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Experiment: Redox Titration and Determination of Percent Iron (Fe)

20 February 2014
Abstract

The purpose of this experiment was to standardize Potassium Permanganate
(KMnO
4
) in order to determine the percent of iron in the sample. In the first part of this
experiment we needed to standardize the Potassium Permanganate through a titration
process. After standardizing the KMnO
4
it was determined that the average molarity was
0.0158 mol. This information was then used for part two of the experiment to determine
the amount of Iron in the unknown sample. The unknown iron sample was titrated with
the standardized potassium permanganate. Upon completing the second part of this
experiment the calculated average percent of Iron in the sample was 13.66%. Our
hypothesis was accepted because we were able to use titration techniques to both
standardize the potassium permanganate and determine the percent of iron in an unknown
sample.

Introduction

A reduction-oxidation reaction (redox) is a reaction that involves elements that
transfer electrons to one another.
Ref-2
In a redox reaction there are two different possible
products. A product is said to have been reduced if during the reaction it gained
electrons. A product is said to have been oxidized if during the reaction it had lost the
electrons. The reactant that has lost electrons during a reaction is said to be the reducing
agent, while the reactant that gains electrons is known as the oxidizing agent.
Ref-2

Because of the laws of conservation, the number of electrons that a product gains must be
the same as the number of electrons that have been lost by the reactant. An important step
during redox reactions is determining the spectator ion. A spectator ion is an element that
does not change its oxidation state in a reaction.
Ref-2
This is important because the
oxidation states allow us to determine which element is oxidizing and which element is
reducing. We can determine which element is experiencing either oxidation or reduction
by comparing their oxidation sates before and after the reaction by observing which
element gains or loses electrons
Ref-1

The titration technique that took place to standardize a product is a little different
compared to the titration technique used to find the percent of an element. In order to
determine the molarity of the Iron in the sample, we first needed determine the molarity
of KMnO
4
. In order to do this, the KMnO
4
needed to have Sodium Oxalate added to it so
that it could become standardized. Additionally, we did not have to add an indicator
because the Potassium Permanganate acted as its own indicator when the end point was
reached.
During this experiment we hypothesized that we can use a titration technique to
standardize KMnO
4
. We also hypothesized that the percent of Iron can be determined in
the sample by using a titration technique similar to the ones in previous experiments.

Materials and Methods

Reference Redox Titration and Determination of % Fe handout given by Dr. Mare
Cudic.

Data

Table 1: Standardization of KMnO
4

Trial 1 Trial 2 Trial 3
Vol Na
2
C
2
O
4
(mL) 10 10 10
Initial Buret (mL) 8.4 9.8 11
Final Buret (mL) 9.8 11 12.2
Vol KMnO
4
(mL) 1.4 1.2 1.2
Moles C
2
O
4
(mol) 5x10
-5
5x10
-5
5x10
-5

Moles KMnO
4
(mol) 2x10
-5
2x10
-5
2x10
-5
Molarity KMnO
4
(M) 0.01422 0.0166 0.0166
Average Molarity(M) 0.015873



Table 2: Determination of Iron (II) Percentage
Trial 1 Trial 2 Trial 3
Mass of Fe sample (g) 0.3693 0.3241 0.3843
Initial Buret (mL) 12.2 23.4 33.2
Final Buret (mL) 23.4 33.2 45.2
Vol KMnO
4
11.2 9.8 12
Moles KMnO
4
1.792x10
-4
1.568x10
-4
1.92x10
-4
Moles Fe(II) 8.96x10
-4
7.84x10
-4
9.6x10
-4
Mass of Sample Fe 0.0500 0.0437 0.0536
% Fe in Sample 13.54% 13.48% 13.95%
Average 13.66%



