Henry Su

Lab Experiment #4
9-1

May 8, 2003
CHE 331
Dr. Rahni

Evaluation of Analytical Parameters in Atomic Absorption Spectroscopy

Purpose
The purpose of this laboratory experiment is to examine the factors which affect the free
atom concentrations in atomic absorption spectroscopy, such as the analytical results (flame
temperature, aspiration rate, solvent, chemical form of the element, height of observation in the
flame, type of burner and nebulizer, fuel to oxidant ratio of the flame, and the degree of ionization
of the element in the flame).
Theory
Atomic absorption spectrometers (AA) use the absorption of light to measure the
concentration of gas-phase atoms. The analyte (usually liquids or solids) must be vaporized in a
flame or a graphite furnace (temperature of 1000-2000 K). 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. The spectra of atoms in gaseous phase consist of very
sharp lines, therefore this technique has a high sensitivity and it is easy to examine many samples.
Graphite furnace atomic absorption spectroscopy is useful when the amount of sample is very
small, when very low levels of detection are required, and when the matrix is dilute or volatile.
This technique can also be used for direct analysis of solid sample.
To analyze a sample by atomic absorption, it must be heated to high temperatures, done
mostly by flame. After the solvent evaporates, the flame dissociates chemical bonds, releasing free
metal atoms that absorbs light characteristic of the individual elements. The wavelengths
absorbed by each element are narrow and unique.
The light source for the atomic absorption spectrum are required to produce a narrow
band of adequate intensity and stability for prolonged periods of time. In order for the mechanism

to follow Beers law, a source of radiation emitting a line of the same wavelength as that which is
used for an absorption analysis. It must also be for excited state atomic lines of the element.
Hollow-cathode tubs are used in order to make this possible, and are constructed from the
elements of interest.
A critical part of atomic absorption spectroscopy is the introduction of the sample into the
flame and its vaporization and atomization to ground state atoms. Any method resulting in a
reproducible cloud of ground state atoms in the light path

Apparatus
The following materials will be needed in order to perform this experiment:

Material
Recording Atomic Absorption
Spectrophotometer and Accessories
Hollow cathode lamps, Cu, Zn, Ca
Compressed Air, Nitrous Oxide, Acetylene
Pipets
Volumetric Flasks
Beakers
Separatory funnels

Quantity

2 each of 10, 25, and 50 ml

4 each of 100 and 1000 ml
5 of 100 ml
4 of 250 ml

Reagents
Solution
Cupric Sulfate
Magnesium Chloride
Stannous Chloride
Manganous Chloride
Ethanol
Methyl Isobutylketone

Please See Lab on Disk.

Concentration(s)