African Journal of Biotechnology Vol. 10(71), pp.

16051-16057, 14 November, 2011

Available online at http://www.academicjournals.org/AJB
DOI: 10.5897/AJB10.1840
ISSN 1684–5315 © 2011 Academic Journals

Full Length Research Paper

Spectrophotometric determination of iron (III) in tap

water using 8-hydoxyquinoline as a chromogenic
reagent
Basheer K. Adebayo1, Segun Ayejuyo1, Hussein K. Okoro2* and B. J. Ximba2
1
Department of Chemistry, Faculty of Science, University of Lagos, Akoka, Lagos State, Nigeria.
2
Department of Chemistry, Faculty of Applied Sciences, Cape Peninsula University of Technology, P. O. Box 1906,
Cape Town Bellville Campus, 7535, South Africa.
Accepted 2 June, 2011

A simple, rapid and sensitive spectrophotometric method was developed for the determinationation of
trace amounts of iron (III) using 8-hydroxyquinoline as a chromogenic reagent. The proposed method
was based on the reaction of iron (III) with 8-hydroxyquinoline in chloroform solution to form a metal-
oxine complex having a maximum absorption at 359 nm. Beers law was obeyed in the range of 1 to 14
ug/ml Fe3+. The recovery was between 98.60 and 103.30% with a coefficient of variation of 1.209%. The
method was successfully applied to tap water samples and comparison with standard method showed
the new method to be accurate and precise as the more sophisticated AAS commonly used for Fe
determination.

Key words: Chloroform, hydroxyquinoline, iron, spectrophometry, oxine, spectrophometry, tap water.

INTRODUCTION

Water is the basis of life, an ecological resource for the suggest that it would cost an excess of USD 109 a year to
earth’s flora and fauna and a fundamental necessity for reduce the problems if ground and surface water
human life. If there is no adequate supply of safe water, contamination goes unchecked.
we have no hope of improving the health of the people in Iron is an objectionable constituent of potable water.
our partner countries (Adebayo et al., 2007: Eddy and Presence of iron in water impacts a bitter and metallic
Ekop, 2007). It has been estimated that 80% of all characteristic taste and oxidized precipitate. Water
diseases are in some way, connected with contaminated containing significant qualities of iron may appear clear
water (WHO, 2007). It is difficult to achieve productive when drawn and change quickly upon exposure to air.
human activity without a functional water supply be it This process is called oxidation and it involves the
agriculture, forestry, trade or industry. conversion of ferrous ion to ferric ion. Iron stains
Adekunle et al. (2007) highlighted some problems everything with which it comes in contact; 0.3 ppm
associated with lack of adequate and quality water standard is often recommended and is based on
resources in Nigeria; they include threat to health of preventing taste and staining problems for humans
about 40 million people. Globally, pathogenic contami- (Damron and Eldred, 2002). The World Health
nation of drinking water poses the most significant health Organization (WHO) recommends 0.3 mg/l (WHO, 1993)
risks to humans. There have been countless numbers of as maximum concentration limit of iron in drinking water.
disease outbreaks and poisoning throughout history Federal and state regulations limit the iron content of
resulting from exposure to non pathogenic, toxic drinking water to <1 ppm, though iron is easily
contaminants that are often globally ubiquitous in drinking determined in contaminated water containing > 1 ppm (1
water (Ritter et al., 2002). The latest World Bank studies mg/l). Iron in excess of 0.2 to 0.3 mg/l may cause
nuisance even though its presence does not affect the
hygienic quality of water (0 to 0.3 mg/l acceptable. 0.3 to
1.0 mg/l satisfactory and over 1.0 mg/l unsatisfactory)
*Corresponding author. E-mail: [email protected]. (Abdoljalaal et al., 2009).
16052 Afr. J. Biotechnol.

