Atomic absorption spectroscopy is a technique that uses the absorption of light to measure the concentration of gas phase atoms. It works by vaporizing a sample using a flame or graphite furnace and measuring the absorption of light from a hollow cathode lamp that emits light at a wavelength specific to the element being analyzed. The amount of light absorbed is directly proportional to the concentration of the element in the sample. The instrument includes a light source, atomizer, monochromator, and detector. It provides a simple and reliable way to analyze over 60 elements and is commonly used to detect metals in environmental samples.
2. Introduction
• It is very reliable and simple to use
• It can analyze over 62 elements
• It also measures the concentration of metals in sample
Atomic absorption spectroscopy is a quantitative
method of analysis of any kind of sample ; that is
applicable to many metals and a few nonmetals.
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3. HISTORY
• The technique was introduced in 1955 by Alan Walsh in
Australia ( 1916 – 1998 ).
• The first commercial atomic absorption spectrometer
was introduced in 1959.
The application of atomic
absorption spectra to chemical
analysis
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4. PRINCIPLE
• The technique uses basically the principle that free atoms ( gas )
generated in an atomizer can absorb radiation at specific frequency.
• Atomic absorption spectroscopy quantifies the absorption of
ground state atoms in the gaseous state.
• The atoms absorb ultraviolet or visible light and make transitions
to high electronic energy levels.
• The analyte concentration is determined from the amount of
absorption.
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5. • Concentration measurements are usually determined
from a working curve after calibrating the instrument
with standards of known concentration.
• Atomic absorption is very common technique for
detecting metals and metalloids in environmental
samples.
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9. LIGHT SOURCE
• Hollow Cathode Lamp are the most common radiation
source in AAS.
• It contains a tungsten anode and a hollow cylindrical
cathode made of the element to be determined.
• These are sealed in a glass tube filled with an inert gas
(neon or argon ) .
• Each element has its own unique lamp which must be
used for that analysis . 7
12. Sample Atomization Technique
Flame
Atomization
Electro thermal
Atomization
Hydride
Atomization
Cold-Vapor
Atomization
Atomization is separation of particles into individual
molecules and breaking molecules into atoms. This
is done by exposing the analyte to high
temperatures in a flame or graphite furnace .
Atomization
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13. FlameAtomization
• Nebulizer suck up liquid samples at controlled rate.
• Create a fine aerosol spray for introduction into flame.
• Mix the aerosol and fuel and oxidant thoroughly
for introduction into flame.
• An aerosol is a colloid of fine solid particles or liquid
droplets, in air or another gas.
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15. Disadvantagesof FlameAtomization
• Only 5-15% of the nebulized sample reaches the flame.
• A minimum sample volume of 0.5-1.0 ml is needed to
give a reliable reading.
• Samples which are viscous require dilution with a solvent.
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16. Electro ThermalAtomization
• Uses a graphite coated furnace to vaporize the sample.
• ln GFAAS sample, samples are deposited in a small
graphite coated tube which can then be heated to
vaporize and atomize the analyte.
• The graphite tubes are heated using a high current
power supply.
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18. Advantages of GraphiteFurnace
Technique
• Small sample size
• Very little or no sample preparation is needed
• Sensitivity is enhanced
• Direct analysis of solid samples
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19. Disadvantagesof GraphiteFurnace
Technique
• Analyte may be lost at the ashing stage
• The sample may not be completely atomized
• The precision is poor than flame method
• Analytical range is relatively low
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20.
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22. MONOCHROMATOR
• This is a very important part in an AA spectrometer. It is
used to separate out all of the thousands of lines.
• A monochromator is used to select the specific
wavelength of light which is absorbed by the sample, and
to exclude other wavelengths.
• The selection of the specific light allows the
determination of the selected element in the presence of
others.
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23. DIFFRACTIONGRATING
The process by which a beam of light or other system of waves is spread out
as a result of passing through a narrow aperture or across an edge, typically
accompanied by interference between the wave forms produced.
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24. DETECTOR
• The light selected by the monochromator is directed
onto a detector that is typically a photomultiplier tube ,
whose function is to convert the light signal into an
electrical signal proportional to the light intensity.
• The processing of electrical signal is fulfilled by a signal
amplifier . The signal could be displayed for readout , or
further fed into a data station for printout by the
requested format.
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26. CalibrationCurve
• A calibration curve is used to determine the unknown
concentration of an element in a solution.
• The instrument is calibrated using several solutions of known
concentrations.
• The absorbance of each known solution is measured and then
a calibration curve of concentration vs absorbance is plotted.
• The sample solution is fed into the instrument, and the
absorbance of the element in this solution is measured.
• The unknown concentration of the element is then calculated
from the calibration curve 22
28. Spectral interferences
•Spectral overlap
(+ positive analytical error)
Cu 324.754 nm, Eu 324.753 nm
Al 308.215 nm , V 308.211nm,
Al 309.27 nm
Avoid the interference by observing the
aluminum line at 309.27 nm
29. • non-absorption line
• molecular absorption(+)
Combustion products (the fuel and oxidant mixture)
Correct by making absorption measurements while a
blank is aspirated into the flame.
30. •light scatter (+)
The interference can be avoided by variation in
analytical variables, such as -
•flame temperature and fuel-to –oxidant ratio
•Standard addition method
•Zeeman background correction
31. Chemical interferences
----- Formation of compound of low volatility due to
incomplete dissociation into atoms
•Increase in flame temperature
•Use of releasing agents (La 3+ )
•Use of protective agents (EDTA)
•Separation
34. Applications
1) Presence of metals as an impurity or in alloys could be done
easily
2) Level of metals could be detected in tissue samples like
Aluminum in blood and Copper in brain tissues
3) Due to wear and tear there are different sorts of metals
which are given in the lubrication oils which could be
determined for the analysis of conditions of machines
4) Determination of elements in the agricultural and food
products
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35. References:
•Vogel’s Textbookof Quantitative Analysis,G.Svehla,Pearson.
•Principles of Instrumental Analysis, Skoog.
•Basic Concepts Of Analytical chemistry,SMKhopkar.
•Instrumental Methods of chemical Analysis by G. Chatwal & S. Anand.