ContrAA ® - A Revolution in Spectroscopy Basics and Applications of High-Resolution Continuum Source AAS.

Slides:



Advertisements
Similar presentations
Good Practices of Fluorescence Spectroscopy
Advertisements

Furnace aa. Today is Guy Fawkes Day L’vov platform furnace Sample is placed on platform Temp of platform rises more slowly than that of walls.
Atomic Absorption Spectroscopy (AAS)I
FLAME SPECTROSCOPY The concentration of an element in a solution is determined by measuring the absorption, emission or fluorescence of electromagnetic.
ATOMIC ABSORPTION SPECTROMETER
All material required to answer the following questions are contained in the lecture notes. Tutorial CM 3007.
Elemental Spectroscopy ICP-OES
7. Beer’s Law and It’s Implications for Instrument Construction.
Atomic Absorption and Atomic Fluorescence Spectrometry Wang-yingte Department of Chemistry
AAS and FES (Ch 9, 7th e, WMDS)
AA and Atomic Fluorescence Spectroscopy Chapter 9
INTRODUCTION TO OPTICAL METHODS
Atomic Absorption Spectrometry Dr AKM Shafiqul Islam University Malaysia Perlis.
HL Chemistry - Option A: Modern Analytical Chemistry ATOMIC ABSORPTION SPECTROSCOPY.
1 Molecular Luminescence Spectroscopy Lecture 31.
Atomic Emission Spectroscopy
ATOMIC SPECTROMETRY 1. Flames 2. Electrothermal Atomizers 3. Plasmas.
Chem. 133 – 4/1 Lecture. Announcements I Lab –Returning Term Project Proposals (I expect to be getting boxes of supplies ready) –Returning Set 2 Period.
announcements and reminders
Atomic Absorption Spectroscopy (AAS)
Fluorescence. Topics Sensitivity (nM-pM) –Contrast UV-vis measurements Derivatization Laser-Induced Fluorescence.
AES: Figures of Merit Linearity over 4 to 5Linearity over 4 to 5 concentration decades concentration decades Reasons for deviations Reasons for deviations.
Atomic Absorption Spectroscopy (AAS)
ATOMIC ABSORPTION AND ATOMIC FLUORESCENCE SPECTROMETRY Chap 9 Source Modulation Interferences in Atomic Absorption Interferences in Atomic Absorption Spectral.
Fluorescence. Topics Definition Instrumentation Sensitivity (nM-pM) –Contrast UV-vis measurements Derivatization Laser-induced Fluorescence.
Atomic Absorption Spectroscopy Elemental analysis Dissolved metals Source –Hallow Cathode Lamp –Cathode of specific element Sample –Acetylene-air flame,
Astronomical Spectroscopy
Atomic Absorption Spectroscopy
ATOMIC ABSORPTION SPECTROSCOPY
BC ILN Atomic Absorption Spectroscopy (AAS) 1 Thompson Rivers University.
Ahmad Aqel Ifseisi Assistant Professor of Analytical Chemistry College of Science, Department of Chemistry King Saud University P.O. Box 2455 Riyadh
IFTSUV: an Imaging Fourier Transform Spectrometer in the UV Anne Millard, 3 rd year PhD student, directed by P. Lemaire and J.-C. Vial.
Spectroscopy (continued) Last time we discussed what spectroscopy was, and how we could use the interaction of light with atoms and molecules to measure.
Atomic Emission Spectrometry
Chapter 10 Atomic Emission Spectrometry
Atomic Absorption Spectroscopy
