SMJC 2701

ANALYTICAL LABORATORY

NAME : NURSHAFIKA BINTI SHAHLI

PARTNER NAME : 1. RASHIATUN BINTI MOHD RASID
2. NURUL RAQIBAH BINTI RIDWAN
3.ESTHER GANIT PENGIRAN
4. CLERA A/P PETER JOHN
5.JAALYNEE A/P KANNIAPPAN

SECTION : 02

EXPERIMENT NO : 1

EXPERIMENT TITLE : REDOX TITRATION

DATE OF EXPERIMENT : 3 APRIL 2019

LECTURE’S NAME : DR KAMYAR SHAMELI

DEMO’S NAME : 1. MOSTAFA YUSEFI

2.NUR AFINI ISMAIL

1.0 EXPERIMENT NO
1

2.0 EXPERIMENT TITLE

Redox Titration

3.0 OBJECTIVES
After doing the experiment, the students are expected to able to:
1. Student should know to describe a redox in general.
2. A balanced oxidation-reduction, the molarity/normality of the standards potassium permanganate, and
the volume of potassium permanganate.
3.Identify reducing and oxidizing agents in a reaction
4. Calculate concentration from the available titration data.

4.0 INTRODUCTION

Titration is a common method for determining the amount or concentration of an unknown

substance. The method is easy to use if the quantitative relationship between two reacting substances is
known. The method is particularly well-suited to acid-base and oxidation-reduction reactions. In this
experiment, you will conduct two separate redox titrations using a standardized permanganate solution. In
the first titration, you will be trying to find the % hydrogen peroxide in a commercially sold solution. In
the second titration, you will be trying to find the % iron in an unknown iron salt.

Permanganate ion is a powerful oxidizing agent, especially in acidic solution, which can be used
to analyze (by titration) solutions containing many different species. In these titration reactions, the
intensely colored MnO4- ion is reduced to form the colorless Mn2+ ion. Potassium permanganate is a
powerful oxidizing agent because of the high positive charge on manganese, and is used in a wide variety of
chemical analyses of reducing agents such as the determination of iron in iron ore or nitrites in aquarium
water. In this lab we will determine the percent purity of an impure sample of sodium oxalate, Na2C2O4.

Titrations involving permanganate are normally carried out in acidic solutions, and the half reaction
for permanganate under these conditions is:

MnO4-(aq) + 8H+(aq) + 5e-  Mn2+(aq) + 4H2O()

There is one problem with using permanganate ion in titrations, and that is it is able to autocatalyze it's
own destruction. This is because as Mn2+ is produced during the titration, the Mn2+ can actually react with
additional MnO4-, producing solid MnO2 as a result:

3Mn2+(aq) + 2 MnO4-(aq) + 2H2O()  5 MnO2(s) + 4H+(aq)

The unfortunate result of this side reaction is that you overestimate the amount of analyte that is being
consumed because you must add more titrant to reach the endpoint. There are several methods that have
been developed to overcome this difficulty, and we will use the McBride method where the titration is
carried out at an elevated temperature. This speeds up the reaction with oxalate ion, and since the reaction
of Mn2+ with MnO4- is relatively slower, the titration error can be minimized.The oxidation half reaction
in the titration occurs when oxalate ion, C2O42-, is oxidized to carbon dioxide:
C2O42-(aq)  2CO2(g) + 2e-

The combination of half-reactions yields the overall reaction :

5 C2O42-(aq) + 2 MnO4-(aq) + 16 H+(aq)  10 CO2(g) + 2Mn2+(aq) + 8 H2O()

An additional advantage of permanganate titrations is that it serves as its own indicator due to its deep purple
color. The titration is stopped at the first persistent light pink color.
5.0 PROCEDURE
A. Standardization of potassium permanganate solution

1. 2 grams of pure ferrous ammonium sulphate was weighed accurately in a weighing bottle. A 100 cm3
volumetric flask was transfered completely. The weighing bottle and others was rinsed with distilled
water and poured into the volumetric flask. 10 cm3 of diluted sulphuric acid was added and when all the
salt has dissolved, more distilled water was added to the mark. Shaked until you get homogenous
solution.

2. 20 cm3 potassium permanganate solution provided was diluted to about 250 cm3. The solution was
homogenous.

3. 20 or 25 cm3 of the standard solution form (1) was pipette and it was transfered to an Erlenmeyer
flask. 10 cm3 dilute sulphuric acid was added. Potassium permanganate was titrated until permanent
faint pink colour is observed.

