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Spectrophotometric Determination of Iron in

Vitamin Tablets
Date:
3rd February 2023.

Lab Partner:
Sarah Harasemiuc.

Aim:
To determine the amount of iron in commercial iron tablets using spectroscopy and
to compare the experimental value with the stated value.

Introduction:
In this experiment, iron from a vitamin pill was dissolved in acid, reduced to Fe(II)
with hydroquinone, and complexed with o-phenanthroline to create a brightly
coloured complex.

2Fe3++C6H6O2⟶2Fe2++C6H4O2+H22Fe 3++C6H6O2⟶2Fe2++C6H4O2+H2

Fe2++3phen⟶[Fe(phen)3] 2+Fe 2++3phen ⟶ Fephen32+

The method used in this experiment was spectrophotometry. Spectrophotometry is a


common method for determining the number of compounds in a solution or the
amount of light absorption is spectrophotometry. The instrument used was the UV-
VIS spectrophotometer (UV-1900i). The amount of iron in a vitamin tablet will be
determined in this experiment by doing a spectrophotometric analysis on the tablet
(Centrum Women,10 mg of iron per tablet). Firstly, the iron will be modified into a
state that absorbs radiation in the visible region. The multivitamin tablet that has
been dissolved in hydrochloric acid will react with 1,10-phenanthroline. Iron doesn't
absorb a lot of light, but when it binds to 1,10-phenanthroline, an extremely stable
reddish-orange compound forms. The current iron ions must be in the Fe(II)
oxidation state for this reaction to take place. A reducing agent called hydroquinone
is added to the solution because Fe(II) is readily oxidized to Fe(III) in the presence of
acid and water. The solutions will be diluted and placed in cuvettes where their
absorbance will be measured. An absorbance vs. is made and the amount of iron in
the original pill can be calculated using the concentration of iron in the solution as a
starting point. This is comparable to the manufacturer's claim of the iron content of
the tablet.
Experimental:
For the preparation of ‘Tablet’ solution, Centrum Women (1.584 g) (multivitamin,
multimineral food supplement) was placed in a 100 cm3 beaker with 25 cm3 6M HCl.
The solution was filtered through filter paper into a 100 cm3 volumetric flask and
made up to the mark with deionised water, labelled “Original Tablet Solution”. 5 cm3
of this solution was pipetted into a 100 cm3 volumetric flask and made up to the mark
with deionised water, this solution was labelled “Tablet”.

For the preparation of the iron (II) standard solutions, 10.00, 5.00, 2.00, 1.00, 0.5,
0.00 cm3 of standard Fe solution was pipetted into 6 separate volumetric flasks. 30
drops sodium citrate solution, 2.00 cm3 hydroquinone solution and 3.00 cm3 of o-
phenanthroline solution was added to each volumetric flasks and made up to the
mark with deionised water and labelled 1,2,3,4,5,6 (in order lowest to highest).

For the preparation of the iron analyte, 10.00 cm3 of ‘Tablet’ solution was pipetted
into 3 separate conical flasks. 30 drops sodium citrate solution, 2.00 cm3
hydroquinone solution and 3.00 cm3 of o-phenanthroline solution was added to each
volumetric flasks and made up to the mark with deionised water and labelled
‘Analyte 1’, ‘Analyte 2’, ‘Analyte 3’.

For the preparation of the Blank Solution, 10.00 cm3 of ‘Tablet’ solution was pipetted
into a 100 cm3 volumetric flask and made up to the mark with deionised water and
labelled ‘Blank’.

For the analysis using UV-Vis spectrometer (UV-1900i), 1 cm3 of each labelled
solution was placed into separate plastic cuvettes (1 cm3) and placed in the UV-Vis
spectrometer where the absorbance was measured.

