Laboratory 5: Determination of Metal in Samples Using AAS

Laboratory 5: Determination of Metal in Samples Using AAS
1. Introduction
Atomic absorption spectroscopy is a method particularly suited to the measurement of small
amounts of elements, usually metals, in a sample. The element to be determined is dissociated
from its environment so that it exists as free atoms in the ground state. Atoms in this state readily
absorb electromagnetic radiation at wavelengths corresponding to excitation to higher energy
levels. The extent of this energy absorption from a radiation source is measured photometrically
and compared with standard samples containing known amounts of the element. The method is
unusually simple, sensitive, and selective.
In this experiment, the students using AAS before analyse the samples and prepared the standard
solutopns to determined which consists of iron, cadmium, zinc and chromium from the soil
samples (dry ashing) and cockles sample (dry ashing).
2. Equipments/ Chemicals
 Volumetric flask
 Standard solutions
 Micro Pipette
 Nitric
3. Objectives
a) To determine the level of heavy metals in a sample by using Atomic Absorption
Spectrometry (AAS)
b) To study for preparing standard solution before analyzing sample.
c) To study on calibration process by using AAS.
4. Methodology
1. 1% HNO3 was prepared as a diluent for all standard solutions.

2. Four standard solutions was prepared at a volume of 50ml each by using dilution
calculation. (M1V1=M2V2). Refer to the table below.
3. Four solutions was taken and sample to the Atomic Absorption Spectrophotometer for
analysis.
METAL Std 1 Std 2 Std 3 Std 4

Chromium 0.1 0.2 0.5 1.0
5. Result
Parameter Soil sample Cockles Sample

(Wet digestion), mg/l (Dry Ashing), mg/l
Chromium 0.085 0.003
Conversion unit from mg/l to mg/kg

For soil sample:
0.085 mg/L x (100 x 10-3) L / 3 x 10-3 kg
=2.83 mg/kg of chromium
For cockle sample:
0.003 mg/L x (50 x 10-3) L / 3 x 10-3 kg
= 0.05 mg/kg of Chromium
6. Discussion
a) Sample preparation
Sample preparation is often simple, and the chemical form of the element is usually
unimportant. This is because atomisation converts the sample into free atoms irrespective
of its initial state. The sample is weighed and made into a solution by suitable dilution.
When making reference solutions of the element under analysis, for calibration, the
chemical environment of the sample should be matched as closely as possible – ie the
analyte should be in the same compound and the same solvent.
b) Calibration
To analyze the sample by AAS, it must calibrated by doing a calibration curve every each
parameter. Calibration Curve Method Prepare standard solutions of at least three different
concentrations, measure the absorbances of these standard solutions, and prepare a
calibration curve from the obtained values. Then measure the absorbance for the test
solution adjusted in concentration to a measurable range, and determine the amount
(concentration) of the object element from the calibration curve.
c) Standard of Chromium
Based on the results obtained through the experiments that has been conducted, the
chromium reading for the soil sample were in the acceptable conditions that is 2.83
mg/kg. By referring to Contaminated Land Management and Control Guidelines No 1:
Malaysian Recommended Site Screening Levels for Contaminated Land, Typical Range
of Natural Occuring Metals Concentration, and the level for Chromium is 14.40 mg/kg.
Thus, chromium level for soil sample comply with the standard.
Malaysian Food Act 1983 and Regulation 1985 and WHO/FAO 2004 did not set any
limit for Cr bivalves. However, IAEA – 407 was reported that a permitted level for Cr in
the marine organism is 0.73 mg/kg base on this permitted limit level the sample is
comply with the standard that is 0.05 mg/kg.
Conclusion
Atomic absorption spectroscopy (AAS) is a spectroanalytical procedure for the
quantitative determination of chemical elements using the absorption of optical radiation
(light) by free atoms in the gaseous state.Atomic absorption spectrometry has many uses
in different areas of chemistry such as:
a) Clinical analysis: Analyzing metals in biological fluids and tissues such as whole
blood, plasma, urine, saliva, brain tissue, liver, muscle tissue, semen
b) Pharmaceuticals: In some pharmaceutical manufacturing processes, minute quantities

of a catalyst that remain in the final drug product
c) Water analysis: Analyzing water for its metal content.

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Laboratory 5: Determination of Metal in Samples Using AAS

1. 1% HNO3 was prepared as a diluent for all standard solutions.

METAL Std 1 Std 2 Std 3 Std 4

Parameter Soil sample Cockles Sample

Conversion unit from mg/l to mg/kg

b) Pharmaceuticals: In some pharmaceutical manufacturing processes, minute quantities

c) Water analysis: Analyzing water for its metal content.

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