Atomic Absorption Spectrometry

ATOMIC ABSORPTION SPECTROMETRY
Presented By:
1. Waleed Ejaz 2. Muhammad Zubair Idrees 4. Muhammad Usman Saeed
Atomic Absorption Spectrometry (AAS)

Atomic absorption spectrometry (AAS) is an analytical technique that measures the concentrations of elements. Atomic absorption is so sensitive that it can measure down to parts per billion of a gram in a sample. The technique makes use of the wavelengths of light specifically absorbed by an element. The analyte concentration is determined from the amount of absorption. Atomic spectroscopy is used for the qualitative and quantitative determination of perhaps 70 elements.
Atomic Absorption Spectrometer
HISTORY
The phenomenon of atomic absorption (AA) was first observed in 1802 with the discovery of the Fraunhofer lines in the sun's spectrum. It was not until 1955 however that Walsch proposed that atomic absorption be used for quantitative chemical analysis. So we can say that AAS was founded by Allen Walsch from Australia in 1955.
Basic Principle of AAS

The technique makes use of absorption spectrometry to assess the concentration of an analyte in a sample. It relies therefore heavily on Beer-Lambert law. In short, the electrons of the atoms in the atomizer can be promoted to higher orbitals for a short amount of time by absorbing a set quantity of energy (i.e. light of a given wavelength). This amount of energy (or wavelength) is specific to a particular electron transition in a particular element, and in general, each wavelength corresponds to only one element. This gives the technique its elemental selectivity.
HOW IT WORKS
Atoms of different elements absorb characteristic wavelengths of light. Analyzing a sample to see if it contains a particular element means using light from that element.
INSTRUMENTATION
Atomic-absorption (AA) spectroscopy uses the absorption of light to measure the concentration of gas-phase atoms. Since samples are usually liquids or solids, the analyte atoms or ions must be vaporized in a flame or graphite furnace. The atoms present in flame absorb ultraviolet or visible light and make transitions to higher electronic energy levels. The analyte concentration is determined from the amount of absorption.
INSTRUMENTATION (Cont.)
Applying the Beer-Lambert law directly in AA spectroscopy is difficult due to variations in the atomization efficiency from the sample matrix, and nonuniformity of concentration and path length of analyte atoms (in graphite furnace AA). Concentration measurements are usually determined from a working curve after calibrating the instrument with standards of known concentration.
INSTRUMENTATION (Cont.)
1. Light source Hollow Cathode Lamp Diode lasers 2. Atomizer Flame Atomizers Electrothermal Atomizer (Graphite Furnace) 3. Light separation and detection Monochromator Photomultiplier Tube (PMT)
Schematic Of An Atomic-Absorption Experiment
1. Light source
The light source is usually a hollow-cathode lamp of the element that is being measured. Lasers are also used in research instruments. Since lasers are intense enough to excite atoms to higher energy levels, they allow AA and atomic fluorescence measurements in a single instrument. The disadvantage of these narrow-band light sources is that only one element is measurable at a time.
1. Hollow Cathode Lamp

Hollow cathode lamps are used as the light source for AA measurements. The majority of HCLs are single element lamps with the hollow cathode coated with the desired element. The lamps are generally filled with neon under reduced pressure (1-5 torr), are operated at a few hundred volts (150 - 400 volts) and require currents anywhere from approximately 3 - 25 mA. When a neon filled tube is operating the hole in the cathode has an orange glow due to Ne emission.
1. Hollow Cathode Lamp (Cont.)
2. Diode lasers:
Atomic absorption spectroscopy can also be performed by lasers, primarily diode lasers because of their good properties for laser absorption spectrometry. The technique is then either referred to as diode laser atomic absorption spectrometry (DLAAS or DLAS) or, since wavelength modulation most often is employed, wavelength modulation absorption spectrometry.
ATOMIZATION
A process by which the sample is converted into an atomic vapour.
Processes occurring during atomization
Source: Skoog, Holler, and Nieman, Principles of Instrumental Analysis, 5th edition, Saunders College Publishing.
Liquid samples introduced to atomizer through a nebulizer
Pneumatic nebulizer
Ultrasonic-Shear Nebulizer
1-Types of Flames
H-C|C-H Fuel / Oxidant acetylene / air acetylene / N2O acetylene / O2 Temperature 2100 C 2400 C (most common) 2600 C 2800 C 3050 C 3150 C
Selection of flame type depends on the volatilization temperature of the atom of interest. interest.
2-Flame Structure
Interzonal region is the hottest part of the flame and best for atomic absorption. Fuel rich flames are best for atoms because the likelihood of oxidation of the atoms is reduced. Oxidation of the atoms occurs in the secondary combustion zone where the atoms will form molecular oxides and are dispersed into the surroundings.
3- Temperature Profiles
It is important to focus the entrance slit of the monochromator on the same part of the flame for all calibration and sample measurements. measurements.
4- Flame Absorption Profiles

Mg - atomized by longer exposure to flame, but is eventually oxidized. oxidized. Ag - slow to oxidize, the number of atoms increases with flame height. height. Cr - oxidizes readily, highest concentration of atoms at the base of the flame. flame.
Types of Atomizers
Flame Atomizer Electrothermal Atomizer
FLAME ATOMIZERS
Total consumption burner: Separate channels bring sample, fuel, and oxidant to combustion area. All of the sample, that is carried into the burner, is burned; Sensitivity is greater than in a burner where the sample is not completely burned. extra turbulence in the flame from variations in droplet size increase noise.
Premix (laminar flow) burner

Sample, fuel, and oxidant mixed prior to entering flame. Turbulence drastically reduced by removing larger droplets. Mixing baffles insure only fine mist makes it through to burner.
Laminar Flow Burners

Sample is pulled into the nebulization chamber by the flow of
fuel and oxidant.