4. The concentration of the potassium permanganate solution was calculated.

5. Three times was repeated. The deviation between two volumes should not exceed 3 units per
thousand.
B. Determination of molecular weight of oxalic acid

1. Three samples of oxalic acid was weighed accurately, the mass should be approximately
0.1 g. Each was putted into an Erlenmeyer flask and 10cm3 of diluted sulphuric acid was
added in each one and it was diluted to about 100 cm3 with distilled water.

2. The solution was heated until approximately 80 celcius (steaming hot) and titrated it with
potassium permanganate solution solution from (A).

3. The molecular weightof oxalic with the number of molecules of water was calculated.
6.0 RESULTS AND CALCULATION

A. Standardization of KMnO₄

Reading taken 1 2 3

Initial Reading(cm3) 0.00 0.00 0.00

Final Reading (cm3) 25.40 25.60 25.90

Total Volume(cm3) 25.40 25.60 25.90

Average Volume(cm3) 25.63

Standard deviation 0.25

B. Determination of Molecular Weight of Oxalic Acid

Reading taken 1 2 3
Initial Reading KMnO₄ (cm3) 0.00 0.00 0.00
Final Reading KMnO₄ (cm3) 28.70 27.1 26.0
Total Volume KMnO₄ (cm3) 28.70 27.1 26.0
Mass of Oxalic Acid(g) 0.10 0.10 0.10

Calculations
Part A: Standardization of KMnO₄
2
∑(𝑣1 −𝑣𝑎𝑣𝑔 )
Standard deviation = √ 𝑛−1

(25.40−25.63)2 +(25.60−25.63)2 +(25.90−25.63)2

=√ 3−1
 = 0.25
(Fe2+ Fe3+ + e-) ×5 oxidation
MnO4- + 8H+ + 5e- Mn2+ + 4H2O reduction
___________________________________________________________________________

MnO4- + 5Fe2+ + 8H+ Mn2+ + 5Fe3+ + 4H2O overall process

Formula of iron(II) ammonium sulphate salt: FeSO4(NH4)2•SO4•6H20

Molecular weight: 392.13g/mol
𝑚𝑎𝑠𝑠
No.of mole = 𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡
2𝑔
=392.13𝑔/𝑚𝑜𝑙

=5.10×10−3 𝑚𝑜𝑙
𝑚𝑜𝑙𝑒
Amount of 𝐹𝑒 2+ , molarity =𝑣𝑜𝑙𝑢𝑚𝑒

5.10×10−3 𝑚𝑜𝑙
= 0.1𝑑𝑚3

=0.051mol/𝑑𝑚3
From the balanced equation, 5mol of Fe will react with 1mol of 𝑀𝑛𝑂4 − , therefore
𝑀𝐹𝑒 𝑉𝐹𝑒 5
=
𝑀𝑀𝑛𝑂4 − 𝑉𝑀𝑛𝑂4 − 1

0.051mol/𝑑𝑚3 ×0.025𝑑𝑚3
=5
𝑀𝑀𝑛𝑂4 − ×0.02663𝑑𝑚3

𝑀𝑀𝑛𝑂4− , 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑀𝑛𝑂4 − = 9.575 × 10−3 𝑚𝑜𝑙/𝑑𝑚3

Part B : Determination of Molecular Weight of Oxalic Acid

{𝑀𝑛𝑂4 − + 8𝐻 + + 5𝑒 − → 𝑀𝑛2+ + 4𝐻2 𝑂} × 2 ( reduction process)

{𝐶2 𝑂4 2− → 2𝐶𝑂2 + 2𝑒 − } × 5 (oxidation process)

2𝑀𝑛𝑂4 − + 16𝐻 + + 5𝐶2 𝑂4 2− → 2𝑀𝑛2+ + 8𝐻2 𝑂 + 10𝐶𝑂2 (𝑜𝑣𝑒𝑟𝑎𝑙𝑙 𝑝𝑟𝑜𝑐𝑒𝑠𝑠)

Molecular weight, MW1 of oxalic acid

 𝑚𝑜𝑙𝑒 𝑜𝑓 𝑜𝑥𝑎𝑙𝑖𝑐 𝑎𝑐𝑖𝑑 5
=
𝑚𝑜𝑙𝑒 𝑜𝑓 𝑀𝑛𝑂4 − 2
𝑚𝑎𝑠𝑠 𝑜𝑓𝐶2 𝑂4 2−
𝑀𝑤1 𝑜𝑓 𝐶2 𝑂4 2− 5
=
𝑀𝑀𝑛04 𝑣𝑀𝑛𝑂4
− − 2
1000
𝑚𝑎𝑠𝑠 𝑜𝑓𝐶2 𝑂4 2−
𝑀𝑤1 𝑜𝑓 𝐶2 𝑂4 2− 5
=
𝑀𝑀𝑛04 − 𝑣𝑀𝑛𝑂4− 2
1000
0.1𝑔
𝑀𝑤1 5
−3 =
9.575 × 10 × 28.70 2
1000
𝑴𝒘𝟏 = 𝟏𝟒𝟓. 𝟓𝟒 𝒈/𝒎𝒐𝒍

