NAME : MANDISA

SURNAME : DONCABE
STUDENT NUMBER : 219072980
DATE : 14 April 2021
PRACTICAL NUMBER: 05
MODULE : INSTRUMENTAL ANALYSIS

ATOMIC ABSORPTION
SPECTROMETRY (AAS)
AIM
The aim of this experiment was to analyse barium using Atomic Emission Spectroscopy
(AES) to examine the effect of ionisation and the use of a buffer and to determine the amount
of metallic element (manganese) present in multivitamin tablets using Atomic Absorption
Spectroscopy (AAS).
INTRODUCTION
Manganese is a trace mineral that is present in small amounts in the body. It is found mostly
in bones, the liver, kidneys, and pancreas. Manganese helps the body form connective tissue,
bones, and blood clotting. It also plays a role in fat and carbohydrate metabolism, calcium
absorption, and blood sugar regulation. Manganese is also necessary for normal brain and
nerve function. It provide antioxidant which helps to fight free radicals. Free radicals occur
naturally in the body but can damage cell membranes and DNA [1].
Low levels of manganese in the body can contribute to infertility, bone malformation,
weakness, and seizures. However, high levels of manganese in the body can cause anemia,
reproductive issues, slowed growth, and loss of appetite. In this experiment the amount of
manganese in multivitamin tablet is determined by using Atomic Absorption Spectroscopy
(AAS).
Atomic Absorption Spectroscopy (AAS) is a technique for measuring the concentrations of
metallic elements in different materials, it uses electromagnetic wavelengths coming from a
light source. Any atom has its own distinct pattern of wavelength at which it will absorb
energy, due to the unique configuration in its outer shell. This allows for the qualitative
analysis of a pure sample [2]. The amount of manganese is then calculated using calibration
curve and absorbance of a sample.
PRINCIPLE
Atomic absorption analysis involves measuring the absorption of light by vaporized ground
state atoms and relating the absorption to concentration. The incident light beam is attenuated
by atomic vapor absorption according to Beer’s law. The process of atomic absorption
spectroscopy involves two steps which are atomization of the sample and the absorption of
radiation from a light source by the free atoms. The sample either a liquid or a solid is
atomized in either a flame or a graphite furnace. Upon absorption of ultraviolet or visible
light, the free atoms undergo electronic transitions from the ground state to excited electronic
states [3].
To obtain the accurate results in AAS, the instrumental and chemical parameters of the
system must be geared toward the production of neutral ground state atoms of the element of
interest. A common method is to introduce a liquid sample into a flame. Upon introduction
the sample solution is dispersed into a fine spray, the spray is then desolvated into salt
particles in the flame and the particles are subsequently vaporized into neutral atoms, ionic
species and molecular species.
All of these conversion process occur in geometrically definable regions in the flame. It
therefore important to set instrument parameters such that the light from source, typically a
hallow-cathode lamp, is directed though the region of the flame that contains the maximum
number of neutral atoms [4].
The light produced by the hallow-cathode lamp is emitted from excited atoms of the same
element which is to be determined. Therefore, the radiant energy corresponds directly to the
wavelength which is absorbable by the atomized sample. This method provides both
sensitivity and selectivity since other elements in the sample will not generally absorb the
chosen wavelength and thus will not interfere with the measurement. To reduce background
interference, the wavelength of interest is isolated by a monochromator placed between the
sample and the detector [5].
There are two methods of adding thermal energy to a sample, a graphite furnace AAS uses a
graphite tube with a strong electric current to heat the sample. In the flame AAS, we aspirate
a sample into a flame using a nebulizer. The flame is lined up in a beam of light of the
appropriate wavelength. The flame, thermal energy, causes the atom to undergo a transition
from the ground state to the first excited state. When the atoms make their transition, they
absorb some of the light from beam. The more concentrated the solution, the more light
energy is absorbed [6].
The light beam is generated by lamp that is specific for a target metal. The lamp must be
perfectly aligned so the beam crosses the hottest part of the flame. The light passed through
the flame is received by the monochromator, which is set to accept and transmit radiation at
the specified wavelength and travels into the detector. The detector measures the intensity of
the beam of light. When some of the light is absorbed by metal, the beam’s intensity is
reduced. The detector records that reduction as absorption. That absorption is shown on
output device by the data system.
We can find the concentration of metals in a sample running a series of calibration standards
through the instrument. The instrument will record the absorption generated by a given
concentration. By plotting the absorption versus the concentrations of the standards, a
calibration curve can be plotted. We can then look at the absorption for a sample solution and
use the calibration curves to determine the concentration of metal[7].