14 October Observational Astronomy SPECTROSCOPY and spectrometers Kitchin, pp
1 Atomic Emission Spectroscopy Lecture Advantages of Plasma Sources 1.No oxide formation as a result of two factors including Very high temperature.
18 October Observational Astronomy SPECTROSCOPY and spectrometers Kitchin, pp
1 Atomic Absorption Spectroscopy Lecture Performance Characteristics of Electrothermal Atomizers Electrothermal atomization is the technique of.
ANALYTICAL CHEMISTRY CHEM 3811 CHAPTER 20
Atomic spectroscopy Elemental composition Atoms have a number of excited energy levels accessible by visible-UV optical methods ä Must have atoms (break.
ANALYTICAL CHEMISTRY CHEM 3811 CHAPTER 19 DR. AUGUSTINE OFORI AGYEMAN Assistant professor of chemistry Department of natural sciences Clayton state university.
Adv. Inst. Techs.  flame emission (eg flame photometer) known as low temperature emission ( K) ◦ first form of spectroscopy ◦ used in commercial.
SEM- Schematic Overview. Electron Detection Tungsten Filament Electron Source.
Atomic-absorption spectroscopy
ATOMIC ABSORPTION SPECTROSCOPY (AAS) Atomization: It is the conversion of molecules to their component atoms in gaseous state using a source of heat (flame).
1 Atomic Emission Spectroscopy Molecular Absorption Spectroscopy Lecture 21.
A TOMIC - ABSORPTION SPECTROSCOPY. Atomic absorption spectroscopy (AAS) is a technique for determining the concentration of a particular metal element.
Visible Spectro-polarimeter (ViSP) Conceptual Design David Elmore HAO/NCAR
What is Atomic Spectroscopy? – Sec Atomic Absorption Spectroscopy (AAS) versus Atomic Emission Spectroscopy (AES)
Atomic-absorption spectroscopy Lab3 Atomic-absorption spectroscopy.
Chapter 10 Atomic Emission Spectrometry
Chemistry 4631 Instrumental Analysis Lecture 18 Chem 4631.
Chem. 133 – 3/29 Lecture. Announcements I Grading – Set 2 lab reports (return?) – Term project proposals (still working on) – UV-Visible seemed to work.
Chapter 28 Atomic Spectroscopy.
Chem. 133 – 4/4 Lecture.
ATOMIC ABSORPTION AND ATOMIC FLUORESCENCE SPECTROMETRY
Flame Emission Spectrometry
Atomic Absorption and Atomic Fluorescence Spectrometry
The ratio of excited state to ground state atoms as a function of temperature is determined by the Maxwell-Boltzmann expression. Fig Excited state.
Spectrophotometer Dr . S. Jayakumar.
Elemental composition
Atomic Absorption and Atomic Fluorescence Spectrometry
Atomic Absorption Spectroscopy
Atomic Absorption Spectroscopy. Atomic absorption spectroscopy is based on the same principle as the flame test used in qualitative analysis.
Fluorescence.
SPECTROPHOTOMETRY Applied Chemistry.
Spectroscopy Uses emission and absorption of light by electrons moving between ground and excited state configuration, hence electronic configuration.
FLAME SPECTROSCOPY The concentration of an element in a solution is determined by measuring the absorption, emission or fluorescence of electromagnetic.
Presentation transcript:

