UNIVERSITI TEKNOLOGI MARA

FACULTY OF CHEMICAL ENGINEERING

(ENVIRONMENTAL ENGINEERING)

Instrumental and Environmental Analysis (CEV 444)

ASSIGNMENT 2:

Analysis of Environmental Sample Using Spectroscopy Technique

LECTURER’S NAME:

Dr. Siti Aminah Binti Md. Ali

DATE SUBMITTED:

16th November 2018

NO. NAME MATRIX NO. CLASS

1. FARADILAH BINTI AJMA’IN 2016691966 PEH2246A1

 Analysis of Lead Content in Water Samples by Using Flame Atomic Absorption
Spectrometry (FAAS)

Water pollutants mainly consist of heavy metal, microorganism, fertilizer and thousands of
toxic organic compounds (Tareen, Sultan, & Parakulsuksatid, 2014). Heavy metal or known as trace
metal is one of the main contaminants in the aquatic environment. It also referred as the metallic
elements in the periodic table. Lead is one of the most toxic heavy metals which has accumulative
effect and an environmental priority pollutant (Islam, Foisal, Rahman, Lisa, & Paul, 2016).

The sources of lead in the water from two main sources which human and natural. The natural
sources of lead in the water are from the rocks and volatiles of volcanic origin. Diffusion of acidic
volcanic gases through water permeable rocks contribute to the hydrological material transfer in
volcanic strata will cause the presence of lead in the soils and water (Akpor, Ohiobor, & Olaolu, 2014).
Besides, soil erosion is one of the natural sources of lead. It occurs during run-off which lead
distributed to the environment and during rainfall lead are washed into poor drainage systems and
then into the nearby rivers (Akpor et al., 2014). In addition, some of human sources of lead in water
are metal finishing and electroplating, mining and textiles activities (Akpor et al., 2014). In metal
finishing and electroplating, the toxic metal which lead may be released into the water from the activity
of deposition of thin protective layers into prepared surfaces of metal by electrochemical process.
Other than that, in textiles activities the lead is released into the water from the compound used for
dyeing processes (Akpor et al., 2014).

Existing lead in the water systems give serious effect on human and aquatic life. Lead that
accumulate in the tissues may cause serious health problem. Lead inhibit biosynthesis and will affects
the kidneys, brain cells and permeability the liver membrane where can reduce some of their function.
In another words, accumulation of lead in body can promote disturbance such as nausea, vomiting,
diarrhea and sweating (Baysal, Ozbek, & Akman, 2013).

The most common analytical techniques for lead trace determination are flame atomic
absorption spectrometry (FAAS) (Najim, n.d.), the electrothermal atomic absorption spectrometry (ET
AAS) (Baysal et al., 2013) and inductivity coupled plasma optical emission spectrometry (ICP-OES)
(Popescu et al., 2009). Among the three analytical technique, ET AAS is the most sensitive technique
with a detection limit in the sub-pictogram range for most metals. At the same time, ICP-OES also
produced a detection limit in the same range with ET AAS (Popescu et al., 2009). FAAS is more
frequently used technique due to its simplicity and lower cost. FAAS are referred to as direct
aspiration determinations. It also normally completed as single element analysis and relatively free

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of interelement spectral interferences (García & Báez, n.d.). This technique need to undergo
preconcentration steps which extraction to improve the detection limit (Najim, n.d.).

From the previous study (Najim, n.d.), the extraction of dithizone complex of lead into
tetrachloride (CCl4) were optimized by considering different parameter such as extraction time,
amount of extraction and pH of aqueous solution. The water samples that contain lead is taken from
river, well, marshes and tap water from different area of Missan province (Najim, n.d.). The water
samples were collected during March 2013 in clean and dry plastic bottles of 1.5 L then filtered by
filter paper of Munktell Filter AB, Grade 292. After that, 5 drops of HNO3 with concentration 69% were
added for each bottle then were kept in fridge for 4 oC before undergoes analysis. The reagent and
solutions were prepared by using lead stock solution with 1000 µg ml-1. It was prepared by dissolving
0.1598 g of Pb in 1% (v/v) nitric acid solution in a 100 ml of volumetric flask. The dithizone reagent
was prepared by dissolving 0.005 g in 100 ml of CCl4. To determine the influence of pH, the HCl
solution with 2M were added to the aqueous solution samples. All measurements were carried out by
using AI Flame Atomic Absorption Spectrometer. Specific instrumental parameters were set for this
instrument. The radiation source was from a lead hollow cathode lamp which operated at 5 mA with
a slit width 0.2 nm and the wavelength was set at 217nm resonance line. The type of flame used was
air-acetylene with fuel flowrate at 1.5 Lmin-1. The calibration curve was carried to determine the lead
content in water sample by FAAS method. Firstly, an appropriate amount of working standard
solutions of lead were transferred to an extraction tube, then, 1 ml of 0.005% dithizone was added.
The obtained solutions were extracted for 120 seconds with CCl4. Finally, after removing the organic
solvent by slow evaporation, the residue was dissolved in 10 ml of NH3 (1:1), transferred to100 ml
volumetric flask and filled to the mark with deionized water. Besides, to determine the amount of lead
in water samples, the analyzed sample (100 ml) was transferred into an extraction tube and the same
preconcentration procedure was followed.