Molecular weight, MW2 of oxalic acid

𝑚𝑜𝑙𝑒 𝑜𝑓 𝑜𝑥𝑎𝑙𝑖𝑐 𝑎𝑐𝑖𝑑 5
=
𝑚𝑜𝑙𝑒 𝑜𝑓 𝑀𝑛𝑂4 − 2
𝑚𝑎𝑠𝑠 𝑜𝑓𝐶2 𝑂4 2−
𝑀𝑤2 𝑜𝑓 𝐶2 𝑂4 2− 5
=
𝑀𝑀𝑛04 − 𝑣𝑀𝑛𝑂4− 2
1000
𝑚𝑎𝑠𝑠 𝑜𝑓𝐶2 𝑂4 2−
𝑀𝑤2 𝑜𝑓 𝐶2 𝑂4 2− 5
=
𝑀𝑀𝑛04 − 𝑣𝑀𝑛𝑂4− 2
1000
0.1
𝑀𝑤2 5
=
9.575 × 10−3 × 27.1 2
1000
𝑴𝒘𝟐 = 𝟏𝟓𝟒. 𝟏𝒈/𝒎𝒐𝒍
Molecular weight, MW3 of oxalic acid
𝑚𝑜𝑙𝑒 𝑜𝑓 𝑜𝑥𝑎𝑙𝑖𝑐 𝑎𝑐𝑖𝑑 5
=
𝑚𝑜𝑙𝑒 𝑜𝑓 𝑀𝑛𝑂4 − 2
 𝑚𝑎𝑠𝑠 𝑜𝑓𝐶2 𝑂4 2−
𝑀𝑤3 𝑜𝑓 𝐶2 𝑂4 2− 5
=
𝑀𝑀𝑛04 − 𝑣𝑀𝑛𝑂4− 2
1000
𝑚𝑎𝑠𝑠 𝑜𝑓𝐶2 𝑂4 2−
𝑀𝑤3 𝑜𝑓 𝐶2 𝑂4 2− 5
=
𝑀𝑀𝑛04 − 𝑣𝑀𝑛𝑂4− 2
1000
0.1
𝑀𝑤3 5
=
9.575 × 10−3 × 26.0 2
1000
𝑴𝒘𝟑 = 𝟏𝟔𝟎. 𝟔𝟕 𝒈/𝒎𝒐𝒍

145.54+154.10+160.67
Average molecular weight of oxalic acid, 𝐶2 𝑂4 2− = 3

= 153.43 g/mol

Theoretical molecular weight of oxalic acid, 𝐶2 𝑂4 2− = 90.03g/mol

Percentage error of molecular weight
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡−𝑎𝑣𝑒𝑟𝑎𝑔𝑒 𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡
=| | × 100%
𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡

90.03−153.43
=| | × 100%
90.03

= 70.43 %
7.0 DISCUSSION

After calculating the concentration of the oxalic acid solution using the values of three distinct
titrations, it was found that all the results lie within the 70.43 % calculated error range. This accuracy
comes from the neat, simple and effective design of the experiment. Moreover, the permanganate redox
titration is exceptionally reliable because of the sharp colour change that greatly decreases the inaccuracy
of the judgment of the equivalence point. It should also be mentioned that no additional indicators
interfered with the reaction.

Nevertheless, there are several limitations and sources of error that must be taken in account
before reflecting on the success of the experiment. The first and most important limitation is the slight
scatter in the volume of permanganate required for titration. The third titration is 26.0 cm3 below the first
two, a difference the size of the error bar. This limitation may be caused by the slow dissolution of the
remaining permanganate crystals in the solution. Indeed, it was noted during the raw data collection that
some crystals were not fully dissolved when the titration was carried out. As the phenomenon takes place,
the concentration of the permanganate solution increases hence less volume is required for titration. A
possible solution is to wait longer, or use a magnetic stirrer so as to fully dissolve all the crystals in the
solution before carrying out the titration. This will allow the solution to remain at a constant concentration
and will improve the reliability of the experiment.

