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FACULTY OF APPLIED SCIENCES

DIPLOMA IN SCIENCE
AS120

CHM256

LABORATORY CASE STUDY


DETERMINATION OF CONCENTRATION OF KMnO4 SOLUTION USING OXALIC
ACID

STUDENT NAME STUDENT ID GROUP

MIRZA KARMILA BINTI ALIZAS 2019428458


CHM2564G2
NURUL IZZATI BINTI RUSLI 2019646266

PREPARED FOR MADAM DIANA BINTI INDIM@HINDIN


DETERMINATION OF CONCENTRATION OF KMnO4 SOLUTION
USING OXALIC ACID

1. OBJECTIVE
The main objective of this case study is to determine the concentration of potassium
permanganate (KMnO4) solution using titration against a standard solution of oxalic acid.

2. ABSTRACT
Determining the concentration of a solution is important before starting an experiment. A
solution with an unknown concentration must be standardized in order to find out its exact
concentration value. Therefore, a proper and exact amount can be used for an experiment to react
properly. This experiment will determine the concentration of potassium permanganate solution
by using oxalic acid, with a method known as titration. The results expected are based on the
volume of potassium permanganate used, it will be used to calculate the molarity. This result will
define the exact amount of potassium permanganate needed in a specific solution for a reaction
to work. At the end of the experiment, there is 0.05 M of KMnO4 based on the average obtained
from two trials. Overall, this experiment will increase the knowledge of calculating a
concentration of a solution using titration methods.

3. INTRODUCTION
Titration is the process of analyzing a chemical. There, the desired sample is needed in a
quantity where it can be added to another solution with a known concentration, amount, and
proportion. Titration is performed by constantly or continuously adding a standard solution. The
solution should be a titrating reagent. Then, it is added into a burette, to be added, it must be with
a known concentration to continue an experiment, otherwise, it cannot be done.

By constantly adding a standard solution into another solution, the “Endpoint” plays an
important role in getting the right calculations and the right number of moles. The “Endpoint”,
where the solution changes its color, is the final sign that shows the chemical reaction has
finished and no more reaction will occur. Below is an example of a titration set up for an
experiment:
Figure 1: Example of a titration set-up for an experiment from
https://classnotes.org.in/wp-content/uploads/Apparatus-of-Titration.jpg

Figure 2: Chemical equation of titration using Oxalic Acid from


https://labmonk.com/wp-content/uploads/2017/12/120517_1536_Preparation2.png

Theoretically, potassium permanganate is a strong oxidizing agent that becomes even


more effective when combined with an acid. In this experiment, permanganate ions are purple.
However, the solution contains manganese ions, Mn2+, which is a colorless solution. That is
why the solution (that reacts with KMnO4) becomes decolorized. Any excess potassium
permanganate in the solution will turn it into purple because there is longer acid to reacts with.
4. METHOD/PROCEDURE

4.1 Materials and apparatus


Materials and apparatus required to operate this experiment are oxalic crystals,
potassium permanganate,𝐾𝑀𝑛𝑂4, diluted sulphuric acid (𝐻2𝑆𝑂4), distilled water,

electronic balance, weighing bottle, spatula, 250 ml beaker, 250 ml standard flask, 250 ml
conical flask, glass rod, funnel, test tubes, dropper, 50 ml burette, burette stand, 20 ml
pipette, and hot plate.

4.2 Procedure
A. Preparation of 250ml, 0.1 molar standard solution of oxalic acid

Firstly, the weighing bottle was placed on the electronic balance and the balance
was tared. Then, the oxalic acid was taken by using the spatula and was transferred into
the weighing bottle. About 3.15 g of oxalic acid was weighed and transferred into the
250ml beaker. The weighing bottle was washed 2 to 3 times with distilled water in order
to transfer it into the beaker.Next, the oxalic acid crystal was dissolved in the beaker by
gently stirred with the clean glass rod.
The entire solution was then transferred from the beaker into the 250ml flask by
using the funnel and glass rod. Soon, the beaker, glass rod, funnel and the funnel tip were
washed 2 to 3 times with distilled water to be certain none of the solution has stuck to the
equipment and that all solution has been transferred to the standard flask. Then, enough
distilled water was added carefully to the standard flask to reach just below the
calibration mark. The last few drops of distilled water were added with the dropper until
the lower level of the calibration mark. Lastly, The measuring flask was stoppered and
gently shook to make the solution uniform throughout.

