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[Chemical Engineering Laboratory V]

SEGi University

Atomic Absorption Spectroscopy (AAS)

Group Members Name: Irfan Anhar


Sharvessh Mahaeswarren
Paul Lim
Kelvin Ho
Teng Yong Kang

Lecturer/ Supervisor: Ms. Chan Yi Shee / Dr. Wong Voon Loong


Date of Submission: 9th March 2016
1.0 Abstract

The main purpose of this experiment was to understand the basic operation of the atomic
absorption spectroscopy and to determine the main factors that can affect the absorption
ability of the machine. Moreover to determine the metal concentrations using the calibration
curve method. Five standard calibration solutions were prepared with different linearity
concentration and one distilled water as a blank solution was prepared as well. Then, the
solutions all were run together including the unknown concentration sample for the analysis
of the atomic absorption spectroscopy. Based on the data obtained, an increasing linear graph
can be plotted comparing the concentration of the metals against the amount of radiation
absorbed. The linear graph produced an equation of y=0.0614x 0.029 with a R 2 value of
0.99786 reflecting a high linear correlation.
2.0 Introduction

Atomic absorption spectroscopy (AAS) can be defined as a spectroanalytical method for the
quantitative determination of chemical elements by the absorption of optical radiation by free
atoms in gaseous state. This atomic absorption technique is very sensitive because it has the
capability to measure down to parts per billion of a gram (g dm -1) in a sample. The
wavelengths of light are specifically absorb from an element that was used during the test.
The wavelengths of light responds to the amount of energies required to stimulate the
electrons from a particular energy level to a different level. In specific would be a lower
energy level to a higher energy level.

This atomic absorption spectrometry technique is used in many different fields such as
clinical analysis, environmental analysis, pharmaceuticals and mining industries. For the
clinical analysis, it can be used to determine the metals present in any organic fluids like
urine and blood. Besides that, in the environment matters, the contents of elements contained
in rivers, air, petrol and any types of drinking fluids such as beer, fruit drinks and even water
can be found. As for the pharmaceutical field, this method can be used in the manufacturing
processes to measure the small amounts of catalyst present in the final product. For any
industries, the levels of toxic or any other impurities can be determine and in mining industry,
in order to save cost, the rocks are first scanned to determine the levels of gold presents. If the
gold levels are high, then it is worth it to be mined.

The substance has to be atomized before analysing it for its atomic contents. Normally flames
and electro thermal atomizers are used to analyse the fluids. Some of the atomizers like glow-
discharge, hydride and cold-vapor are only used for special cases only. The atoms are
exposed to slight radiation by optical radiation and the source of radiation would be a
continuum radiation source or an element specific line radiation source. The radiation will
pass through a monochromator which would then separate the element-specific radiation
from other radiation sources emitted and lastly measured by a detector present. The higher the
number of atoms in the vapour, the more radiation is absorbed.

A calibration curve can be plotted by testing several samples of known substances


concentration with the same conditions with the unknown substance. The standards amount
absorbed is compared with the plotted curve and the unknown substance concentration can be
calculated. The atomic absorption spectrometer basically needs three components such as a
light source, a sample and a way to measure the specific light absorbed. The light source can
be a hollow cathode lamp which contains tungsten anode and a cylindrical hollow cathode
made of substance that needed to be found.

During this absorption process, atoms and molecules from the substance apart from the
element that needed to be found can be absorbed or scatter slight radiation from the light
source. Those elements are able to bond with the metals that needed to be analysed and
affecting the absorption process of the wanted element. In order to avoid this from happening,
two light sources should be used. One light source should be the hollow lamp cathode
whereas the other one would be a deuterium lamp. This would help to obtain an accurate
result. The main absorption would be measured by using the main light source and the
secondary absorption would be measured by the deuterium lamp. The difference in the values
from the total absorption from the secondary absorption would provide absorption from the
main element only.

Calibration curve would be plotted in order to determine the unknown concentration of the
element. The machine would be standardised using a few solutions with concentration levels
known. A curve then can be plotted which it then slowly rescaled as the concentration
increases. The radiation rate would increase as the concentration of the solution increases.
Figure 2.1 shows a sample of calibration curve of concentration against the amount of
radiation absorbed.
Concentration vs Amount of radiation absorbed
7

4
Amount of radiation absorbed 3

0
0 2 4 6

Concentration

Figure 2.1: Sample calibration curve of concentration against amount of radiation absorbed

At times slight deviations are possible to take place due to the difference in the solution
concentration, unabsorbed radiation, decompositions of certain solution at high
concentrations. The graph with slight curve cannot be avoided but is able to be minimized.
Minimum five solutions should be prepared to be tested and an unknown concentration
solution in order to fit the criteria of the graph. Consistency can be maintained if the five
solutions rule and the unknown concentration solution method are practiced. Figure 2.1 the
curved line shows the slight deviation of the graph.