Iron is commonly present in surface and drinking the determination of elements are based on the
water. This occurs from dissolution processes of iron- absorption of visible and near ultraviolet radiation. Visible
stones in nature and partially from the corrosion spectrophotometry was often called colometry and such
processes in pipes (Pitter, 1990). Industrial wastewater is definitions as colorimetric photometric or absorptometric
also a significant source of iron. The iron concentration in methods are sometimes used in the literature, as
water can vary over several orders of magnitude from equivalent to the terms spectrophotometric method
tens of µg/l (sea water) to tens of mg/l (source). The (Sandwell, 1985). The basis of spectrophotometric
concentration of iron in most ground and surface water is methods is the simple relationship between the absor-
not very impor-tant from the hygienic point of view; its ption of radiation by the solution and the concentration of
content influences, however the organoleptic properties species in the solution. In order to determine a species or
of drinking water, mainly the color, taste and turbidity. analyte in the solution spectrophotometrically, it is usually
Iron concentration thus becomes a parameter for the converted into a colored complex. The colour of the
quality of drinking water. However, wastewater also has analyte or itself is utilized much less often (Sandwell,
concentration limits, but their limit varies for various 1985).
industrial branches. From the literature, maximum limits When the determinant is not coloured, or forms no
are set between 5 and 10 mg/l (Pavael et al., 1997). coloured compound, indirect spectrophotometric method
The iron content of water can cause technical faults may be used for its determination or ultraviolet spectro-
rather than sanitary problems; iron concen-tration of just photometry may sometimes be used. Spectrophotometric
0.5 mg/l can lead to turbidity of water. Small amounts of methods are remarkable for their versatility, sensitivity
Fe (II) can cause iron bacteria growth leading to the and precision. Almost all are direct and can be used for
clogging of pipes and an offensive odour of water. all the elements except for the noble gases. A very
Several analytical methods have been used for the extensive range of concentration may be covered from
determination of iron in water. They include HPLC macro quantities to trace (10-8 to 10-6%). Spectro-
methods (Nagosa et al., 1991; Yi et al., 1992), which are photometric methods are among the most precise
based on the separation of various complexes of iron and instrumental methods of analysis (Edisbury, 1990). This
other cations offering the possibility of multielement study was aimed at determining iron in tap water
analysis. Necessity of sample pre-treatment such as SPE collected from University of Lagos and some selected
or solvent extraction is the demerit of these methods. locations in Lagos metropolis, Lagos Nigeria using the
Various spectrophotometric procedures have also been proposed spectrometric method.
employed; some of them are combined with flow injection
analysis (Pavel et al., 1997). Atomic absorption spectro-
metry and inductively coupled with plasma spectrometry MATERIALS AND METHODS
have also been applied for the determination of iron in
Chemicals and apparatus used were 8-hydroxquinoline (oxine),
water and other cations (Abollino et al., 1995). Iron has sulphuric acid, chloroform, distilled water, ferric ammonium
been separated by capillary isotachophoresis as an sulphate, analytical grade aluminum sulphate, separating funnel,
EDTA complex for the simultaneous determination of beaker, test tubes, pipettes, volumetric flasks, measuring cylinder
EDTA-Fe (III) and free EDTA not in water but in wash and UV spectrophotometer (spectronic 20D+).
liquids used for the desulfurization of gases. EDTA-Fe
(III) complex has also been used for the determination of
Preparation of stock solutions
EDTA in manganese (Ito et al., 1980). However, an
intensely colored complex must be formed to detect the 8.635 g of ferric ammonium sulphate was weighed and dissolved in
presence of these low levels of iron spectropho- distilled water containing 3 ml of concentrated H2SO4, the solution
tometrically. Usually, when trace quantities of an analyte was diluted to 1 L in standard flask. Working solutions were
obtained by suitable dilution of the stock solution with dilute
are being measured, cleanliness of equipment, glassware sulphuric acid (0.005 M).
etc. is essen-tial to prevent positive determinate errors 1.0 g of oxine was accurately weighed and dissolved in 100 ml
due to laboratory contamination (Skoog et al., 2010). acidified water with pH 1 to 2. 1.0 g of 8-hydroxquinoline was
Furthermore, in analytical chemistry, special attention is weighed and dissolved in chloroform in a 100 ml volumetric flask
given to development of methods simultaneously com- and made up to the mark with chloroform. The flask was covered
bining preconcentration and determination. A promising immediately to avoid evaporation.
technique therefore, is the use of ready analytical
methods (Gavrilenco and Markova, 2008). Determination of absorption maxima for metal-oxine complex
Methods are continually being developed to improve
the selectivity, sensitivity and specificity of an analyte. It A solution containing 10 ppm of iron standard was placed in a
separating funnel, 10 ml of oxine-chloroform was added and the
is equally important to consider new methods in terms of
content was properly shaken for 3 to 5 min. The aqueous layer was
cost, convenience and the number of sample throughout. allowed to separate by a clear partition between the 1 upper layer
The precision and accuracy of methods are also critical (the aqueous layer) and the denser chloroform oxine-metal complex
factors in any analysis. Spectrophotometric methods for layer. The oxine-metal complex was separated into a test tube and
 Adebayo et al. 16053

Figure 1. Absorption maxima for iron-oxine complex.

covered immediately. A blank was prepared by adding 10 ml of technique for comparison.