Results:

Solution Concentration of Fe Absorbance at λmax


(mg)
Blank 0 0.000
Standard 1 0 0.014
Standard 2 0.02 0.050
Standard 3 0.04 0.095
Standard 4 0.08 0.183
Standard 5 0.2 0.435
Standard 6 0.4 0.608
Analyte 1 - 0.102
Analyte 2 - 0.101
Analyte 3 - 0.104
Graph of absorbance at 508nm versus the Concentration of Fe (mg) in the
standards:

Concentration vs. Absorbance


0.5
0.45 y = 1.0642x - 0.0017
0.4 R² = 0.9913
0.35
0.3
Absorbance

0.25
0.2
0.15
0.1
0.05
0
-0.05 0 0.05 0.1 0.15 0.2 0.25 0.3 0.35 0.4 0.45
Concentration (mg)

Calculations:
Discussion:

After carrying out this experiment and observing and calculating the results, the
results seem inaccurate. A tablet containing Fe was dissolved in 6 M HCl. A suitable
aliquot was taken after diluting the resulting solution. The Fe2+ was then combined
with hydroquinone in the solution to change Fe3+ forms to Fe2+. 1.10-o-
phenanthroline was added to create the stable red-orange compound after all the
iron had been transformed to Fe2+. The resulting Fe(phen)32+ complex has an
absorption maxima at 508 nm, therefore determining a solution's absorbance at the
max would indicate how much Fe is present in the solution. The amount of mg
present in the tablet came out to be 4.4 mg while the manufacturers’ claim was 10
mg. These results were not as expected, therefore there must have been an
unknown experimental error or an error made in the calculations, such as the 25 cm3
6M HCl and iron tablet solution not being filtered through the filter paper enough. The
standard deviation, mean and uncertainty @ 95% CI n=6 was also calculated. The
values obtained from these calculations, except the standard deviation, also seem
inaccurate. This may also be due to an unknown experimental error or an error made
in the calculations, such as the 25 cm3 6M HCl and iron tablet solution not being
filtered through the filter paper enough. These results were not as expected as the
experiment carried out quite well so it must have been an unnoticed error.

Comprehension:

1. Briefly outline why is iron required in our diet?


Iron is required in our diet because haemoglobin, a class of protein found in
red blood cells and responsible for transporting oxygen from your lungs to
every area of your body, is heavily reliant on iron. Fatigue results from an
insufficient supply of red blood cells to carry oxygen.

2. Why is the ferric ion first reduced with hydroquinone?


Because Fe(II) and semiquinone radicals are produced as a result of
hydroquinone's reduction of Fe(III). Hydroquinone reduces Fe(III) in acidic
conditions, which then generates semiquinone radicals.

3. Mention two other possible methods for performing this analysis


(include your references).
Another possible method for performing this analysis would be using
colorimetry. By applying the Beer-Lambert equation, which states that the
concentration of a solute is proportional to the absorbance, colorimetry is a
scientific technique used to quantify the concentration of coloured compounds
in solutions.
https://pubs.acs.org/doi/10.1021/ed052p550
The analysis of present iron in a supplement tablet can be done by a redox
titration reaction. In an acidic solution, potassium permanganate can ionize
iron (II) ions to produce iron (III) ions. The potassium permanganate is one of
the most often utilized strong oxidizing agents for the redox titration reaction
(KMnO4).
https://www.ukessays.com/essays/chemistry/experiment-learn-amount-iron-
iron-2913.php
Conclusion:

The aim of this experiment was to determine the amount of iron in commercial iron
tablets using spectroscopy and to compare the experimental value with the stated
value. The iron content of the tablet the manufacturer claims is 10 mg of iron per
tablet and the value of iron obtained by this experiment was 4.4 mg. This difference
in values may be due to an unknown experimental error such as the 25 cm3 6M HCl
and iron tablet solution not being filtered through the filter paper enough resulting in
loss of product, or an error made in calculation. The calculations of the concentration
of iron in the standard solutions seem accurate as they match with many literature
values.

Appendix/ Raw Data:


References:

• https://pubs.acs.org/doi/10.1021/ed052p550
• https://www.ukessays.com/essays/chemistry/experiment-learn-amount-iron-
iron-2913.php
• https://sites.middlebury.edu/chem103lab/2016/09/04/spectrophotometric-
determination-of-iron-in-a-multivitamin/
• http://jupiter.plymouth.edu/~jsduncan/courses/2015_Spring/Techniques/Labs/
08-SpecFeInVitamin.pdf

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