SPECTROSCOPIC DETERMINATION OF IRTON IN WATER SAMPLE USING

STANDARD ADDITION METHOD.

GOBE JAM CHEM 301

INTRODUCTION
To gauge how much light a particular sample absorbs, spectrophotometers are employed. In a
spectrophotometer, there are two components. The photometer, which gauges light intensity, and
the spectrometer, which generates light, are the two instruments. While using a
spectrophotometer, the photometer and spectrometer are separated by a cuvette filled with liquid.
A portion of light is passed through the sample and is absorbed by the photometer which
calculates the amount of light that was absorbed (Carter, P., 1971). The light is measured in
nanometers and the machine can release different wavelengths of light to pass through samples.
Understanding the term "absorbance" is necessary because this device measures the absorbance
of a certain wavelength. The amount of light that a sample absorbs or takes in is known as its
absorbance in spectroscopy. Each item absorbs light differently due to its absorbency. By putting
a substance in the spectrophotometer, the absorbance may be determined. It determines the
amount of light that was absorbed and then releases light through the material (Smart, J.A. and
Amis, E.S., 1955). The ratio of absorbance to a substance's concentration is direct. The two
create a linear graph that is used to display Beer’s Law. Beer’s Law is A = abc where A is
absorbance, a is molar absorptivity (a constant), b is the path length (constant in cm.), and c is
the concentration’s molarity (Westerlund, S., 1978). Multiple solutions with different
concentrations can construct the graph and create the linear equation. An unknown solution’s
concentration can be found by finding the absorbency of the solution and plugging it into the
given linear equation.

OBJECTIVE

 The purpose of this experiment was to determine the concentration of iron (II) in an
unknown sample.

MATERIALS

 Volumetric flask
 Beaker

 REAGENTS
 Nitric acid
 Hydrochloric acid
 Potassium thiocyanate
 Ammonium iron (3)
METHOD

Standard solution of iron (Fe3+) was prepared by dissolving 0.864g ammonium (fe 3+) sulphate in
deionized water then 10ml of concentrated hydrochloric acid and dilution to 1L hence giving
100µg ml-1 Fe3+ solution. And thiocyanate solution was prepared by dissolving 20g potassium
thiocyanate in 100ml deionized water. Six 50 ml volumetric flasks were filled with 30ml of water
to each flask. Each flask was labeled by a number from 1 to 7 including one as for the blank
solution. After filling flask with 30 ml water, o,1,2,3,4 and 5ml of standard iron 3 solution. To
each flask excess SCN of about 5 ml was then added followed by 3ml of 4 M nitric acid. Finally
deionized water was added to fill all flasks to the mark. The blank was also prepared using the
same reagents and 30 ml deionized water instead of the sample. The reagent blank was taken in
reference cell of the instrument. The 2.5 ml aliquot was transferred from flask 1 to the sample
cell and measured the absorbance at 480 nm.

RESULTS
Table 1. Observation

Flask No. Blank 0 1 2 3 4 unknow

Absorbance 0.000 -0.074 0.126 -0.022 0.196 0.196 0.024

Figure 1
SAMPLE CALCULATION
Y= mx + b
y=A
A = mx + b
A = 0.024
A = 0.0037 x + 0.0194
0.024 = 0.0037x + 0.0194
(0.024 – 0.0194) /0.0037 =0.0037x/0.0037
X= 1.24 ppm
Finding concentration in terms of molarity
M= Concentration in mg/L
Molecule weight of solute X 1000
1ppm = 1mg/L
1.24 ppm = 1.24 mg/L
M= 1.24 mg/L
55.85g/ml X 1000
M = 2.22 × 10 -5

% arrow = actual – theoretical X 100 %

Theoretical
= 1.03/2.3× 100%
= 46.1 %
DISCUSSION
The spectrophotometer is a simple instrument for measuring the amount of light transmitted
through solutions. It has a diffraction grating that can be used to adjust the wavelength of light
transmitted. In general, the light used should be the complimentary color of the solution being
tested. The amount of light at a given wavelength that a sample absorbs is often directly
proportional to the concentration of the absorbing species in the sample and to the distance (path
length) the light must travel through the sample.
In this experiment, (Smart, J.A. and Amis, E.S., 1955) the concentration of iron was determined
with the use of a single-beam spectrophotometer. Metal complexes do not form in strongly acidic
solution (Morris, R., 2015). Spectrophotometry. Current Protocols Essential Laboratory
Techniques, 11(1), pp.2-1. On the other hand, most metals form insoluble metal hydroxides in
basic solutions. For these reasons the iron determination using the standard solution is carried out
in a slight. In most water samples, iron exists in its oxidized form, Fe (III), due to the presence of
oxygen (Carter, P., 1971). The absorbances of the prepared standards were measured using a
spectrophotometer at a wavelength (Morris, R., 2015. Spectrophotometry. Current Protocols
Essential Laboratory Techniques, 11(1), pp.2-1.of 408) nm where maximum absorbance is
observed. The concentration of the standards was computed, and a curve was plotted absorbance
vs volume. Sample calculation in the determination of the concentration of the standard
unknown is shown in calculation section above. The plot is shown in figure 1 above.
The standard solutions of the known concentrations were diluted, and the absorbance was
calculated for a wavelength to calculate the unknown concentration of [Fe+]. A calibration curve
was constructed using Excel, absorbance vs sample volume. The best fit line of the linear
equation was created y = 0.0037x + 0.0194 (Spec 20) the R2 value is near 1 which represents
that the values are close to the actual linearity to the data. Westerlund, S., 1978
CONCLUSION
The purpose of this experiment was met because the concentration of the unknown iron (II)
solution was discovered. The concentration in ppm was1.24 and the concentration in terms of
molarity was 2.22 x 10 -5. The percentage error for this experiment was 46.1%. An error that
occurred in the lab was the when the standard solution is made, it was contaminated by nitric
acid.
REFERENCE
 Viollier, E., Inglett, P.W., Hunter, K., Roychoudhury, A.N. and Van Cappellen, P.,
2000. The ferrozine method revisited: Fe (II)/Fe (III) determination in natural waters.
Applied geochemistry, 15(6), pp.785-790.

 Danielsson, L.G., Magnusson, B. and Westerlund, S., 1978. An improved metal

extraction procedure for the determination of trace metals in sea water by atomic
absorption spectrometry with electrothermal atomization. Analytica chimica acta,
98(1), pp.47-57.

 Carter, P., 1971. Spectrophotometric determination of serum iron at the submicrogram

level with a new reagent (ferrozine). Analytical biochemistry, 40(2), pp.450-458.

 Harvey Jr, A.E., Smart, J.A. and Amis, E.S., 1955. Simultaneous spectrophotometric
determination of iron (II) and total iron with 1, 10-phenanthroline. Analytical
Chemistry, 27(1), pp.26-29.

 Soifer, B.T., Willner, S.P., Rudy, R.J. and . 4-8 micron spectrophotometry of OH
0739-14. The Astrophysical Journal, 250, pp.631-635.