B. Determination of concentration of KMnO4 using a standard solution of oxalic acid


Firstly, the burette was taken and rinsed with distilled water. The water then was
drained and the process was repeated 2 to 3 times to drain out the impurities from the
burette. Then, a small volume of KMnO4 solution was poured into the burette through
the funnel and then the burette was rinsed as well as the solution was drained out. This
process was repeated 2 to 3 times to remove any moisture inside the burette. Next, the
funnel was used to fill the burette with KMnO4 solution to just above the zero mark.the
beaker then was taken and placed below the burette and the stopcock was opened slowly
so that the KMnO4 solution is allowed to run out into the beaker. Then, the initial burette
reading was set as zero.

Next, the 20 ml pipette was taken and a small volume of distilled water was
pipetted out. The distilled was then rinsed out and the water was drained. This process
was repeated 2 to 3 times to remove the impurities from the pipette. After the water was
rinsed, a small volume of oxalic acid solution was pipetted out and was rinsed as well as
drained. This step was repeated 2 to 3 times to remove any moisture inside the pipette.
Then, the oxalic acid solution was pipetted out from the standard flask until the solution
level is just above the calibration mark on the pipette.

After that, the upper end of the pipette was closed with the index finger as shown
in figure 3 below. Next, the finger was slowly released so that the solution is allowed to
run slowly until the lower edge of the meniscus just touches the mark on the pipette so
that the volume of the solution becomes 20ml. Soon, the 20ml oxalic acid solution was
carefully transferred into the clean conical flask. The tip of the pipette with the bottom of
the conical flask was touched to transfer the remaining solution from the pipette. Then,
about 20 ml which is a test tube full of dilute sulphuric acid, H2SO4 was added to the
oxalic acid solution in the conical flask.

Later, the flask was placed over the hot plate and the content of the conical flask
was heated to 60-70 degrees celsius. After that, the conical flask was placed on the white
surface of the stand under the burette to correctly view the color change. Next, the
KMnO4 solution was run dropwise from the burette into the conical flask with constant
shaking of the solution. This process was continued until the color of the solution
changed from colorless to light pink in addition to the last single drop of KMnO4. Then,
the final burette reading was noted down and the same procedure was repeated until the
concordant values were obtained. Lastly, the observations were recorded.
5. RESULTS AND DATA ANALYSIS
Below are the observations that we obtained from the experiment:

Table 1 : Titration of oxalic acid with KMnO4.

No. of Initial burette reading Final burette reading Volume of KMnO4


Trial used (ml)

1. 0 16 16

2. 0 16 16

Calculations:
Molecular mass of Crystalline oxalic acid, 𝐶2𝐻2𝑂4. 2𝐻2𝑂

= 2(16) + 2(1) + 4(16).(4(1)+2(16))


= 24 + 2 + 64. (4 + 32)
= 90 + 36
= 126 𝑔/𝑚𝑜𝑙
To find mass of crystalline oxalic acid,

(volume) (molarity) (mass)


ml M g

1000 1 126

250 0.1 ?

