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SUMMARY OF ATOMIC ABSORPTION SPECTROSCOPY (AAS) A) Instruments 1. Used for qualitative identification and quantitative of atoms. 2.

Atomic absorption spectrophotometers used single beam or double beam optics. 3. Involved process of atomization. It is a process of converting the analyte into a free atom. For example, converting an analyte in solid liquid to a free gaseous atom. 4. 2 general methods of atomization: 1) Flame atomization 2) Electrothermal atomization

1) Flame atomizers: a) Sample is converted into a fine mist (small droplets solution). b) Accomplished using a nebulizer. c) Sample is aspirated into a spray chamber by passing a high-pressure stream (combustion gases) until it past the end of capillary tube. d) The impact of the sample with the glass impact bead produces an aerosol mist. e) The aerosol mist mix with the combustion gases in the spray chamber before passing the burner where the flames thermal energy desolvates the aerosol mist to solid particles. f) Thermal energy volatilizes the particles to ionic species and free atoms.

Advantage: a) Reproducibility


a) Efficiency is quite poor.

2) Electrothermal atomizers: a) For improvement in sensitivity used resistive heating in place of a flame. b) Known a s graphite furnace c) Consists of a cylindrical graphite tube. d) A power supply is used to pass a current through the graphite tube, resulting in resistive heating. e) Sample is injected into the graphite tube. f) Atomization is achieved in three stages:

First stage: i) The sample is dried using a current. (raises the temperature of the graphite tube to about 110c). Desolvation leaves the sample as a solid residue.

Second stage: i) ii) Called as ashing. The temperature is increased to 350-1200c, where any organic material in the sample is converted to CO2 and H2O and volatile inorganic materials are vaporized. The gases are removed by the inert gas flow.


Third (final) stage: i) ii) iii) Take time about 45-90 s. (time used for drying and ashing the sample). The sample is atomized by increasing the temperature to 20003000c. The result is a transient absorbance peak whose height or area is propotional to the absolute amount of analyte.

Advantages: i) ii) iii) Improvement in sensitivity. The analytes concentration resulting vapor phase may be as much a 1000 times greater than flame atomization. Improvement in detection limits.

B) Quantitative applications: 1) Analyze trace metals. 2) Example: zinc (zn) in water, wastewater, air, blood, urine, muscle tissue, hair, milk, breakfast cereals, shampoos, alloys, industrial platting baths, gasoline, oil, sediments and rocks. 3) Several considerations are required in using atomic absorption method: i) Choose the method of atomization ii) Selecting the wavelength Iii) Preparing the sample of analysis iv) Minimizing spectral and chemical interferences v) Selecting method of standardization.


Choose the method of atomization

Flame or electrothermal atomization: 1) It depends on the analytes concentration. 2) Usually used electrothermal atomization because of its greater sensitivity and detection limits. 3) Electrothermal is used for the analytes concentration lower than detection limits of flame. 4) Electrothermal also will be used when the volume of the sample is limited. 5) While flame is used when the analytes concentration is greater than detection limit of electrothermal.

For more information of detection limits between both methods, refer table 10.10 ,page 417, modern analytical chemistry book.


Selecting the wavelength

1) Based on the concentration of the analytes. Refer table 10.11 page 418. 2) It also being selected if the wavelength provides the best sensitivity. 3) The wavelength is produce by hollow cathode lamp. 4) In hollow cathode lamp, there are anode and cathode enclosed within a glass tube filled with a low pressure of ne or ar. 5) When a potential is applied across the electrodes, the filler gas is ionized. 6) Positive charge ions collide with negatively charged cathode. 7) It will sputtering atoms from the cathodes surface. 8) The puttered atoms are in excited state emit radiation chracteristics. 9) Thats mean the hollow cathode lamp provides emission lines where we called it as absorption spectrum.

Preparing the sample of analysis 1) The sample must be in liquid. If solid, need to digest it. 2) If the concentration of the sample is high, the sample needs to dilute. Minimizing spectral and chemical interferences Minimizing spectral interferences: 1) It will occurs when an analytes absorption line overlaps with an interferants absorption line. 2) It is because of absorption of radiation by flame. It may scatter the radiation from the source and exhibit broad band absorption. 3) So the most common method used is a continuum source such as D2 lamp. The absorbance of its radiation by the analytes narrow absorption line is negligible. This method called as background correction. Minimizing chemical interferences: 1) The 2 most common chemical interferences are : a) The formation of nonvolatile compounds. Examples: Al3+ and PO43- in Ca2+. It can be minimized by increasing the temperature of flame, adding high concentration of an ionization suppressor.


Selecting method of standardization.

1) Atomic absorption calibration curve must be linear. 2) So it must be set up in computer by analyze the standard solution, where the curve is plotted between absorbance and concentration.