figure 2: Atomic Absorption Spectroscopy

AAS is a great method of producing accurate results. AAS advantages includes high
sensitivity, precision over the classical gravimetric methods, relatively inexpensive, easy to
use and low element detection limits.
ABSTRACT

The purpose of this experiment was to analyse barium by Atomic Emission Spectroscopy using
potassium as a buffer to examine the effect of ionisation and the use of a buffer and to determine
the metallic elements present in different sample using AAS. As such in this experiment the
amount of manganese found in multivitamin tablet was determined. It was done using
calibration curve of concentrations of different manganese standards against absorbance. The
amount of manganese obtained was 1.282mg. A calibration graph was drawn to observe effects
of using potassium ion at different concentrations which are 10, 100, 500, 1000, 2500 and 500
ppm while keeping barium constant with a concentration of 10 ppm. The correlation coefficient
of the drawn calibration graph was found to be 0.9656 which shows the concentration the
strong relationship between the concentration and absorbance of a sample.

EXPERIMENTAL

Barium by AES:

This part of the experiment was done by the demonstrator where Ba standards of 0, 5.0, 10.0,
15.0, 20.0 and 25.0 ppm all of which contained 2500 ppm of K+ were used to obtain a
calibration curve. The 10 ppm Ba solutions which contained 0, 10, 100, 500, 1000, 2500 and
5000 ppm of K+ were also aspirated. The instrument was set to a specific wavelength and 2
calibration curves of concentration against intensity and concentration of K against Ba were
plotted which showed the effect of ionization and the use of a buffer.

Multivitamin/Mineral tablets

A tablet was putted in a 250ml beaker and 7ml of concentrated hydrochloric acid was added.
This was heated gently on a tripod stand with a Bunsen burner in a fume cupboard to be
dissolved completely and became black and charred. An amount of 50 ml of water was added
to the mixture and filtered into a 100ml standard flask. The residue was washed with 25 ml of
water then diluted to the volume.

A set of manganese standards containing 2,4,6,8 and 10ppm was prepared.

RESULTS

Table 1: Different Barium standards containing 2500ppm potassium

Barium Emission Emission Emission Average
concentration/ppm intensity rep1 intensity rep2 intensity rep3 emission
intensity
0 4351 4344 4348 4347,67
5.0 5003 4945 4996 4981,33
10 8563 8486 8450 8499,67
15 14476 14075 14167 14239,33
20 19368 18074 18494 18645,33
25 23366 23181 23175 23240,67
25000
y = 806,84x + 2240,2
R² = 0,9656
20000
Emission intensity/au

15000

10000

5000

0
0 5 10 15 20 25 30
Barium concentration/ppm

Figure 2: Calibration curve of standard concentrations of Ba with constant 2500ppm

K+ against emission intensity

Table 2: 10ppm barium with different concentration of potassium

[K+] /ppm Emission Emission Emission Average
intensity intensity intensity emission
Rep 1 Rep 2 Rep 3 intensity
0 0.200 -0.100 0.000 0.050
10 2.000 2.000 2.000 2.000
 100 5.300 5.200 5.200 5.230
500 6.800 6.500 6.700 6.670
1000 7.100 7.200 7.200 7.170
2500 8.300 8.200 8.200 8.230
5000 9.500 10.600 9.700 9.930
12

10
Barium concentration/ppm

0
0 1000 2000 3000 4000 5000 6000
[K+]/ppm

Figure3: concentration of 10ppm of barium with increasing concentration of potassium ion

Table 3: concentration of manganese standards with absorption intensity.
Manganese Absorption Absorption Absorption Average
concentration/ppm intensity intensity intensity Absorption
Rep1 Rep2 Rep3 intensity
0 0.074 0.074 0.074 0.074
2 0.104 0.097 0.102 0.101
4 0.117 0.112 0.114 0.114
6 0.129 0.136 0.129 0.132
8 0.141 0.145 0.146 0.144
10 0.171 0.173 0.172 0.172
Sample 0.192 0.195 0.194 0.194
 0,2
0,18 y = 0,0091x + 0,0773
0,16 R² = 0,9844
Absorption intensity/au