3.0 Experimental Method

3.1 Apparatus

1. 100 mL volumetric flask


2. 50 mL volumetric flask
3. 10 mL beaker
4. 50 mL beaker
5. 10 mL pipette
6. 5 mL pipette
7. Pipette filter
8. Copper (II) sulphate
9. Iron (II) nitrate
10. Lead (II) nitrate
11. Cadmium (II) nitrate
12. Unknown sample

3.2 Procedures

3.2.1 Preparation of standard calibration solution

1. 100 ppm solution was diluted into different range of concentration base on the
linearity of metal.

Table 3.3: Linearity concentration of heavy metal for AAS analysis.


Heavy metal Linearity concentration, ppm
Copper 2,4,6,8,10
Lead 2,4,6,8,10
Iron 2,4,6,8,10
Cadmium 2,4,6,8,10

3.2.2 Dilution

1. 50 mL of 1000 ppm Cu2+, Pb2+, Fe2+, and Cd2+ standard solution was poured into a
beaker and 1000 ppm standard solution was diluted to 100 ppm for each metal.

M1V1=M2V2

M1: initial concentration in ppm

V1: initial volume in mL (volume of solution required)

M2: final concentration in ppm

V2: final volume in mL (volume of volumetric flask)

3.2.3 Analysis of calibration solution by AAS.


1. Five standards calibration solutions were prepared covering range from Table 3.3.

2. Distilled water was prepared as blank solution. (reference solution)

3. Analysis of AAs was conducted by the lecturer.

4. An unknown solution was given. Firstly, all the standard calibrations were ran and
the unknown sample were ran

5. Analysis process for the experiment was triplicated.

6. The step of the whole analysis was recorded.

7. The data of analysis was obtained and the standard solution curve was plotted.
From the standard calibration curve, the percentage of heavy metal ions present in
the unknown sample was calculated.
4.0 Results & Tabulations

Table 4.1: Preparation of Sample

Sample Stock Stock Diluted Diluted


Concentratio Volume of concentratio Volume of
n of Copper Copper n of Copper Copper
(ppm) (ml) (ppm) (ml)
1 100 0.8 2 40
2 100 1.6 4 40
3 100 2.0 5 40
4 100 2.4 6 40
5 100 4.0 10 40

m1 v 1=m 2 v 2
Standard dilution formula of is used to prepare the dilute sample of various

concentration. For sample 1, a concentration of 2 ppm is needed; hence to calculate the


volume of the stock concentration to be used, the aforementioned formula is used.

m1 v 1=m2 v 2

100 v 1=2 40

v 1=0.8 ml

0.8 ml of the stock concentration is added to sample 1 test tube with the rest of the volume is
made up by distilled water.
Table 4.2: Result obtained

Concentratio Absorbanc
n e
0 -0.0258
2 0.0813
4 0.2266
6 0.3445
8 0.4566
Unknown 0.1028

Absorbance versus Concentration of Copper


0.5

f(x) = 0.06x - 0.03


0.4 R = 1

0.3

Absorbance 0.2

0.1

0
0 1 2 3 4 5 6 7 8 9

-0.1

Concentration (ppm)

Figure 4.1: Relationship of absorbance and concentration of Copper


5.0 Discussions

The aim of the experiment is to analyze sample and come out with a conclusion of the
concentration of the specific heavy metal by comparing it with a calibration curve of the
specific heavy metal. In this experiment, Copper was selected as the test subject. The
concentration of copper in a sample is to be determined at the end of the experiment.

To assist in testing the sample, a range of known concentration of copper sample is prepared.
Copper concentration from 2 ppm to 10 ppm is prepared as shown in Table 4.1. The sample is
prepared from a stock solution in a beaker. Marginal human error could occur and affect the
result, however, this error would be insignificant, as the parallax error would only lead to
overshoot of material by a minimal percentage.

The known sample is then tested in the atomic absorption spectroscopy machinery to produce
a calibration curve. The calibration curve is as shown in Figure 4.1. From the graph, it could
be seen that the absorbance and concentration of copper produce a linear relationship. The
regression analysis is also high at 0.99786, which further justify the aforementioned linear
relationship.

6.0 Conclusions

It can be deduced that the absorbance of a heavy metal is directly proportional to the
concentration of atomic vapor in the flame. However, since the experiment was only
conducted at concentration of 10 ppm and lower, the relationship might differ at higher
concentration of heavy metal in a sample.
7.0 Reference

1. Elena Sevostianova. 2010. Atomic absorption spectrometry. [ONLINE] Available


at:http://web.nmsu.edu/~esevosti/report.htm. [Accessed 04 March 16].

2. R.Levinson. 2015. Atomic absorption spectrometry. [ONLINE] Available at:


http://faculty.rmu.edu/~short/chem3550/chem3550-references/RSC-AA-Leaflet.pdf.
[Accessed 04 March 16].

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