You are on page 1of 8

Introduction

Water is essential to human life for us to drink and for daily life activities. Unfortunately,
people always assume that the water they used everyday are safe to be consume. This is because
the water may contain trace amount of mineral matter, gases and other substances including
heavy metals. These heavy metals are toxic for us to consume and they have a wide range of
effects to us such as acute poisons and chronic diseases. Examples of them are nickel (Ni),
cadmium (Cd), copper (Cu), zinc (Zn), lead (Pb) and arsenic (As). These heavy metals are
discharged in effluents by industries that uses these metals in their operational such as
petrochemical and electroplating. Besides that, there are many opportunities for the water to
have these heavy metals as they located underground which they come in contact with mineral
deposits. Hence, it is necessary for us to determine the concentration of the heavy metals inside
the water by measuring the quantity of light of specific wavelength absorbed by atoms of the
elements released in a flame. Figure 1 shows an atomic absorption spectrophotometer, which
consist of an atomizer-burner to convert the element in solution to free atoms in an air acetylene
flame. This is followed by a monochromator to disperse and isolate the light waves emitted
and a photomultiplier to detect and amplify the light passing through the monochromator. The
light source is a lamp with a cathode formed of the same element being determined since each
element has characteristic wavelengths that are readily absorbed. The light passing through the
sample is separated in the monochromator into its component wavelength. The photomultiplier
then receives the only the isolated resonance wavelength. The amount of energy at the
characteristic wavelength absorbed in the flame is proportional to concentration of the element
in the sample. But then, sample containing particulates or organic material generally require
pre-treatment before spectroscopic analysis. This is to reduce interference by organic matter
and to convert metals associated with particulates to a form that can be determined by atomic
absorption spectrometry. Nitric acid digestion is the one suitable to be use for lead (Pb) because
this method presents one approach trace levels where lead usually at very low concentration (
0.1 mg.-1).
Figure 1: Simplified schematic diagram of an atomic absorption spectrophotometer

Objectives

To familiarize in general the atomic absorption spectrophotometer


To determine the concentration of lead (Pb) in water sample
To compare the concentration of heavy metal present in the water sample with the
values of Standard B
Method

Preparation of standard 100mg/L from stock solution 1000mg/L Pb


1. The stock solution is first diluted to become 100mg/L by transferring 10mL of
1000mg/L into 100mL capacity volumetric flask.
2. Then, distilled water was added to the mark.
3. The flask was then inverted several times to properly mix the contents.

Nitric Acid Digestion Process

1. 100 mL of waste water sample was put in a beaker and heated using hot plate.
2. 5 mL of 65% concentration nitric acid, HNO3 was added to the sample in the beaker.
The beaker was covered with ribbed watch glass.
3. During the heating of the solution, 5 ml of nitric acid was gradually inserted at interval
of 20 minutes.
4. Temperature of hot plate was increased so that a gentle reflux action occurs. Heating
was continued and it was necessary to add additional amount of acid, until digestion is
complete. (After 3-4 times gradually inserting nitric acid, observes the colour of sample
is noticeably changes from dark brown to pale yellow).
5. Slow down the heat to cautiously evaporate to less than 5 mL, making certain that
sample does not boil and that no area of the bottom of the container is allowed to go
dry.
6. The hot plate was turned off and the sample is left for 5 minutes for cooling.
7. Beaker walls and watch glass were washed with metal-free water, and then filtered to
remove insoluble material that could clog the nebulizer.
8. After preparation for sample, standards and blanks has been completed, the technician
operated the AAS, the standard curve was plotted and the concentration of
lead (Pb) was measured.
Data & Result

Mixture Observation Explanation


Adding 5 m conc. HNO3 The water sample change its HNO3 act as an oxidizing
into the water sample while colour from dark black to agent where zero valence Pb
heating it every 20 minutes. light yellow which seems to and HNO3 are oxidized and
be a clear solution. brought into the solution
where the nitric acid does not
form any insoluble
compounds reacting with
lead.

Table 1: Observation during the water sample undergoes nitric acid digestion

Sample Lead Concentration (mg.-1) Absorbance


Standard 1 1.00 0.02400
Standard 2 2.00 0.04800
Standard 3 3.00 0.07200
Water Sample 0.09 0.00216

Table 2: The absorbance of the sample with different lead concentration (mg.-1)

Lead Concentration (mg.-1) vs Absorbance


0.08
Standard 3
3, 0.072
0.07

0.06 Standard 2
y = 0.0240x
2, 0.048
0.05
Absorbance

0.04
Standard 1
0.03 1, 0.024

0.02 Water Sample


0.09, 0.00216
0.01
0, 0
0
0 0.5 1 1.5 2 2.5 3 3.5
Lead Concentration (mg.-1)

Figure 2: The graph of lead concentration (mg.-1) vs absorbance


Discussions

Sample containing particulates or organic material generally require pretreatment before


spectroscopic analysis including heavy metals such as lead. Nitric acid digestion is the one
suitable to be use for lead (Pb) because this method presents one approach trace levels where
lead usually at very low concentration ( 0.1 mg.-1). For nitric acid digestion, 5 m conc.
HNO3 was added into the water sample while heating it every 20 minutes. It was observed that
the water sample change its colour from dark black to light yellow which seems to be a clear
solution. According to Gaines (2016), the chemical reaction occurred during this acid digestion
is shown below.