Figure 1: Working principle of atomic absorption spectroscopy (AAS) (Khalid, Alaama, & Abbas,
2016)

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 Based Figure 1, for FAAS, the radiation source is hollow cathode lamp which will emit the light
or photon into the atomizer which is flame where the samples are introduced as an aerosol by the
nebulizer. The monochromator will eliminate scattered light of other wavelength by several lenses
and mirrors to focus the radiation and the detector which photomultiplier tube that converts the light
signal into the electrical signal which represent the light intensity (Khalid, Alaama, & Abbas, 2016).

From the study (Najim, n.d.), the efficiency of extraction procedure is depending on the contact
time, the effect of extraction time on the analytical signal of the lead was estimated. The results
obtained that the necessary time for complete extraction is 120 s. Meanwhile, for the effect of
extracted volume, the optimum volume was obtained is at 10 ml of CCl4. At the same time, the
optimum pH for the better complexation is in range of 8 to 11.5. Figure 2 show the calibration curve
obtained for Pb by using FAAS. Besides, the results at Table 1 and graph at Figure 3 shows that Al-
Uzer sample collection station (T33) have highest concentration of Pb which 0.085 mg/L while the
lowest concentration of Pb is at AL-Meger sample collection station (TJ) which 0.021 mg/L.

Figure 2: Calibration curve of Pb from FAAS (Najim, n.d.)

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 Table 1: Result of Pb content in each water sample (Najim, n.d.)

No. Sample site Pb concentration determined by

FAAS (mg/L)
1. TSH (Al-Musherh sample collection station) 0.067
2. TM (Al-MEymonah sample collection station) 0.050
3. T33 (Al-Uzer sample collection station) 0.085
4. TJ (AL-Meger sample collection station) 0.021
5. T32 (Al-Kalah sample collection station) 0.036
6. Tap water 0.072
7. Rain water 0.031
8. Well water 0.081
9. MO (Al-Oudah Marshes sample collection station) 0.056

Figure 3: Graph of sample site versus the concentration of Pb (Najim, n.d.)

As conclusion, FAAS is a suitable technique to determine metal with good precision. It also
moderate interferences that can be easily corrected and relatively low cost. The combination of FAAS
with preconcentration of analyte by liquid-liquid extraction. The complexation of lead with dithizone
was efficient enabling its preconcentrate from water. The determination of lead in natural water
samples were selected from different areas of Missan province. In addition, the analytical costs of the
proposed extraction method are low, it is simple, quick and the operation techniques are easy. Thus,
the proposed preconcentration methodology offers a simple and sensitive technique. This proposed
procedure for determination of lead can be suitable for routine application for water analysis.

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 References

Akpor, O. B., Ohiobor, G. O., & Olaolu, T. D. (2014). Heavy metal pollutants in wastewater effluents :
Sources , effects and remediation, 2(4), 37–43. http://doi.org/10.11648/j.abb.20140204.11

Baysal, A., Ozbek, N., & Akman, S. (2013). Determination of Trace Metals in Waste Water and Their
Removal Processes.

García, R., & Báez, A. P. (n.d.). Atomic Absorption Spectrometry ( AAS ).

Islam, R., Foisal, J. Al, Rahman, M., Lisa, L. A., & Paul, D. K. (2016). Pollution assessment and heavy
metal determination by AAS in waste water collected from Kushtia industrial zone in Bangladesh,
10(1), 9–17. http://doi.org/10.5897/AJEST2014.1994

Khalid, R. S., Alaama, M., & Abbas, S. A. (2016). Main Analytical Techniques Used for Elemental
Analysis in, 15(February), 427–434.

Najim, S. S. (n.d.). Determination of lead in river water by Flame Atomic Absorption Spectrometry,
55–62.

Popescu, I. V, Stihi, C., Dima, G., Gheboianu, A., Bancuta, I., Ghisa, V., … Laboratories, P. (2009).
ENVIRONMENTAL SAMPLES ANALYSIS BY ATOMIC ABSORPTION, 54, 741–746.

Tareen, A. K., Sultan, I. N., & Parakulsuksatid, P. (2014). Detection of heavy metals ( Pb , Sb , Al ,
As ) through atomic absorption spectroscopy from drinking water of District Pishin , Balochistan
, Pakistan, 3(1), 299–308.