126
𝑜𝑥𝑎𝑙𝑖𝑐 𝑐𝑟𝑦𝑠𝑡𝑎𝑙 𝑟𝑒𝑞𝑢𝑖𝑟𝑒𝑑 = 1000
× 250 × 0. 1

= 3. 150𝑔

Volume of oxalic acid = 20 ml


Molarity of oxalic acid = 0.1 M
Volume of KMnO4 = 16 ml
From the equation:
2𝐾𝑀𝑛𝑂4 + 3𝐻2𝑆𝑂4 + 5𝐻2𝐶2𝑂4. 2𝐻2𝑂 → 𝐾2𝑆𝑂4 + 2𝑀𝑛𝑆𝑂4 + 18𝐻2𝑂 + 10𝐶𝑂2

𝑀𝐴𝑉𝐴 𝑎
𝑀𝐵𝑉𝐵
= 𝑏

𝑀𝐾𝑀𝑛𝑂4 𝑉𝐾𝑀𝑛𝑂4 𝑛𝑜. 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝐾𝑀𝑛𝑂4


𝑀𝐶2𝐻2𝑂4 𝑉𝐶2𝐻2𝑂4
= 𝑛𝑜. 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝐶2𝐻2𝑂4

𝑀𝐾𝑀𝑛𝑂4 (16) 2
(0.1)(20)
= 5

(2)(0.1)(20)
𝑀𝐾𝑀𝑛𝑂4 = (16)(5)

= 0. 05 𝑀

𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑜𝑓 𝐾𝑀𝑛𝑂4 = 158 𝑔/𝑚𝑜𝑙

𝑠𝑡𝑟𝑒𝑛𝑔𝑡ℎ 𝑜𝑓 𝐾𝑀𝑛𝑂4 = 𝑚𝑜𝑙 𝑜𝑓 𝐾𝑀𝑛𝑂4 × 𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑜𝑓 𝐾𝑀𝑛𝑂4

= 0. 05𝑀 × 158 𝑔/𝑚𝑜𝑙


= 7.9 g/l
6. DISCUSSION
This experiment focuses on how to determine the molarity of the given potassium
permanganate,KMnO4 by titrating it against the standard solution of Oxalic acid. This
experiment required 2 types of procedure which is the preparation of 250ml, 0.1 molar standard
solution of oxalic acid and another one is the determination of KMnO4 using standard solution
of oxalic acid. The first procedure aims to obtain the molarity of oxalic acid to be used in the
second procedure. The molarity of the prepared solution of oxalic acid that has been obtained is
0.1M . When doing this experiment, washing the beaker, glass rod, funnel and funnel tip should
be done at least three times to make sure none of the solution has stuck to the equipment and all
the solution has been transferred to the standard flask. Or else, the final molarity of oxalic acid
that should be obtained will have the error, thus will interfere with the result in the second
procedure.
In the second procedure which is the main objective in this study, there were two trials that have
been done using the same volume of KMnO4 that is 16 ml, 20 ml of oxalic acid and 0.1 M
molarity of oxalic acid that was obtained from the procedure 1. Based on the result, the initial
reading of the burette was set to 0. After doing the titration, both of the trials show the same final
burette reading that is 16ml. The titrant in this titration is potassium permanganate, and the
analyte is oxalic acid. The oxidising agent is potassium permanganate, and the reducing agent is
oxalic acid. Because permanganate is a highly strong oxidising agent in an acidic medium, the
reaction between potassium permanganate and oxalic acid is carried out in an acidic medium.
The acidity is introduced by adding the diluted sulphuric acid, 𝐻2𝑆𝑂4.

− + − 2
𝑀𝑛𝑂4 + 8𝐻 + 5𝑒 → 𝑀𝑛 + 4𝐻2𝑂

From the equation above, Because KMnO4 acts as the indicator, no other indicators are used to
− −
determine the endpoint. The coloring of permanganate (𝑀𝑛𝑂4 ) ion is dark purple. 𝑀𝑛𝑂4 is
2+
converted to colourless manganous (𝑀𝑛 )ions in an acidic medium. On reaching the end point,
the last single drop of permanganate adds a light pink colour to the solution. The chemical
equation can be used to represent the chemical reaction that occurs during titration.
The equation are as follows:

Molecular equation
2𝐾𝑀𝑛𝑂4 + 3𝐻2𝑆𝑂4 → 𝐾2𝑆𝑂4 + 2𝑀𝑛𝑆𝑂4 + 3𝐻2𝑂 + 5[𝑂]

