1

Redox Titration: Determination of % Fe

2+
in an Unknown Salt
Igor Soloninko
School of Mathematics and Science, CCBC Essex, 7201 Rossville Boulevard, Baltimore, MD
21237
October 1, 2014
Abstract
This experiment is used to gain the knowledge and understanding of redox titration and how
to use it to determine molarity of a substance and percent of iron(II) in an unknown sample.
Also, this experiment includes the use of titration in elevated temperature, this is crucial
because when titrating there are 2 things that need to be looked out for. There are two parts
for this, first part is to determine the molarity of KMnO
4
solution using redox titration at
elevated temperature. In this experiment the molarity was determined to be 0.01780 M
KMnO
4
. The second part was to determine % Fe
2+
in unknown sample, using redox titration.
Using the molarity of the KMnO
4
solution from the first part percent iron(II) in the unknown
sample was calculated to be 11.76%
Introduction
Titration is defined as gradual addition of one solution to another until the chemical
amount of one reactant being added matches stoichiometrically the amount of another
reactant in the solution initially present.
2
Titration traces back all the way to the 18
th
century,
the very first burette was made in France by a guy named Francois Antoine Henri Descroizilles
2
.
Karl Freiderich Mohr wrote the first book about titration in 1855 and he is responsible for
advancing the burette to the one we use today.
2

There are many uses for redox titrations, one of those uses is to determine the amount
of vitamin C there is in a green pepper when its raw, steamed, boiled, etc.
1
The titration that
was done to determine vitamin C in green pepper brought up one major problem with titration.
Since the paper is cooked the color of the solution is never consistent, this brings up a problem
because when a student goes to titrate he or she does not know when that slight color change
happens and over or under titrates the solution. The student kept on getting very inconsistent
values. To solve this problem a filter was used on the solutions to give them a consistent color
of light yellow or green so they can easily tell when it turns slightly blue.
1

Several objectives and goals were achieved through that completion of this experiment.
Determining the molarity of KMnO
4
and percent iron(II) of unknown sample through the use of
titration were the two objectives that were achieved in the experiment. Also, gaining
experience doing redox titration and titration on elevated temperature
3
were some of the goals
that have been achieved through this experiment.
2

Experimental Section
Equipment/Materials: 50-mL buret, 250-mL volumetric flask, 250-mL Erlenmeyer flasks (4), 25-
mL pipet, 50-mL graduated cylinder, buret clamp, ring stand, hotplate, thermometer, KMnO
4

solution, 1.25 M H
2
SO
4
, Na
2
C
2
O
4
(s), unknown iron(II) salt, H
3
PO
4
solution
Procedure
Standardizing KMnO
4
solution: Weigh out 1.2 g 1.3 g of Na
2
C
2
O
4
, make sure measurement is
up to 0.1 mg accuracy. Take the pure sodium oxalate and transfer it in to a 250-mL volumetric
flask, add some distilled water to it and shake it till the solid is completely dissolved. Then fill
the volumetric flask to 250-mL mark with distilled water. Next, Pipet 25.00 mL of the Na
2
C
2
O
4

solution in to 4 Erlenmeyer flasks, one being a rough and 3 trails and add 50.0 mL of 1.25 M
H
2
SO
4
to each flask. Heat the solutions on a hotplate until they reach 80C 90C. While they
are heating prepare the buret by cleaning it with distilled water and then rinsing it with roughly
10 mL of KMnO
4
. Fill the buret with the KMnO
4
solution a little pass the 0 mark and drain some
to get rid of any air bubbles in the tip, record the initial reading of the buret. After the Na
2
C
2
O
4

solution reaches the desired temperature begin titrating, make sure that the Na
2
C
2
O
4
solution
does not get below 70C will titrating. If the solution starts to get cool stop titrating and put it
back on the hotplate for a bit. When the solution turns faint pink and persists for about 30
seconds the titration is over and the final buret reading should be recorded. This should be
done to all of the Na
2
C
2
O
4
solutions in the Erlenmeyer flasks to get the average volume titrated.
After all the solutions have been titrated prepare a solution consisting 50.0 mL of 1.25 M H
2
SO
4

