Atomic Absorption Spectroscopy - Principles and Applications

Atomic absorption spectroscopy Introduction Atomic Absorption Spectroscopy is a very common technique for detecting metals and metalloids in samples It is very reliable and simple to use. It can analyze over 62 elements. It also measures the concentration of metals in the sample. History The first...

Atomic absorption spectroscopy Introduction Atomic Absorption Spectroscopy is a very common technique for detecting metals and metalloids in samples It is very reliable and simple to use. It can analyze over 62 elements. It also measures the concentration of metals in the sample. History The first atomic absorption spectrometer was built by CSIRO scientist Alan Walsh in 1954. Elements detectable by atomic absorption are highlighted in pink in this periodic table 1 Principle of atomic absorption spectroscopy 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 higher electronic energy levels. The analyte concentration is determined from the amount of absorption. Concentration measurements are usually determined from a working curve after calibrating the instrument with standards of known concentration. Advantages of Atomic absorption spectroscopy High sensitivity [10-10g] Good accuracy (Relative error 0.1 ~ 0.5 % ) High selectivity Disadvantage of Atomic absorption spectroscopy A resonance line source is required for each element to be determined 2 Component of the atomic absorption spectrometry 1- Hollow cathode lamps: Hollow Cathode Lamps 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. 3  2- 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. 3- Atomizer Elements to be analyzed needs to be in atomic sate. 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. a- Flame atomizer: To create flame, we need to mix an oxidant gas and a fuel gas. In most of the cases air-acetylene flame or nitrous oxide- acetylene flame is used. Liquid or dissolved samples are typically used with flame atomizer. 4  b- Graphite tube atomizer: uses a graphite coated furnace to vaporize the sample. In 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. 4- Monochromator: This is a very important part in an atomic absorption 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. 5- 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. Calibration Curve 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 versus 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. 5 Applications: Determination of even small amounts of metals (lead, mercury, calcium, magnesium, etc) as follows: Environmental studies: drinking water, ocean water, soil. Food industry. Pharmaceutical industry. Determination of lead in contaminated soil: 1- Sampling: Samples of approximately 50g should be taken from specified sampling points on the site. The sampling point should include surface soil and two further samples taken at depth, at 0.5 and 1.0 m. The exact location of these points should be noted, for it may be necessary to take further samples. 2- Procedure: 6  Weight out about 1g of sieved soil and transfer to a 100 ml beaker. Add 20 ml of 1:1 nitric acid. Boil gently on a hot plate until the volume of nitric acid is reduced to 5 ml. Add 20 ml of deionized water and boil gently again until the volume is 10 ml. Cool the suspension and filter through a whatman filter paper. Wash the beaker and filter paper with deionized water until a volume of about 25 ml is obtained. Transfer the filtrate to a 50 ml flask and make up to the mark with deionized water. Setup acetylene-air flame with resonance line 217 nm. Standard lead solutions containing 1-10 mg ml-1 are suitable for measurement. 7