0,14
0,12
0,1
0,08
0,06
0,04
0,02
0
0 2 4 6 8 10 12
Manganese concentration/ppm

Figure4: calibration curve of manganese concentration against absorbance

Multivitamin/Mineral tablet sample absorbance = 0.194

y = 0.0091x + 0.0773

0.194 = 0.0091x + 0.0773

X= 12.82 ppm

12.82 ppm = 12.82 mg/L

12.82 mg/L × 0.1L = 1.282 mg

DISCUSSION

The aim of this experiment was to examine the effect of ionisation of Barium and the use of a
buffer by Atomic Emission Spectroscopy and to determine the metallic element (manganese)
present in solution from multivitamin/mineral tablet samples using Atomic Absorption
Spectroscopy (AAS).

The calibration curve for absorption against concentration of different manganese standards
was plotted. Absorbance of a sample was used as the y-intercept. The amount of manganese
obtained is 1.282mg. Not all multivitamin/mineral supplements contain manganese, but those
that do typically provide 1.0 to 4.5mg manganese. 1.28mg is a good amount because is between
the range. Too high or too low level of manganese in the body have negative impact.
Due to high sensitivity of AAS technique contamination should be avoided because affects
results. Thus sample must be kept clean as well as the environment around AAS.

The effect of ionization was investigated by using an ionization suppresser. Potassium was
found to be a very good buffer. Potassium is added if there is insufficient energy in the flame
to dissociate molecule to give atoms.

In Figure 2 Calibration curve of standard concentrations of Ba with constant 2500ppm K+

against emission intensity that was determine by AES indicates a positive linear relationship
between the standards concentration of Ba against emission intensity. It was found that
R2=0.9656 is close to 1 which indicates a strong relationship between the two variables.

CONCLUSION

The experiment was conducted to determine the amount of manganese in multivitamin/mineral

tablet. Results obtained was accurate because the value of R2 is 0.9844 is too close to 1. In the
analysis of barium, the role of potassium ions is vital because it hinders the ionisation of
barium. The buffer which was potassium in this experiment was added to minimise the
chemical interference of the molecules.

REFERENCES

1.Haswell, S.J.,1991. Atomic Absorption Spectrometry, Theory, Design and Applications.

Elsevier, Amsterdam, pp 852-857.

2.Reynolds, R.J. et al., 1970. Atomic Absorption Spectroscopy. Plenum Press, New York, pp
240-245.

3.Schrenk, W.G., 1975. Analytical Atomic Spectroscopy. Plenum Press, New York, pp 650-
658.

4.Varma, A., 1985. Handbook of Atomic Absorption Analysis. Vol. I. CRC Press, Boca Raton,
pp 1041-1044.

5. B. Welz and M. Sperling, Atomic Absorption Spectrometry, 3rd Ed, Wiley-VCH. New York
(1996)

6.Instrumental analysis laboratory manual,2021, UKZN, PP.28-32.

ANSWER TO QUESTIONS

For 1000 ppm calcium standard solution:

1. Dissolve approximately 3g. of calcium carbonate (CaCO3) in 25ml beaker using
hydrochloric acid. This should be added dropwise to avoid losses during the vigorous
effervescence. Dilute to 100ml in a volumetric flask with deionised water.
For 1000 ppm magnesium standard solution:

Dissolve 1.000g of magnesium metal in 50ml. of hydrochloric acid. Dilute to 1 litre in

a volumetric flask with deionised water.

2.Acetylene is a flammable gas and acts a fuel in the AAS/AES. When the fuel
(acetylene) flow is increased the flame becomes yellow, it becomes cooler and becomes
reducing in nature
3.Nitrous oxide flame has the reducing ability thus eliminating interferences that may
be caused by chemical interactions during the determination of the barium absorption.
Ba is a heavy metal which form stable oxides at certain temperatures and a higher
atomization potential. The nitrous oxide flames burn and reaches higher temperatures
of about a range between 2600-2800℃ which is enough to atomize Ba atoms.