3Pb + 6H2 O+ + 2HNO3 2NO + 3Pb+2 + 10H2 O

Gaines (2016) stated that the HNO3 act as an oxidizing agent / acid combo where zero valence
lead is oxidized and brought into the solution. In addition, nitric acid does not form any
insoluble compounds with lead. Hence, the colour change from dark black to light yellow
which seems to be a clear solution.

Atomic absorption spectrophotometer (AAS) is an analytical technique that measures the


concentrations of elements. Based on Kumar and Kumar (2016), it is so sensitive that it can
measure down to parts per billion of a gram in a sample. The technique makes use of the
wavelengths of light specifically absorbed by an element. Atoms of different elements absorb
characteristic wavelengths of light. Analysing sample to see if it contains a particular element
means using light from that element. In AAS, the sample is atomized by converting it into
ground state free atoms in vapour state and then a beam of electromagnetic radiation emitted
from excited heavy metal atoms are passed through the vaporized sample. Some of the radiation
is absorbed by the heavy metal atoms in the sample. The greater the number of atoms there is
in the vapour, the more radiation is absorbed. Besides that, Harris (2003) stated that the amount
of light absorbed is proportional to the number of heavy metal atoms. A calibration curve is
constructed by running several samples of known heavy metal concentration under the same
conditions as the unknown. The amount of the standard absorbs is compared with the
calibration curve and this enables the calculation of the heavy metal concentration in the
unknown sample. According to Skoog et al. (1999), it is called the external standard method.
According to Table 2, there are three standard solutions was used to construct a calibration
curve which have the concentration of 1.00, 2.00 and 3.00 mg.-1 and the absorbance of 0.024,
0.048 and 0.072.
Hence, the unknown concentration of lead of the water sample can be determined by using its
absorbance which 0.00216. By using the equation given for the straight line in Figure 2, the
lead concentration of the water can be calculated.

= 0.024

Where y is the absorbance of the solution

x is the lead concentration inside the sample (mg.-1)

Hence, the concentration of Lead inside the water sample are calculated to be 0.09 mg.-1.
According to the Environmental Quality (Industrial Effluents) Regulations 2009 (PU (A) 434),
the Standard B for concentration of lead is 0.5mg.-1. By comparing this results with Standard
B, it shows that this sample is safe and acceptable in conditions for discharge of industrial
effluent for mixed effluent as it is not more than 0.5 mg.-1. If the concentration of heavy metals
is higher than the standard, this means that the water is not safe to use. It is because heavy
metals can be very harmful to health if found in a drinking water. According to Davis and
Cornwell (2008), this can cause severe effects such as reduced development and growth,
cancer, damage in organs, and in extreme cases, death. Thus, exposure of metals like lead may
cause autoimmunity, that is a persons immune system attacks on its own cells, which can lead
to rheumatoid arthritis, kidneys disease, circulatory and nervous system disease.
Conclusions & Recommendation

The objectives of this experiment are achieved. Atomic Absorption Spectrophotometer is a


quantitative analytical instrument that measures the concentration of elements inside a sample.
The sample will be heated in an acetylene flame so that the lead atom is vaporized while it
absorbs the electromagnetic radiation emitted to it whereby the concentration of lead is higher
when the value of absorption is larger. The external standard method is used to plot the
calibration curve where 3 standards with known lead concentration undergoes the AAS and
using this calibration curve, the concentration of lead inside the water sample could be
calculated using the straight line equation given whereby the concentration of lead inside the
water sample is 0.09 mg.-1. Hence, by comparing the sample with Standard B, the water is
safe and acceptable in conditions for discharge of industrial effluent for mixed effluent.

In this experiment, it is recommended that do not hesitate to add additional acid to the sample
during heating. This is because adding more will fasten the reaction of digestion process in
sample besides increasing the temperature. Next, make sure to use mineral-free water during
beaker washing because it can prevent from the sample from contaminated with other heavy
metals. By doing this, the result will be more accurate and the sample will be free from other
contaminants.

References

Davis, M.A., & Cornwell, D.A. (2008). Introduction to Environmental Engineering. (4th
Edition). New York: McGraw-Hill Education

Gaines, P. (2016). Acid Digestion of Inorganic Samples. [Online]. [Accessed 29-08-2017].


Available from world wide web: www.inorganicventures.com/acid-digestions-inorganic-
samples.

Harris, D.C. (2003). Quantitative Chemical Analysis. (6th Edition). New York: W. H.
Freeman and Company

Kumar, K., & Kumar, N. (2016). A Study of Heavy Metal Removal by Adsorption. IJSRD.

Skoog, D.A., West, D.M., Holler, F.J., & Crouch, S.R. (1999). Analytical Chemistry An
Introduction. (7th Edition). Singapore: Thomson Learning Inc.
Appendix