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Chapter 9 Atomic Absorption and Atomic Fluorescence Spectrometry.

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Presentation on theme: "Chapter 9 Atomic Absorption and Atomic Fluorescence Spectrometry."— Presentation transcript:

1 Chapter 9 Atomic Absorption and Atomic Fluorescence Spectrometry

2 Atomic Spectroscopy Atomization is by far the most critical step in atomic spectroscopy. In AAS and AFS there are two factors involved.  The intensity of light source.  The probability of transition.

3 Flame Atomization

4 Flame Structure

5 Flame Atomizer

6

7 Electrothermal Atomizers Graphite furnace atomic absorption spectrometry (GFAAS) is also known by various other acronyms, including electrothermal atomic absorption spectrometry (ETAAS). An ideal graphite furnace should fulfill the following requirements:  A constant temperature in time and space during the interval in which free atoms are produced  Quantitative atom formation regardless of the sample composition  Separate control of the volatilization and atomization processes  High sensitivity and good detection limits A minimum of spectral interferences

8 Specialized Atomization Techniques  Glow Discharge Atomization  Hydride Atomization  Cold-Vapor Atomization

9 Flame Atomic Absorption Spectroscopy

10 Radiation Sources  Doppler Broadening  Pressure Broadening  Electrodeless Discharge Lamps  Source Modulation  Hollow Cathode Lamps:

11 Spectrophotometers In general, the instrument must contain:  Narrow bandwidth to isolate the line chosen for measurement  Sufficient glass filter  Interchangeable interference filters  Good-quality ultraviolet/visible monochromators  Photomultiplier tubes

12 Spectrophotometers  Single-Beam  Double-Beam

13 Spectral Interferences  The Two-Line Correction Method  The Continuum-Source Correction Method  Background Correction Based on the Zeeman Effect  Background Correction Based on the Source Self-Reversal

14 Chemical Interference The equilibria of principle interest include:  Formation of Compounds of Low Volatility  Dissociation Reactions  Ionization

15 Calibration Curves  Should follow Beer’s Law

16 Standard Addition Method

17 Instrumentation Sources:  Hollow Cathode Lamp- only observed the fluorescent signal during pulses  Electrodeless Discharge Lamp- produced intensities that exceed those of hollow cathode lamps  Lasers- ideal source with high intensities and narrow bandwidths

18 Instrumentation Dispersive Instruments- They are made up of a modulated source, an atomizer, a monochromator or an interference filter system, a detector, and a signal processor and readout. Nondispersive Instruments- They ideally are made up of a source, an atomizer, and a detector. Advantages:  Simplicity and low-cost instrumentation  Ready adaptability to multi-element analysis  High-energy throughput and thus high sensitivity  Simultaneous collection of energy from multiple lines, enhancing sensitivity

19 References  www.anachemumu.se.htm  www.aurora-instr.com/right.htm  www.anachem.umu.se/jumpstation.htm  www.anachem.umu.se/cgi/jumpstation.exe?AtomicSpectroscopy  www.anachem.umu.se/cgi/jumpstation.exe?OpticalMolecularSpectrosc opy  www.minyos.its.rmit.edu.au/~rcmfa/mstheory.html  http://science.widener.edu/sub/ftir/intro_it.html  http://www.s-a-s.org/  http://www.chemsw.com  http://www.scimedia.com/chem-ed/spec/atomic/aa.htm  http://nercdg.org  http://www.analyticon.com  www.lcgmag.com/  www.lcms.com/

20 References  www.dq.fct.unl.pt/QOF/Chroma.html  www-ssg.chem.utas.edu.au/  www.yahoo.com/science/chemistry/chromatography/  www.onlinegc.com  http://www.scimedia.com/chem-ed/analytic/ac-meth.htm  http://www.scimedia.com/chem-ed/spec/atomic/aa.htm  http://www.scimedia.com/chem-ed/spec/atomic/afs.htm  http://www.cee.vt.edu/program_areas/environmental/teach/smprimer/a a/aa.html#Features  http://www.anachem.umu.se/aas/gfaas.htm  http://www.agsci.ubc.ca/fnh/courses/food302/atomic/aatomic03.htm#el ectro  http://www.scpscience.com/products/AA/hollowlamps.asp  http://las.perkinelmer.com/catalog/Product.aspx?ProductId=N3050691  http://elchem.kaist.ac.kr/vt/chem-ed/spec/atomic/aa.htm


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