Moreover, another limitation is the difficulty in judging on the position of the meniscus in the
burette. The bright colour of the solution decreased the visibility and the accuracy of the titration
readings. By taking more readings and repeating the titration a number of times, it is possible to decrease
the effect of this systematic error. Other than that, it is important to mention the possible effects of
uncontrolled factors in the environment, the context, or even the chemistry taking place. Indeed,
temperature, humidity, pressure or luminosity may change the outcome of the experiment. In this case, we
are especially concerned with any factor that may have caused the decay of the permanganate solution
into more complex compounds that would react differently.

By carrying out the whole experiment in a controlled environment, it is possible to minimize

the effects of such factors. Luminosity and temperature, for example, can easily be kept constant by
running the titration in an isolated environment.
 Last but not least, despite the inevitable effects of these limitations, the results of the
experiment lie within the calculated error bars. The concentration of the oxalic acid solution was found to
be 70.43 % error bar. The experiment is a quite success since it was well controlled and performed. We
can have good confidence in the result.

8.0 Precaution steps

1. This experiment uses sulfuric acid, which is very corrosive. Wear personal protective gear and get an
lab assistant to guide you.
2. Always work in a well ventilated area.
3. Potassium permanganate is a skin and eye irritant and will stain clothing and skin.
4. Make sure no air bubbles are present in the burette while the titrant is being filled in the burette
5. Make sure the end point of the reaction is achieved before ending the titration
6. Swirl the reaction mixture gently to ensure complete mixing of reagents

9.0 Conclusion

The purpose of the laboratory exercise was to perform an oxidation/reducation titration

between a standardized solution of potassium permanganate and an unknown iron (II) sulfate solution in
order to determine the concentration of the latter. The permanganate ion in the titrant was reduced to
Mn2+ and the Fe2+ in the analyte was oxidized to Fe3+. Everything was done in a solution acidified by
sulfuric acid so that the MnO4- would get reduced to Mn2+ and the extra oxygen atoms could form water.
From the titration data and the balanced oxidation/reduction equation the normality and molarity of the
FeSO4 solution were gotten.

Overall, it is unlikely that error played a major role in the experiment. The three values for the
molecular weight of the oxalic acid were very close, 145.54 g/mol 154.1 g/mol, and 160.67 g/mol and the
results were precise. A more likely source of error is the oxidation/reduction reaction between the iron
sulfate and oxygen in the air. Oxygen got reduced and reacted with H+ in the analyte to form water while
the Fe2+ in the FeSO4 analyte got oxidized to give Fe3+. Because the newly formed Fe3+ did not react
with the potassium permanganate, less potassium permanganate was added than was needed to oxidize all
the Fe2+ originally present in solution. Thus, the actual molarity of the FeSO4 solution was probably
higher but the spontaneous reaction of the solution with air made it appear lower than it really was. This
can be avoided by performing the reaction in a vacuum.

10.0 Reference
1. https://www.mikeblaber.org/oldwine/chm1046/notes/Electro/Balance/Balance.htm

2. https://www.scribd.com/document/290038370/Report-4-Redox-Titration

3. http://faculty.uml.edu/james_hall/84124/16.htm

4. https://www.coursehero.com/file/9422043/Experiment-9-Lab-Report/

5. https://www.scribd.com/document/290038370/Report-4-Redox-Titration

11.0 QUESTIONS

1. Potassium permanganate is a good oxidation agent compared to other elements such as fluorine,
chlorine and potassium dichromate. Explain why?
For any substance to be able to be an oxidising agent ,it should be able to accept electrons. A definition is
,for any substance to be an oxidising agent, it should donate oxygen atoms. For Permanganate ion the
molecular formula is MnO4- ,it is negatively charged . The oxidation state of Mn is +7 . That is,it needs 7
electrons to achieve it’s element form Mn. Now,going to our first definition of an oxidising agent,we see
that the permanganate ion accept a lot of electrons and hence a strong oxidising agent.

2.Indicate the form of manganease(Mn) produced when the above reaction takes place under the
following condition :

a) Acidic : 2MnO4- + 16H+ + 10e-  2Mn2+(aq) + 8H2O(l)

b) Basic : 2MnO4-(aq) + 4H2O(l) + 6e-  2MnO2(s) + 8OH-(aq)

3. Why it necessary to heat the oxalic acid solution before titrating it with the potassium
permanganate solution ?
The oxalic acid is heated to increase the rate of reaction which is very slow at room temperature.
4. Balance the equation given:-
I. 6𝐹𝑒 2+ + 𝐶𝑟2 𝑂7 2−
+ 14H+ 6 𝐹𝑒 3+ + 𝐶𝑟 3+ +7 H2O

II. 𝐻3 𝑆𝑂4 + 2𝐼 − + 2𝐻 + 𝐻3 𝐴𝑆𝑂3 + 𝐼3 +H2O