Contains
spoilers (baffles) to allow only the finest droplets to reach the burner head. head.
Burner head has a long
path length and is ideal for atomic absorption spectroscopy. spectroscopy.
Electrothermal Atomization
0.5-10 QL of sample evaporated at low temperature, then ashed at higher temperature in electrically heated graphite furnace. Finally, current rapidly increased causing temperature increase (to 2000-3000 C) and rapid atomization. Usually used only when flame or plasma atomization provides inadequate detection limits.
Light Separation And Detection

AA spectrometers use monochromators and detectors for uv and visible light. The main purpose of the monochromator is to isolate the absorption line from background light due to interferences. Simple dedicated AA instruments often replace the monochromator with a band pass interference filter. Photomultiplier tubes are the most common detectors for AA spectroscopy.
1. Monochromator
The monochromator is placed between the graphite furnace and the detector and is used to isolate the wavelength of interest and reduce background interference.
2. Photomultiplier Tube (PMT)

Photomultiplier Tubes (PMTS) are light detectors that are useful in low intensity applications such as fluorescence spectroscopy. Due to high internal gain, PMTs are very sensitive detectors. PMTs are similar to phototubes. They consist of a photocathode and a series of dynodes in an evacuated glass enclosure. Photons that strikes the photoemissive cathode emits electrons due to the photoelectric effect. Instead of collecting these few electrons (there should not be a lot, since the primarily use for PMT is for verly low signal) at an anode like in the phototubes, the electrons are accelerated towards a series of additional electrodes called dynodes.
2. Photomultiplier Tube (PMT) (Cont.)

These electrodes are each maintained at a more positive potential. Additional electrons are generated at each dynode. This cascading effect creates 105 to 107 electrons for each photon hitting the first cathode depending on the number of dynodes and the accelerating voltage. This amplified signal is finally collected at the anode where it can be measured.
Applications Of Atomic Absorption Spectrometry

Atomic absorption spectrometry has many uses in different areas of chemistry. 1. Clinical analysis: Analysing metals in biological fluids such as blood and urine. 2. Environmental analysis: Monitoring our environment e.g. finding out the levels of various elements in rivers, seawater, drinking water, air, petrol and drinks such as wine, beer and fruit drinks. 3. Pharmaceuticals: In some pharmaceutical manufacturing processes, minute quantities of a catalyst used in the process (usually a metal) are sometimes present in the final product. By using AAS the amount of catalyst present can be determined.
Applications Of Atomic Absorption Spectrometry (Cont.)

4. Industry: Many raw materials are examined and AAS is widely used to check that the major elements are present and that toxic impurities are lower thanspecified eg in concrete, where calcium is a major constituent, the lead level should be low because it is toxic. 5. Mining: By using AAS the amount of metals such as gold in rocks can be determined to see whether it is worth mining the rocks to extract the gold.
Use of AAS for the Quantitative Determination of Metallic Impurities in Pure Uranium Compounds
Atomic Absorption Spectrometry is used for the Quantitative Determination of Metallic Impurities in Pure Uranium Compounds. Several elements (V, Mo, Fe, Mn, Cd, Zn) as metallic impurities in pure uranium compounds were quantitatively determined by atomic absorption spectrometry. The effects of uranium and that of other factors on the absorption intensity of each element were studied. The analyzed samples were dissolved in 6 M nitric acid, and uranium was selectively extracted with tributylphosphate. The aqueous solution containing impurities was then evaporated and thus these impurities are obtained
REFERENCES
www.anachemumu.se.htm www.aurora-instr.com/right.htm www.anachem.umu.se/jumpstation.htm www.anachem.umu.se/cgi/AtomicSpectroscopy www.anachem.umu.se/cgi/Spectroscopy www.minyos.its.rmit.edu.au/rcmfa/mstheory.html
HOPE U HAVE NO QUESTION.
THANK YOU
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Atomic Absorption Spectrometry

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ATOMIC ABSORPTION SPECTROMETRY

Atomic Absorption Spectrometry (AAS)

Atomic Absorption Spectrometer

Basic Principle of AAS

Schematic Of An Atomic-Absorption Experiment

1. Hollow Cathode Lamp

1. Hollow Cathode Lamp (Cont.)

A process by which the sample is converted into an atomic vapour.

Processes occurring during atomization

Liquid samples introduced to atomizer through a nebulizer

4- Flame Absorption Profiles

Premix (laminar flow) burner

Laminar Flow Burners

fuel and oxidant.

Burner head has a long

path length and is ideal for atomic absorption spectroscopy. spectroscopy.

Light Separation And Detection

2. Photomultiplier Tube (PMT)

2. Photomultiplier Tube (PMT) (Cont.)

Applications Of Atomic Absorption Spectrometry

Applications Of Atomic Absorption Spectrometry (Cont.)

HOPE U HAVE NO QUESTION.

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