Post on 04-Apr-2018
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Unternehmen der Analytik Jena Gruppe
Powerful Analytics based on Modern Spectrometers
Gerhard SchlemmerAnalytik Jena AG, Konrad- Zuse- Str. 1, 07745 Jena
g.schlemmer@analytik-jena.de
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Unternehmen der Analytik Jena Gruppe
Powerful Analytics based on Modern Spectrometers
• Optimizing Analytical Quality
• Absorption: Line oder Spectrum?
• Atomic Fluorescence: simple optics, excellent
S/N: Where are the limits?
• Absorption/ Emission
– Sequential or simultaneous?
• Bio Analytics
– Limitations and chances due to new materials
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Unternehmen der Analytik Jena Gruppe
Recovery;Calibration
Detector, Optics, Source,
Elektronic, Correktions,
Sample presentation
Long Term Stability
Range of UseDetector, Optics, Source, Elektronics Corrections, Sampel presentation
Detection Limit
Repeatability Time for Measurement
Atomizer, Meas.Volume, Corrections
(Detektor, Optics)
RSD
DL, RSD Working range.
Detector, Optics, Source, Elektronics
Noise
DL
RSD
Working range.
Atomizer, Meas.Volume, Optics, Source
Sensitivity
InfluencesSystem ComponentAnalyt. Parameter
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Absorption:Line oder Spectrum?
Line Source AAS OpticsCzerny- Turner MonochromatorResolution~ 200 pm
Double Echelle-MonochromatorResolution ~ 2 pmBased on „DEMON“ ISAS-Berlin
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Unternehmen der Analytik Jena Gruppe
Absorption:Line oder Spectrum?
LS AASSource IntensityMn – Triplet:
279, 4817 nm279, 8269 nm280, 1085 nm
0 , 0
0 , 2
0 , 5
0 , 7
1 , 0
2 7 9 , 3 2 7 9 , 4 2 7 9 , 5 2 7 9 , 6 2 7 9 , 7 2 7 9 , 8 2 7 9 , 9 2 8 0 , 0 2 8 0 , 1 2 8 0 , 2 2 8 0 , 3
W e l le n lä n g e ( n m )
Ab
so
rpti
on
CS AASAbsorption spectraMn – Triplet:
279, 4817 nm279, 8269 nm280, 1085 nm
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Unternehmen der Analytik Jena Gruppe
Spectral window 200 pm
Absorption profile 1-5 pm
....................................................................................
LS
CS
Emission line ~2 pm
Spectral window 200 pm
CCD-Array with a resolution of ~ 2pm/ pixel
Absorption: Linie oder Spektrum?
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Absorption: Line oder Spectrum?
Is a source line really one line?: Emission of a Cd- hollow cathode lamp as a function of the lamp current.
Ref. T. Labatzke, Analytik- Jena,
C. Scholz, D. Mory, LTB, Berlin 2002
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Unternehmen der Analytik Jena Gruppe
reference pixels
simultaneous
optical double beam
sequential
source drift
reference pixels
Reference spektra
simultaneous
BG correction, sequential(D2 lamp, Zeeman effekt, line reversemethod)
unspecific absorption
reference pixels
simultaneous
lamp modulation
sequential
thermal emission
correction HR-CS- AAScorrection LS-AASsource of error
Corrections required in AAS
Absorption: Line oder Spectrum?
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Example: complex Background close to the analyte line
NO- Structure in the vicinity of 213,857 nm
HR-CSAASA New Way to look at Atomic Absorbance
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HR-CSAASA New Way to look at Atomic Absorbance
Determination of P on PO- Band at 246,400 nm using theC2H2/ Air Flame (Absorbance reading on molecular Band)
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HR-CSAASA New Way to look at Atomic Absorbance
Abs. wave length spectra 3D
Abs. wave length spectra 2D
Gain in information: absorbance becomes 3. dimensional
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Unternehmen der Analytik Jena Gruppe
Absorption: Line or Spectrum?
• Extended application range: atomic+molecular
• Simultaneous corrections for better accuracy
• Much more information on background– Atomic lines
– Molecular band and fine structure
– Pushing the limits in complex matrices
• Independence of c0/m0 on lamp type, age or fine structur– Opening a new chapter on the way towards absolute
analysis
• Will we finally approach real simultaneous AAS?
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Atomic Fluorescence
System Mercur „Duo“fluorescence and absorption in one system; measurement of mercury vapour in an argon carrier stream
Signalvergleich AFS / AAS
0,00
0,01
0,01
0,02
0,02
0,03
0 5 10 15 20 25 30 35 40
Integrationszeit [ sec. ]
Inte
nsitä
t [ In
ts ]
-0,005
0
0,005
0,01
0,015
0,02
0,025
0,03
Extik
tion
[ E
xt ]
AFS-Signal 1µg/L
AAS-Signal 1µg/L
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AAS vers.AFS
Background Abs.Source driftBackground Abs.
Quenching
Interferences
102,5104Lin. Calib. range
3 ng/L (Hg)0.3 ng/L (Hg)DL
All techniquesCVG onlyApplication
AASAFSParameter
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Simultaneous vers. Sequential Reading ICP- OES
++++Content of info
+++Ruggedness
+++DL
+++Interferences
+++Cost
+++++Working range
++++Speed p. element
++Speed p. sample
ICP- Simult.ICP- SequentialParameter
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Simultaneous vers. Sequential ReadingUV/VIS
+++S/N
Moving partsFixed opticsRuggedness
Selected WLFull illuminationSample
0.5 nm1-2 nmOptical resolution
0.3%T*/0.005%T0.9%T*/0.05%T**Stray light
~3A~2ALin.Calib.Range
Slow 1 minVery fast <<1sSpectra
Sequential (S250)
Simultaneous (S600)
Parameter
* Validation at 198 nm; ** Validation at 220 nm
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Bio AnalyticsLimitations and chances due to new applications
• Chips/cells/ flow system require photons and detection on a spot
• Direct contact with bio- media may require biocompatible materials
• Often extrem cost sensitive parts (disposables)
– Use of lightwave guides-
– Use of fiber- optic sensors-
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Bio Analyticsjust a few examples of light wave
guides/ fiber-optical sensors
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Gesellschaft Deutscher ChemikerFachgruppe Analytische Chemie
Deutscher ArbeitskreisSpektroskopie
DASp: DoktorandentreffenJena, 9-10 Juli 2008
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ESAS 2008Weimar, Sept 28th-Oct 1stThe European Spectroscopy Symposiumwww.esas-symposium.de