Atomic Emission Spectroscopy

Slides:



Advertisements
Similar presentations
Lecture 6 ATOMIC SPECTROSCOPY
Advertisements

FLAME SPECTROSCOPY The concentration of an element in a solution is determined by measuring the absorption, emission or fluorescence of electromagnetic.
427 PHC. Direct-Current Plasma  A direct-current plasma (DCP) is created by an electrical discharge between two electrodes. A plasma support gas is necessary,
ACADs (08-006) Covered Keywords analytical balance, conductivity bridge with flow cell, inductively coupled plasma analyzer, in-line sodium monitor, ion.
Lecture 16. LIPS. Introduction a type of atomic emission spectroscopy which uses a highly energetic laser pulse as the excitation source. The laser is.
Atomic Emission Spectroscopy
1 Atomic Absorption Spectroscopy Atomic Emission Spectroscopy Lecture 18.
Chapter 10 ATOMIC EMISSION SPECTROMETRY
AAS and FES (Ch 10, 7th e, WMDS)
Atomic Emission Spectroscopy
Inductively Coupled Plasma Mass Spectrometry or ICP-MS
Atomic Absorption Spectroscopy Prof Dr Hisham E Abdellatef 2011.
Atomic Absorption and Atomic Fluorescence Spectrometry Wang-yingte Department of Chemistry
1 A TOMIC SPECTROMETRIC METHODS PART 9. 2 Interferences : Four classes of interferences: 1-Spectral interferences 2-Chemical interferences 3- Refractory.
AAS and FES (Ch 9, 7th e, WMDS)
Atomic Emission Spectroscopy. Chem Introduction Atomic absorption is the absorption of light by free atoms. An atomic absorption spectrophotometer.
AA and Atomic Fluorescence Spectroscopy Chapter 9
Atomic Spectroscopy Atomic Spectroscopic Methods Covered in Ch 313: Optical Atomic Spectrometry (Ch 8-10) Atomic X-ray Spectrometry (Ch 12) Atomic Mass.
1 Atomic Absorption Spectroscopy. 2 Atomic Transitions: Excitation and Emission.
Flame photometry.
1 Molecular Luminescence Spectroscopy Lecture 31.
Emission Spectroscopy Based upon Plasma, Arc, and Spark Atomization Arc Arc Higher Temperature Higher Temperature Lower interelement interference Lower.
427 PHC.  Atomic emission spectroscopy (AES) is based upon emission of electromagnetic radiation by atoms.
Instrumental Chemistry Chapter 11 Atomic Mass Spectrometry.
Atomic Emission - AES M* → M + hn Thermal excitation M → M*
Atomic Absorption Spectroscopy (AAS)
Monroe L. Weber-Shirk S chool of Civil and Environmental Engineering Atomic-Absorption (AA) 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
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 Spectroscopy
Atomic Emission Spectrometry
Chapter 10 Atomic Emission Spectrometry
1.1 Inductively coupled plasma (ICP) Three Argon flow 1.Plasma gas (10-20 L/min) 2.Nebulizer gas (~1L/min) 3.Optional auxiliary gas (~0.5L/min) Radio-frequency.
Honors Forensic Science.  Introduction  Organic substances constitute a substantial portion of physical evidence submitted to crime labs  Carbon does.
Atomic Absorption Spectroscopy
1 Components of Optical Instruments Lecture Silicon Diode Transducers A semiconductor material like silicon can be doped by an element of group.
1 Atomic Emission Spectroscopy Lecture Advantages of Plasma Sources 1.No oxide formation as a result of two factors including Very high temperature.
1 Atomic Absorption Spectroscopy Lecture Emission in Flames There can be significant amounts of emission produced in flames due to presence of flame.
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.
1 Introduction to Atomic Spectroscopy Atomic Absorption Spectroscopy Lecture 12.
Beers Law for a Single Component Sample I0I0 A = Absorbance = - log 10 I I / I 0 b = Optical path length c = Solution Concentration (M/L) ε = Molar Absorptivity.
Mass spectrometry (Test) Mass spectrometry (MS) is an analytical technique that measures masses of particles and for determining the elemental composition.
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.
Plasma A Plasma consists of a collection of free-moving electrons and ions and is very hot. Energy must be continually applied to sustain the plasma.
Atomic Emission Spectroscopy
1 Introduction to Atomic Spectroscopy Lecture 10.
Chapter 10 Atomic Emission Spectrometry
Chapter 6 Inorganic Analysis 6.1 Notes Pg
1 Atomic Emission Spectroscopy Lecture 18 Arcs, Sparks And Plasma.
Chemistry 4631 Instrumental Analysis Lecture 18 Chem 4631.
Chapter 29 Mass Spectrometry. 29 A Principles of mass spectrometry In the mass spectrometer, analyte molecules are converted to ions by applying energy.
Atomic Emission Spectroscopy Lecture 18
Flame Emission Spectrometry
Chapter 6 INORGANIC ANALYSIS
Introduction to Atomic Spectroscopy
Elemental composition
Instrumental Chemistry
Inorganic Analysis 6.1 Notes Pg
Atomic Absorption Spectroscopy. Atomic absorption spectroscopy is based on the same principle as the flame test used in qualitative analysis.
Spectroscopy Uses emission and absorption of light by electrons moving between ground and excited state configuration, hence electronic configuration.
Atomic Emission Spectroscopy
FLAME SPECTROSCOPY The concentration of an element in a solution is determined by measuring the absorption, emission or fluorescence of electromagnetic.
Inductively Coupled Plasma
Presentation transcript:

Atomic Emission Spectroscopy Lecture 20

Applications of Plasma Sources 1. Since plasma sources result in a very large number of emission lines, these sources can be used for both qualitative and quantitative analysis. 2. The signal obtained from plasma sources is stable, has a low noise and background, as well as freedom from interferences. 3. Requires sample preparation similar to AAS

4. Plasma sources are usually best suited for operation in the ultraviolet region, therefore, elements having emission lines below 180 nm (like B, P, S, N, and C) can only be analyzed under vacuum since air components absorb under 180 nm. Also, alkali metals are difficult to analyze since their best lines under plasma conditions occur in the visible or near infrared. 5. An analytical emission line can easily be located but will depend on the other elements present since spectral line interferences are encountered in plasma sources due to the very high temperatures used.

6. Linear calibration plots are usually obtained but departure from linearity is observed at high concentrations; due to self absorption as well as other instrumental reasons. An internal standard is often used in emission methods to correct for fluctuations in temperature as well as other factors. The calibration plot in this case is a plot between the concentration of analyte and the ratio of the analyte to internal standard signal. The internal standard is a substance that is added in a constant amount to all samples, blanks, and standards; therefore it must be absent from initial sample matrix. The internal standard should have very close characteristics (both chemically and physically) to analyte.

Elements by ICP-AES Different elements have different emission intensities. Alkalis (Na, K, Rb, Cs) are weakly emitting. Alkaline Earths (Be, Mg, Ca, Sr, Ba ) are strongly emitting.

INDUCTIVELY COUPLED PLASMA-MASS SPECTROMETRY (ICP-MS) - Very sensitive and good for trace analysis - Plasma produces analyte ions - Ions are directed to a mass spectrometer - Ions are separated on the basis of their mass-to-charge ratio - A very sensitive detector measures ions - Very low detection limits

Introduction of Solid Samples A variety of techniques were used to introduce solid samples into atomizers. These include: 1. Conductive Samples If the sample is conductive and is of a shape that can be directly used as an electrode (like a piece of metal or coin), that would be the choice for sample introduction in arc and spark techniques. Otherwise, powdered solid samples are mixed with fine graphite and made into a paste. Upon drying, this solid composite can be used as an electrode. The discharge caused by arcs and sparks interacts with the surface of the solid sample creating a plume of very fine particulates and atoms that are swept into the plasma by argon flow.

Laser Ablation Sufficient energy from a focused intense laser will interact with the surface of samples (in a similar manner like arcs and sparks) resulting in ablation. The vapors of molecules and atoms are swept into the plasma source for complete atomization and excitation. Laser ablation is becoming increasingly used since it is applicable to conductive and nonconductive samples.

The Glow Discharge Technique The technique is used for sample introduction and atomization as well. The electrodes are kept at a 250 to 1000 V DC. This high potential is sufficient to cause ionization of argon, which will be accelerated to the cathode where the sample is introduced. Collision of the fast moving energetic argon ions with the sample (cathode) causes atomization by a process called sputtering. Samples should thus be conductive to use the technique of glow discharge. The vapors of molecules and atoms are swept into the plasma source for complete atomization and excitation by flowing argon. However, nonconductive samples were reported to be atomized by this technique where they were mixed with a conductor material like graphite or powdered copper.

Emission Spectroscopy Based on Arcs and Sparks Samples are excited in the gap between a pair of electrodes connected to a high potential power supply (200 VDC or 2200- 4400 VAC). The high potential applied forces a discharge between the two electrodes to occur where current passes between the two separated electrodes (temperature rises due to very high resistance).

The very high temperature (4000-5000 oC) realized in the vicinity between the two electrodes provide enough energy for atomization and excitation of the samples in this region or when the sample is, or a part of, one of the electrodes. Arc and spark methods are mainly used as qualitative techniques and can also be used as semiquantitative techniques.

Sample Handling and Preparation If the sample is conductive and is of a shape that can be directly used as an electrode (like a piece of metal or coin), that would be the choice for sample introduction in arc and spark techniques. Otherwise, powdered solid samples are mixed with fine graphite and made into a paste. Upon drying, this solid composite can be used as an electrode. The discharge caused by arcs and sparks interacts with the surface of the solid sample creating a plume of very fine particulates and atoms that are excited and emission is collected. The figure below shows some common shapes of graphite electrodes used in arc and spark sources.

Carbon electrodes Sample pressed into electrode or mixed with Cu powder and pressed - Briquetting (pelleting) Cyanogen bands (CN) 350-420 nm occur with C electrodes in air -He, Ar atmosphere Arc/spark unstable each line measured >20 s needs multichannel detection

Instruments for Arcs and Sparks In most cases, emission from atoms in an arc or spark is directed to a monochromator with a long focal length and the diffracted beams are allowed to hit a photographic film. This typical instrument is called a spectrograph since it uses a photographic film as the detector.

Spectrograph Beginning 1930s photographic film detector Cheap Long integration times Difficult to develop/analyze Non-linearity of line "darkness“

Potential Source Photographic Film Graphite Electrodes