[𝐻2𝐶2𝑂4. 2𝐻2𝑂 + [𝑂] → 2𝐶𝑂2 + 3𝐻2𝑂] × 5

Overall Equation:
2𝐾𝑀𝑛𝑂4 + 3𝐻2𝑆𝑂4 + 5𝐻2𝐶2𝑂4. 2𝐻2𝑂 → 𝐾2𝑆𝑂2 + 2𝑀𝑛𝑆𝑂4 + 18𝐻2𝑂 + 10𝐶𝑂2

Ionic equation
− + − 2+
𝑀𝑛𝑂4 + 8𝐻 + 5𝑒 → 𝑀𝑛 + 4𝐻2𝑂] × 2

2− −
𝐶2𝑂4 → 2𝐶𝑂2 + 2𝑒 ] × 5
− + 2− 2+
Overall Reaction: 2𝑀𝑛𝑂4 + 16𝐻 + 5𝐶2𝑂4 → 2𝑀𝑛 + 8𝐻2𝑂 + 10𝐶𝑂2

From the balanced chemical equation, it is clear that 2 moles of 𝐾𝑀𝑛𝑂4 reacts with 5 moles of

oxalic acid.
According to the molarity equation,
𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑜𝑓 𝐾𝑀𝑛𝑂4 × 𝑉𝑜𝑙𝑢𝑚𝑒 𝐾𝑀𝑛𝑂4 𝑁𝑜.𝑜𝑓 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝐾𝑀𝑛𝑂4 2
𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑜𝑓 𝑜𝑥𝑎𝑙𝑖𝑐 𝑎𝑐𝑖𝑑 × 𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑜𝑥𝑎𝑙𝑖𝑐 𝑎𝑐𝑖𝑑
= 𝑁𝑜.𝑜𝑓 𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑜𝑥𝑎𝑙𝑖𝑐 𝑎𝑐𝑖𝑑
= 5
𝑀𝑜𝑙𝑎𝑟𝑖𝑡𝑦 𝑜𝑓 𝑜𝑥𝑎𝑙𝑖𝑐 𝑎𝑐𝑖𝑑 × 𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑜𝑥𝑎𝑙𝑖𝑐 𝑎𝑐𝑖𝑑 ×2
Therefore, Molarity of 𝐾𝑀𝑛𝑂4=
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝐾𝑀𝑛𝑂4×5

If the titration of oxalic acid is required, the amount of diluted H2SO4 needs to be added to the
flask and heating them to 60-70 celsius would be necessary. The goal of heating is to speed up
the reaction, which would otherwise be slow at room temperature.
After the molarity was obtained, the strength can be determined by multiplying the concentration
of KMnO4 with its molecular mass as shown in the calculation.
In order to do this experiment, there are some safety precautions that need to be considered:
1. Always keep the lower end of the pipette in the liquid when sucking it.
2. Fill the burette with care and make sure the stopcock does not leak.
3. While taking a burette reading with KMNO4 solution, read the upper meniscus since
KMnO4 is dark in colour.
4. Make sure no drops of solution should be at the tip of the burette at the end point.
5. To guarantee uniform distribution of potassium permanganate solution, rotate the titration
flask throughout the titration.
7. CONCLUSION
In conclusion, the objective of this experiment, which is to determine the concentration of
potassium permanganate (KMnO4) using titration against a standard solution of oxalic acid is
achieved with the value of the concentration of KMnO4 is 0.05M with the strength is 7.9 g/L.
REFERENCES
1. Why must the KMnO4 solution must be standardized before use? - eNotes.com. (2021).
Retrieved 29 June 2021, from
https://www.enotes.com/homework-help/why-kmno4-solution-must-standardized-before-
use-299421
2. Titration of Oxalic Acid with KMnO4. (2021). Retrieved 29 June 2021, from
https://byjus.com/chemistry/titration-of-oxalic-acid-with-kmno4/

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