contrAA ® - A Revolution in Spectroscopy Basics and Applications of High-Resolution Continuum Source AAS

Methods for element analysis contrAA ® - A Revolution in Spectroscopy2 AAS – a well established method for more than 50 years BUT !!  Simplicity  Less interferences  Robustness  Low purchase cost  Low operation cost  Single element method  Specific HCLs required  Unprofitable for many elements  Limitation in background correction

New instrument development needs motivation contrAA ® - A Revolution in Spectroscopy3 AAS goes multielement!

LS AAS Cx CuPb Fe Cd Ni Zn Single element method New instrument development needs motivation: We expect fast results 4contrAA ® - A Revolution in Spectroscopy

Real multielement Analysis CS AAS Sequential multi element analysis Cu, Pb, Fe, Cd, Ni, Zn… New instrument development needs motivation: We expect fast results 5contrAA ® - A Revolution in Spectroscopy

New instrument development needs motivation contrAA ® - A Revolution in Spectroscopy6 In case of a spectral interference, we can see only the result, but not the reason – therefore the optimization of method parameters to avoid the spectral interferences is difficult. Background correction failed, but why??? We need more information!

Key components of HR-CS AAS contrAA ® - A Revolution in Spectroscopy7 HR-CS AASLS-AAS Radiation source Xenon – short arc lampHCL, EDL, boosted HCL Atomizer Identical atomizer for flame and graphite technique Monochromator High resolution >1:140000Low resolution Detector CCD array detectorSingle spot detector (PMT) Software ASpectCS ® WinAAS ®

 Optical set up CS AAS Furnace Echelle grating Flame Arc lamp High Resolution Monochromator prism CCD detector ISAS Berlin  Low focal length: f  400 mm  High spectral resolution: / Δ > contrAA ® - A Revolution in Spectroscopy

Radiation source contrAA ® - A Revolution in Spectroscopy9  LS AAS Hollow cathode lamp (HCL) line radiator Cathode contains the element to be analyzed Xenon short arc lamp continuum radiator Covers whole wave length range 185 – 900 nm Determination of more than 67 elements with one lamp only  HR-CS AAS

Radiation source contrAA ® - A Revolution in Spectroscopy10 Different radiation sources in comparison A Xenon-short arc lamp, XBO 301, 300 W, (GLE Berlin), „Hot - Spot“ - Mode B Xenon lamp, L 2479, 300 W, (HAMAMATSU), diffuse mode C D2 - Lamp, MDO 620, 30 W, (HERAEUS) Source: „High-resolution continuum source AAS“ Welz,Becker-Roß,Florek,Heitmann Ag Au Pb Cd Pb Zn As

Atomizer in HR-CS AAS contrAA ® - A Revolution in Spectroscopy11 Graphite furnace atomizer Quartz cell atomizer Flame atomizer

Double Echelle Monochromator contrAA ® - A Revolution in Spectroscopy Source: ISAS Berlin 1: entrance slit (fixed) 2: off-axis parabolic mirror 3: prism in Littrow- position 4: intermediate slit (variable) 5: Echelle- grating in Littrow- position 6: CCD – array detector

LS AAS Emission scan Mn – Triplet: nm nm nm Monochromator resolution LS AAS vers. HR-CS AAS CS AAS Absorption spectra Resolution factor 100 better than LS AAS !!! 13contrAA ® - A Revolution in Spectroscopy

AnalyteWavelength (nm)Disturbing elements Wavelength (nm) -Difference (pm) Se196.03Fe As193.70Fe Zn Fe Cd228.80As Fe Ni Fe Sn Pb Fe Mn279.48Fe Cu324.75Fe Al396.15Fe High Resolution – spectral interferences 14contrAA ® - A Revolution in Spectroscopy

CCD Detector contrAA ® - A Revolution in Spectroscopy15 New detection technology Detector “Pixels” are illuminated and read out simultaneously and independently. 200 Pixels are used analytically 200 independent detectors ! 3 Pixels for AA measurement - and the others???

Corrections contrAA ® - A Revolution in Spectroscopy16 Type of interferenceLS-AASHR-CS AAS Lamp intensity driftOptical double beam sequential Reference pixels simultaneous Thermal emissionLamp modulation sequential Reference pixels simultaneous Non specific absorptionBG correction sequential Reference pixels reference spectrum simultaneous

Corrections contrAA ® - A Revolution in Spectroscopy17 In HR-CS AAS we have a Third Dimension, i.e. we can see a lot more !  We can see the spectral interference  We can avoid the spectral interference  And we have much better ways to correct for spectral interferences

Background correction and resolution contrAA ® - A Revolution in Spectroscopy18 V V Ni Fe

Corrections of discontinuous events contrAA ® - A Revolution in Spectroscopy19  OH, NO, CN are natural constituents of flame gases  NO, PO, SiO, CS etc. might be generated in the presence of high matrix concentration  Neither the D2 nor the Smith-Hieftje system can correct for this background,  the Zeeman system can only correct if the background is not affected by the magnetic field !  In HR-CS AAS we can measure and store a reference spectrum that can be subtracted from the sample spectrum using a least-squares algorithm Diatomic molecules with rotational fine structure

A Short Glance on Correction Models “Least Squares Background Correction ” 20contrAA ® - A Revolution in Spectroscopy

NO- Structure on Zn- line nm Corrections of discontinuous events - Recording of reference spectra blank: 1% HNO 3 1% HNO mg/L Zn 21contrAA ® - A Revolution in Spectroscopy

Correction of NO structure at nm Zn- line NO structures corrected Zn absorption spectra Corrections of discontinuous events - Recording of reference spectra 22contrAA ® - A Revolution in Spectroscopy

23 Quality is the difference Quality is the difference

contrAA ® - A Revolution in Spectroscopy24 Thank you for your attention!