
Electrothermal Electrothermal SamplingSampling
Flame Flame AESAES
DCPDCP ICPICP
Dynamic Dynamic rangerange
limitedlimited limitedlimited widewide widewide WideWide
Qualitative Qualitative analysisanalysis
poorpoor poorpoor excellentexcellent excellentexcellent excellentexcellent
Elemental Elemental rangerange
Trace Trace analysisanalysis
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Comparison of Metal Spectroscopic Techniques
Performance Performance CriteriaCriteria
Flame Flame AAAA
Electrothermal Electrothermal SamplingSampling
Flame Flame AESAES
DCPDCP ICPICP
Dynamic Dynamic rangerange
limitedlimited limitedlimited widewide widewide WideWide
Qualitative Qualitative analysisanalysis
poorpoor poorpoor excellentexcellent excellentexcellent excellentexcellent
Elemental Elemental rangerange
excellentexcellent excellentexcellent excellentexcellent excellentexcellent excellentexcellent
Trace Trace analysisanalysis
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Comparison of Metal Spectroscopic Techniques
Performance Performance CriteriaCriteria
Flame Flame AAAA
Electrothermal Electrothermal SamplingSampling
Flame Flame AESAES
DCPDCP ICPICP
Dynamic Dynamic rangerange
limitedlimited limitedlimited widewide widewide WideWide
Qualitative Qualitative analysisanalysis
poorpoor poorpoor excellentexcellent excellentexcellent excellentexcellent
Elemental Elemental rangerange
excellentexcellent excellentexcellent excellentexcellent excellentexcellent excellentexcellent
Trace Trace analysisanalysis
excellentexcellent excellentexcellent excellentexcellent excellentexcellent excellentexcellent
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Comparison of Metal Spectroscopic Techniques
Performance Performance CriteriaCriteria
Flame Flame AAAA
Electrothermal Electrothermal SamplingSampling
Flame Flame AESAES
DCPDCP ICPICP
Dynamic Dynamic rangerange
limitedlimited limitedlimited widewide widewide WideWide
Qualitative Qualitative analysisanalysis
poorpoor poorpoor excellentexcellent excellentexcellent excellentexcellent
Elemental Elemental rangerange
excellentexcellent excellentexcellent excellentexcellent excellentexcellent excellentexcellent
Trace Trace analysisanalysis
excellentexcellent excellentexcellent excellentexcellent excellentexcellent excellentexcellent
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Comparison of Metal Spectroscopic Techniques continued
Performance Performance CriteriaCriteria
Flame Flame AAAA
Electrothermal Electrothermal SamplingSampling
Flame Flame AESAES
DCPDCP ICPICP
Matrix Matrix interferncesinterfernces
highhigh highhigh highhigh lowlow lowlow
Spectral Spectral InterferenceInterferencess
Precision & Precision & AccuracyAccuracy
CostsCosts
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Comparison of Metal Spectroscopic Techniques continued
Performance Performance CriteriaCriteria
Flame Flame AAAA
Electrothermal Electrothermal SamplingSampling
Flame Flame AESAES
DCPDCP ICPICP
Matrix Matrix interferncesinterfernces
highhigh highhigh highhigh lowlow lowlow
Spectral Spectral InterferenceInterferencess
lowlow lowlow lowlow moderatemoderate highhigh
Precision & Precision & AccuracyAccuracy
CostsCosts
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Comparison of Metal Spectroscopic Techniques continued
Performance Performance CriteriaCriteria
Flame Flame AAAA
Electrothermal Electrothermal SamplingSampling
Flame Flame AESAES
DCPDCP ICPICP
Matrix Matrix interferncesinterfernces
highhigh highhigh highhigh lowlow lowlow
Spectral Spectral InterferenceInterferencess
lowlow lowlow lowlow moderatemoderate highhigh
Precision & Precision & AccuracyAccuracy
Better Better for for unskilledunskilled
Same Same skilledskilled
Worse Worse for for unskilled unskilled same same skilledskilled
CostsCosts
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Comparison of Metal Spectroscopic Techniques continued
Performance Performance CriteriaCriteria
Flame Flame AAAA
Electrothermal Electrothermal SamplingSampling
Flame Flame AESAES
DCPDCP ICPICP
Matrix Matrix interferncesinterfernces
highhigh highhigh highhigh lowlow lowlow
Spectral Spectral InterferenceInterferencess
lowlow lowlow lowlow moderatemoderate highhigh
Precision & Precision & AccuracyAccuracy
Better Better for for unskilledunskilled
Same Same skilledskilled
Worse Worse for for unskilled unskilled same same skilledskilled
CostsCosts $$$$ $$$$$$ $$ $$$$$$ $$$$$$$$
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Comparison of Metal Spectroscopic Techniques continued
Performance Performance CriteriaCriteria
Flame Flame AAAA
Electrothermal Electrothermal SamplingSampling
Flame Flame AESAES
DCPDCP ICPICP
Costs Costs
InstrumentatInstrumentationion
lowlow lowlow lowlow moderatemoderate highhigh
MaintenanceMaintenance
Sample Sample PreparationPreparation
Operator Operator skillskill
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Comparison of Metal Spectroscopic Techniques continued
Performance Performance CriteriaCriteria
Flame Flame AAAA
Electrothermal Electrothermal SamplingSampling
Flame Flame AESAES
DCPDCP ICPICP
Costs Costs
InstrumentatInstrumentationion
lowlow lowlow lowlow moderatemoderate highhigh
MaintenanceMaintenance lowlow lowlow lowlow moderatemoderate highhigh
Sample Sample PreparationPreparation
Operator Operator skillskill
![Page 24: Emission Spectroscopy](https://reader033.fdocuments.us/reader033/viewer/2022061111/545463efb1af9fb5468b47f9/html5/thumbnails/24.jpg)
Comparison of Metal Spectroscopic Techniques continued
Performance Performance CriteriaCriteria
Flame Flame AAAA
Electrothermal Electrothermal SamplingSampling
Flame Flame AESAES
DCPDCP ICPICP
Costs Costs
InstrumentatInstrumentationion
lowlow lowlow lowlow moderatemoderate highhigh
MaintenanceMaintenance lowlow lowlow lowlow moderatemoderate highhigh
Sample Sample PreparationPreparation
moderatemoderate moderatemoderate lowlow moderatemoderate moderatemoderate
Operator Operator skillskill
![Page 25: Emission Spectroscopy](https://reader033.fdocuments.us/reader033/viewer/2022061111/545463efb1af9fb5468b47f9/html5/thumbnails/25.jpg)
Comparison of Metal Spectroscopic Techniques continued
Performance Performance CriteriaCriteria
Flame Flame AAAA
Electrothermal Electrothermal SamplingSampling
Flame Flame AESAES
DCPDCP ICPICP
Costs Costs
InstrumentatInstrumentationion
lowlow lowlow lowlow moderatemoderate highhigh
MaintenanceMaintenance lowlow lowlow lowlow moderatemoderate highhigh
Sample Sample PreparationPreparation
moderatemoderate moderatemoderate lowlow moderatemoderate moderatemoderate
Operator Operator skillskill
lowerlower higherhigher higherhigher higherhigher higherhigher