DETERMINATION OF IRON IN WATER AND WASTEWATER

NAME: UYAPO R.S BATISANI

PROGRAM: PURE AND APPLIED CHEMISTRY
STUDENT ID: 19000149
CHEM 205
 DETERMINATION OF IRON IN WATER AND WASTEWATER
AIM
To determine the concentration of iron (ii) in an unknown sample using
spectrochemical measurements.
INTRODUCTION
Any solution which is coloured or can be made coloured by adding a
complexing agent can be analysed using a visible spectrophotometer.
Spectrometer measures the amount of light absorbed by a sample. According
to (Donald L. Pavia 2009), this experiment uses spectrochemical measurements
to determine the concentration of iron (ii) in an unknown sample. Iron in the
+2-oxidation state reacts with o-phenanthroline to form the orange – red Fe(o-
phen)32+ complex. The intensity of the complex’s colour is independent of
solution acidity between a pH of 3 and 9. Due to a faster rate of complex
formation in a more acidic solutions, the reaction is usually carried out in a pH
within the range of 3.0 – 3.5. This is done by analysing a series of Fe 2+ standards
and light intensities of the red colour of this solution will be measured and
graph is plotted ( Annem, 2017)
In this experiment, a stock solution will be prepared with correct dilutions and
concentrations. Fe 3+ will be reduced to Fe2+ with hydroxylamine before adding
o-phenanthroline increasing solubility. To buffer the environment ammonium
acetate d added and interferents like Cu2+, Zn2+ and Ni2+ are minimised by
adding excess hydroxylamine and phosphate by boiling the samples in the
presence of an acid.
Iron(ii) and 1, 10- phenanthroline form a complex that absorbs visible light. The
absorbance of the samples and standards is measured at a wavelength 510nm
using a 1cm cuvette/cell (UV-vis spectrophotometer). Beers law is obeyed for
concentrations within 0.2-4.0 ppm thus absorbance becomes linear with the
concentration to Eq. 1:
A = Ɛlc (1)
Where Ɛ =Molar absorptivity (L mol-1 cm-1)
I= Pathlength
c= Concentration (M)
Fe3+ + 3 phen Fe(phen)32+
APPARATUS AND MATERTIAL
Beakers
100ml volumetric flask (8)
1ml pipette
10ml pipette
125 conical flask (8)
UV-vis spectrophotometer with cuvets
Measuring cylinder
CHEMICALS
Ammonium acetate buffer solution
10% Hydroxylamine hydrochloride solution
1,10-phenathroline solution

PROCEDURE
1.00, 2.00, 5.00, 10.00, 15.00 and 20.00 mL of standard iron solution were
pipetted into separate 125 mL conical flasks and were labelled A- F
respectively. Each of them was filled with distilled water to 50mL mark using a
measuring cylinder. A blank solution of 50mL and 50mL distilled water was
transferred into the same 125mL Erlenmeyer flask using measuring cylinder.
1% of Hydroxylamine hydrochloride solution was then added to the unknown
sample in the 125mL conical flask. The was then heated to boiling for 15mins
until the solution reduces to 17mL and it was then cooled in ice bath.
Thereafter the solution was transferred into a 100mL volumetric flask and
added 10mL of ammonium acetate buffer solution, followed by 4mL of o-
phenanthroline and diluted to the mark with distilled water and mixed
thoroughly. The solution was allowed to settle for 2minutes for colour
development before measuring absorbance. Blank solution and calibration
standards were also prepared by similar procedure. The absorbance of
standards and unknown sample was measured at the wavelength of maximum
absorbance using a spectrophotometer at a fixed wavelength of 510nm. The
reference was the blank solution.
RESULTS

DISCUSSION
This experiment was aimed at determining the concentration of unknown
sample using spectrochemical measurements by spectrophotometric average.
The Fe3+ was reduced to Fe2+ due to excess addition of hydroxylamine
hydrochloride solution and ammonium acetate created a buffer environment
for different concentrations which vary in absorbance. At wavelength 520nm,
the amount of visible light absorbed was directly proportional to the
concentration of the sample. As proven by results above, at first concentration
was 0.0997 ppm with absorbance of 0.038 and as concentration increased to
1.9940 ppm absorbance increased to 0.399. The Beer’s Lambart law relates
concentration to absorbance. During this experiment errors might have been
encountered thus altering the results. Sources of error like, parallax error
when taking the reading from the measuring cylinder whilst measuring the
volume of water. Also, instrumental error on the readings of the UV-vis
spectrometer. The experiment was carried out with care to reduce errors.

CONCLUSION
The ppm of the unknown sample was calculated using the equation y=mx+c
from the graph and was 0.5261 ppm and the equation of the graph is
y=0.1996x. According to The World Health Organization (WHO) recommends
0.3 mg/l (WHO, 1993) as maximum concentration limit of iron in drinking
water.

REFERENCES
Introduction to Spectroscopy Donald L. Pavia - 4th edition 2009
Annem, Screenivasareddy, Determination of Iron Content In Water,2017. All
Capstone projects.
World Health Organisation Determination of Iron In Water Content 1993