Calculations

Table 1 Trial 1:
Vol KMnO
4
= final buret (mL) initial buret (mL)
o 9.8 8.4 = 1.4 mL
Moles of C
2
O
4

o 0.05 x 0.0005 = 5x10
-5

Moles of KMnO
4
= moles of C
2
O
4
* (4/5)
o 5x10
-5
* (4/5) = 2x10
-2

Molarity KMnO
4
= (moles KMnO
4
) / vol KMnO
4

o 2x10
-2
/ 0.0014 = 0.0143
Average Molarity = (Molarity Trial 1 + Molarity Trial 2 + Molarity Trial 3) / 3
o (0.0143 + 0.0166 + 0.0166) / 3 = 0.0158






Table 2 Trial 1:
Vol KMnO
4
= final buret (mL) initial vuret (mL)
o 23.4 12.2 = 11.2
Moles KMnO
4
= average mol. KMnO
4
* vol. KMnO
4

o 0.0158 * 0.0112 = 1.792x10
-4

Moles Fe(II) = moles KMnO
4
*5
o 1.792x10
-4
* 5 = 8.96x10
-4

Mass of Sample Fe = mol Fe * mFe
o 8.96x10
-4
* 55.85 = 0.0500
% Fe in Sample = (Mass of sample Fe / Mass of Fe sample) * 100
o (0.0500 / 0.3693) * 100 = 13.54%

Discussion

The purpose of this experiment is to standardize Potassium Permanganate so we
can determine the percent of iron in the sample. For the first part of this experiment we
needed to standardize KMnO
4
. A redox titration technique was performed to find the
molarity of KMnO
4
. Sodium oxalate was mixed with sulfuric acid and water and then
heated to 60 degrees Celsius so that it can be titrated with the potassium permanganate.
We did not need to add an indicator like phenolphthalein to this experiment because the
permanganate acts as its own. When the endpoint (color change) was reached we
calculated the amount of permanganate that was added so that we can determine the
molarity of KMnO
4
. After completing this step the average molarity of KMnO
4
was
determined to be 0.0158 M. It is important to convert mL to L so that we can get the
proper Molarity for the next step of the experiment. Data table 1 shows the calculations
for the standardization of KMnO
4
.
After determining the molarity of the KMnO
4
we could then begin the titration of
the Iron salt to determine the percent composition of Iron. First we dissolved a sample of
iron salt into water and then we added both sulfuric and phosphoric acid. The reason we
added acid to both parts of the experiment is because we needed to ensure that the
experiment occurs under acetic conditions. The reason we added the phosphoric acid was
because the reaction of the iron ion can hinder our ability to see the endpoint. As the
redox reaction occurs the iron II becomes iron III that has a brown color. This color can
interfere with the pink color of the end point and the phosphoric acid neutralizes the
coloration allowing us to accurately see the endpoint. When the end point was reached,
an average of 11 mL of KMnO
4
was dispensed. The average moles of KMnO
4
in the
three trials was 1.76x10
-4
, the average moles of Fe in all three trials was 8.8x10
-4
. We
were then able to calculate the % Fe in the sample. To do this, the mass of the iron in the
sample was divided by the entire mass of the sample and multiplied by one hundred. The
average percent of Iron in the sample was 13.66%. Data table 2 shows the calculations
that we used to determine the percentage of Iron II in the sample.

Conclusion

The hypothesis that we can use a titration technique similar to the ones in
previous experiments to standardize KMnO
4
and to determine the percentage of Iron in
the sample was accepted. This was accepted because we were able to accurately
determine the average molarity of KMnO
4
. This molarity was then used in determining
the percentage of Iron in the sample that was taken. The average molarity of KMnO
4
was
determined to be 0.0158. The average percent of Iron II in the sample was calculated to
be 13.66%. One error that could have occurred during this experiment involved heating
of the mixtures. If the trials had different temperatures this could have influenced how
much of the KMnO
4
was absorbed. Another possible error that could have influenced our
results is when it came time to reading the buret. If the amount dispensed was calculated
incorrectly then the results could have been heavily influenced by that.
Literature Cited
1
Tro, N. (2010). Principles of chemistry: A molecular approach. (2nd ed., pp.151-158).
Illinois: Pearson.
2
Redox Titration and Determination of Percent Iron www.nova.edu/~giarikos