distilled water to 10 ml of chloroform in a separating funnel. The 2-
layers were properly shaken for 3 to 5 min and then separated into
test tubes. The absorbance of the 10 ppm oxine-metal complex was Recovery and stability studies of the proposed method
scanned at various wavelengths in order to establish the maximum
absorbance (Amax). To 10 ml aliquot of the water sample, 3 ppm of Fe (III) standard
solution was added. The extraction procedure was carried out as
described earlier. The absorbance was measured. The standard
Standard solution preparation concentrations were studied for about 72 h by continually
monitoring the absorbance. The absorbance of the standard
The stock solution was diluted serially by 0.005 M sulphuric acid. To concentration was recorded against time.
each of the standard solutions (1 to 10 ppm), 10 ml of chloroform
oxine reagent was used for the extraction of the metal oxine
complex and their absorbances were recorded. Oxine was Standard addition recovery studies on 10 ppm
prepared in deionised water by weighing and 100 g oxine was
accurately weighed and dissolved in 100 ml acidified water (pH 1 to To 10 ml of the water samples, 10 ppm of Fe (III) standard was
2). added. The procedure to develop the color was as described
earlier.
Preparation of calibration curve
Amount covered 100
Series of iron (III) standard solution were prepared from 1 to 14 % Recovery = ×
ppm. To 10 ml of the solution containing each of the standards, Spiked amount 1
about 0.5 ml of the oxine solution was added. Their corresponding
absorbance was measured.
RESULTS AND DISCUSSION
Interference studies
Preliminary studies had shown that oxine could react with
Using oxine chloroform reagent and acidified water solution iron III to form a colored complex that could be monitored
and developed into a simple spectrophotometric method
To a solution containing l0 ppm of iron (lll) standard, l0 µg/ml of Al
(III) was added; the solution was made up to 10 ml. The extraction
for the determination of Fe in samples. Efforts were
was carried out the same way as described earlier. For acidified therefore made to optimize the reaction conditions. The
water solution, a solution containing 10 ppm of iron (III) standard, spectrum of the complex has a maximum absorption at
10 µg/ml of A13+ was added, and the solution was made up to 10 ml 359 nm (Figure 1) and this Amax was used in subse-
in a volumetric flask. 0.5 ml of acidified oxine reagent was added to quent experiments.
form a greenish color metal oxine complex.

Determination of iron (III) in water samples

Preparation of calibration curve

To 10 ml each of the water samples, a drop of sulphuric acid was As shown in Figures 2 and 3, the calibration curves were
added. It was later treated the same as the standard. Levels of iron rectilinear up to 10 ppm on investigation using oxine
were also assessed in the water sample using atomic absorption chloroform reagent and up to 14 ppm using acidified
16054 Afr. J. Biotechnol.

Absorbance

Figure 2. Calibration curve using oxine chloroform solution.

Absorbance

Figure 3. Calibration curve using oxine acidified reagent.

oxine as reagent. water samples are shown in Table 3. As indicated in

As presented in Table 1, the mean values for iron in the Table 3, the method gave very good recovery and the
samples were similar with the results involving the more determination of iron (III) using the proposed method
expensive AAS determination. would be quantitative.

Reproducibility of oxine method Interference studies performed using oxine

chloroform reagent
With the coefficient of variation of 1.209%, the
reproducibility of the proposed method for iron The result of interference studies using oxine chloroform
determination is good (Table 2). reagent is presented in Table 4.

Recovery studies Interference studies using oxine acidified reagent

The results of recovery of spiked amounts of iron III in Aluminum is noted for its reaction with oxine and its
 Adebayo et al. 16055

Table 1. Comparison of proposed method result with AAS (ppm).

Sample Proposed method AAS

W1 1.02 1.04
W2 1.50 1.52
W3 1.04 1.07
W4 1.96 1.20
W5 2.54 2.55

Table 2. Result of reproducibility of oxine methods.

Sample Absorbance
1 0.480
2 0.474
3 0.470
4 0.479
5 0.480
6 0.478
7 0.476
Mean value: 3.321; standard deviation: 0.006; coefficient of variation:
1.209%.

Table 3. Recovery studies of spiked Iron (III) from proposed quantitative method.

Sample Amount added (µg/ml) Amount recovered (µg/ml) Percent recovery (%)
1 3.00 3.10 103.33
2 3.00 3.00 100.00%
3 10.00 10.05 100.50
4 10.00 9.85 98.50

Table 4. Results of interference studies.

Sample Absorbance
10 ppm Fe (standard) 0.562
10 ppm Al3+ + 10 ppm Fe3+ standard 0.560

Table 5. Results of interference studies using oxine

acidified reagent.

Sample Absorbance
10 ppm Fe III (standard) 0.565
3+
10 ppm Fe + 10 ppm Al 0.567

possible interference effect on the proposed method was The stability studies of the proposed method
studied. As shown in Table 5, Al did not interfere in the
analysis under the optimized conditions. The absorbance remained almost constant for the 72 h
16056 Afr. J. Biotechnol.

Table 6. Results of the stability studies of the proposed method.

Concentration Absorbance at 24 h Absorbance at 48 h Absorbance at 72 h

10 ppm 0.565 0.567 0.567

Absorbance

Time (h)

{Time (h)}

Time (h)

Figure 4. The stability curve of the proposed method.

study period as shown in Table 6 and Figure 4, available and affordable. The work has increased the
respectively. This is an indication of the stability of the array of methods that are available for the determination
technique being proposed. Accurate measurement of iron of iron in water. The proposed method gave similar
within a reasonable time without any loss or fear of any results when compared with other established and com-
side reaction can therefore be ensured. At the monly used methods. It does not involve any laborious
recommended pH (2 to 3), Al did not interfere with the procedure. It can be accomplished within a very short
determination of Fe (III) using both the oxine-chloroform period, thereby allowing the handling of large number of
and oxine-acidified water reagent solutions. The results samples.
of stability studies for oxine acidified water showed that
the absorbance was stable for about 72 h; oxine-chloro-
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