Analytical Chemistry Laboratory 2

Atomic Absorption Spectroscopy Measurement
Mr. *****
Department of Chemical Engineering and Chemistry, Mapua Institute of Technology

The effects of instrumental parameters on calcium absorption are studied. The calcium sample in its pure form was determined by comparing the absorbance with that of standards. The concentration calculated by linear regression was 19.35 ppm for an absorbance of 0.459 for sample number 3. The calibration curve revealed by the computer was in linear form. The analyte to be examined is calcium. The metal is obtained mainly by electrolysis of fused calcium chloride, a costly process. Until recently the pure metal had little use in industry. It is being used to an increasing extent, however, as a deoxidizer for copper, nickel, and stainless steel. Because calcium hardens lead when alloyed with it, lead-calcium alloys are excellent for bearings, superior to ordinary lead antimony for grids in storage batteries, and more durable as sheathing for leadcovered cable. Calcium is present in the chemically combined state in lime (calcium hydroxide), cement and mortar (as calcium hydroxide or a variety of silicates of calcium), teeth and bones (as a calcium hydroxyphosphate), and in many body fluids (as complex proteinaceous compounds) essential to muscle contraction, the transmission of nerve impulses, and the clotting of blood. Methodology 500 mL of 50 ppm stock solution of Ca2+ primary standard was prepared. Preparation was made with 50 mL standards from the stock solution corresponding to 5 ppm, 15 ppm, and 30 ppm concentrations. The pH of the standards was adjusted to the pH of the sample. The solution was filtered.

Objective The purpose of this experiment is to familiarize the principles and operation of the Atomic Absorption Spectrophotometer (AAS), and to determine the concentration of calcium in a sample using AAS. Discussion Overview Atomic Absorption 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 absorb ultraviolet or visible light and make transitions to higher electronic energy levels. The analyte concentration is determined from the amount of absorption. 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.

The standards and the sample were aspirated using the required instrument parameters for calcium (Ca) of the Perkin Elmer AAAnalsyt 100 Spectrophotometer. The K content (concentration) of the sample was then calculated. Instrumentation
Schematic of an atomic-absorption experiment:

Interpretation The sample solution is aspirated into a flame and the sample element which is calcium is converted to atomic vapor. The flame then contains the calcium atoms. Some are thermally excited by the flame, but most remain in the ground state. These ground-state atoms can absorb radiation of a particular wavelength that is produced by a special source made from that element. The wavelengths of radiation given off by the source are the same as those absorbed the atoms in the flame. Here are the absorbance from the experimental data, including the unknown sample:
Concentration 1 ppm 5 ppm 15 ppm 30 ppm Unknown Absorbance 0.018 0.098 0.333 0.733 0.459

Light source The light source is usually a hollowcathode lamp of the element that is being measured. Since lasers are intense enough to excite atoms to higher energy levels, they allow AA and atomic fluorescence measurements in a single instrument. Atomizer AA spectroscopy requires that the analyte atoms be in the gas phase. Ions or atoms in a sample must undergo desolvation and vaporization in a high-temperature source such as a flame or graphite furnace. Flame AA can only analyze solutions, while graphite furnace AA can accept solutions, slurries, or solid samples. Light separation and detection AAS 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.
Picture of a flame atomic-absorption spectrometer

The absorbtion follows Beer’s law. That is, the absorbance is directly proportional to the pathlength in the flame and to the concentration of atomic vapor in the flame. The read-out computer prepared a calibration curve of concentration in the solution versus absorbance. From this curve, as it is a straight line, the unknown sample #3 computed was 19.35 ppm by linear regression. Conclusion AA specophotometry uses a flame as the atomizer and follows Beer’s law. The major disadvantage of making measurements by atomic absorption is that a different source is required for each element. The concentration of the sample was 19.35 ppm according to the read-out. References

1. Christian, G.D., Analytical Chemistry, 6th edition, New Jersey, John Wiley, 2004. 2. Skoog, D. A., and Leary, J. J., Principles of Instrumental Analysis, 4th edition, Saunders, New York 1992. 3. Harris, D.C., Quantitative Chemical Analysis, 3rd edition, Freeman, New York, 1991. 4. © 1993-2003 Microsoft Corporation. All rights reserved.

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