and 50.0 mL of distilled water then titrate it at the same temperature as the other trails. This
titration should be complete after 1 or 2 drops of KMnO
4
, if more is needed then subtract the
volume of this titrations from the other trails. Finally, with all the determined information
calculate molarity of KMnO
4
.
Determining % Fe
2+
in soluble salt: Weigh out 5 g 6 g of the unknown, make sure
measurement is up to 0.1 mg accuracy. Take the unknown salt and transfer it in to a 250-mL
volumetric flask, add some distilled water to it and shake it till the solid is completely dissolved.
Then fill the volumetric flask to 250-mL mark with distilled water. Next, pipet 50.00 mL of the
unknown solution into 4 250-mL Erlenmeyer flasks as before. Then, to each flask add 20.0 mL of
1.25 M H
2
SO
4
and 5.0 mL of H
3
PO
4
solution as precisely as possible. As before, clean the buret
and then fill it with KMnO
4
solution making sure all the air bubbles are out of the buret. Titrate
each of the unknown solutions until it turns pink and stays for about 30 seconds upon swirling.
After all of the titrations are complete calculate the % Fe
2+
in the sample.
Results and Discussion
Mass of Sodium Oxalate: 1.2004 g
Chemical equations
3

5C
2
O
4
2-
(aq)
+2MnO
4
-
(aq)
+16H
-
(aq)
2Mn
+
(aq)
+10CO
2(g)
+8H
2
O
KMnO
4
K
+
+MnO
4
-

Na
2
C
2
O
4
2Na
+
+C
2
O
4
2-

Table 1: Titration of KMnO
4

Buret Reading Rough Trail 1 Trail 2 Trail 3
Final (mL) 19.15 39.65 27.80 47.70
Initial (mL) 0.00 19.15 8.00 27.60
Volume dispensed (mL) 19.15 20.50 19.80 20.10
Average volume (mL) 20.13
Molarity of KMnO
4
:

) (

) (

) (

)
(

) (

)
Deviation: | |

Deviation
Trail 1 0.37 mL
Trail 2 0.33 mL
Trail 3 0.03 mL
Average Deviation 0.24 mL
RMD:



According to the data from table 1 average volume used for titration was 20.13 mL. The
average deviation of 0.24 mL and RMD shows that the results were very imprecise. Whenever a
titration is done the deviations should be very small, the large deviation indicates a big percent
error in the final result. For this part of the experiment it was important to keep the
temperature of the solution above 70C, it is very difficult to keep the temperature up and
cautiously titrate the solution, therefore an error could have occurred when the solution fell
below the required temperature.
Table 2: Volume of KMnO
4
used
Buret Reading Rough Trail 1 Trail 2 Trail 3
Final (mL) 19.70 44.50 22.50 46.15
Initial (mL) 0.00 19.70 0.00 22.50
Volume dispensed (mL) 19.70 24.80 22.50 23.65
Average Volume (mL) 23.65
4

Chemical Equations
MnO
4
-
(aq)
+8H
+
(aq)
+5Fe
2+
(aq)
Mn
2+
(aq)
+4H
2
O
(l)
+5Fe
3+
(aq)

KMnO
4
K
+
+MnO
4
-

Mass of Unknown Fe #6: 5.0004 g
Grams Fe used:

) (

) (

)
(

Grams Fe salt used: (


)
% Fe
2+
in soluble compound: (


)

Deviation
Trail 1 1.17 mL
Trail 2 1.15 mL
Trail 3 0 mL
Average Deviation 0.77 mL
RMD: 33
The huge deviation and RMD indicate the results were all over the place and most likely quite
inaccurate. Not following directions all the way though could have caused the error in the
results. It was very important to get the 5.00 mL of H
3
PO
4
as accurate as possible when adding
it to the flasks with the unknown solution. Not enough care was put into adding the H
3
PO
4

solution to the unknown causing the titration to be spread out from trail to trail.
Conclusion
The first part of the experiment was used to determine the molarity of the KMnO
4

solution, which was calculated to be 0.01780 M. The second part of the experiment was used to
determine the main purpose of the experiment, which is to determine the % Fe in unknown
sample. The resulting data and calculations indicated that the % Fe in the unknown sample #6
was 11.76%.
Through this experiment one can conclude that there are way to determine the amount
of certain substance in unknown sample is present.
This method had its drawbacks and advantages. One of the bigger draw backs was that
it was very difficult keeping the substance above 70 degrees Celsius in air conditioned room.
However, titration is a very good system for this type of experiment because it is easier to get
the mixture to the accuracy of a single drop.
5


References
1. Deal, S. T., & Pope, S. R. (1996). Improved end point detection in the redox titration of
vitamin C in green peppers. Journal of Chemical Education, 73(6), 547. Retrieved
from http://search.proquest.com/docview/211991212?accountid=3784
2. "History." Titration. Creative Commons Attribution, n.d. Web. 26 Sept. 2014.
<http://chemteacher.chemeddl.org/services/chemteacher/index.php?option=co
m_content&view=article&id=56>.
3. Chemistry 124 Experiments, Hamilton, P. Ed. CCBC Printing: Baltimore MD. 2014
pg. 54-57