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International University, Vietnam National University - HCMC 1

CHEMISTRY LABORATORY

REPORT
EXPERIMENT 3: REDOX TITRATION

Group: ______3______ Class: ______________ Date: ____________

Group members:

Declaration of
Full name Student ID Signature
Contribution

1 Giang Ngọc Phương Thanh BEBEIU22191 25%

2 Nguyễn Ngọc Khánh Như BEBEIU22107 25%

3 Hoàng Trần Minh Nhật BTBTIU22263 25%

4 Võ Trần Anh Khôi BEBEIU22270 25%

Total score: _______/100


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Table of contents
Part 1. Introduction ............................................................................................................................... 4

1. Lab objectives ................................................................................................................................. 4

2. . Background Information ............................................................................................................ 4

2.1. Redox reaction.......................................................................................................................... 4

2.2. Redox titration ......................................................................................................................... 5

2.3. Titration’s endpoint ................................................................................................................. 5

2.4. Gram equivalent weight .......................................................................................................... 6

2.5. Normality ................................................................................................................................. 6

2.6. Overview of today’s experiment. ........................................................................................... 6

Part 2. Materials and Methods ............................................................................................................. 7

1. Materials ...................................................................................................................................... 7

2. Methods ........................................................................................................................................ 8

Experiment 1: Handling with burette ........................................................................................... 8

Experiment 2: Standardization of prepared KMnO4 solution ................................................... 9

Experiment 3: Determination of unknown concentration H2C2O4 solution ............................. 9

Experiment 4: Determination of unknown concentration FeSO4 solution.............................. 10

Part 3. Results and Discussion ............................................................................................................ 10

1. STANDARDIZATION OF PREPARED KMnO4 SOLUTION .............................................. 10

2. DETERMINATION OF UNKNOWN CONCENTRATION H2C2O4 SOLUTION............... 12

3. DETERMINATION OF UNKNOWN CONCENTRATION FeSO4 SOLUTION................. 13

Part 4. Conclusions .............................................................................................................................. 15

References ............................................................................................................................................. 15
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List of figures
Figure 1. Redox reaction between two atoms A and B [1] ................................................................. 4
Figure 2. Titration's endpoint of diphenylamine in solution 𝑪ⅇ𝟒+ .................................................... 5
Figure 3. Equiment and materials were used for the experiments .................................................... 8
Figure 4. The process of conducting Experiment 1............................................................................. 9
Figure 5. The process of conducting Experiment 2............................................................................. 9

List of tables
Table 1. The results table of Experiment 1 ........................................................................................ 11
Table 2. The results table of Experiment 2 ........................................................................................ 12
Table 3. The results table of Experiment 3 ........................................................................................ 14
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Part 1. Introduction
1. Lab objectives

This experiment will demonstrate how to compute a substance's gram-equivalent weight and apply
it to oxidation-reduction processes. It will also show how to standardize the concentration of KMnO4
solution, a commonly used oxidizing agent, and use it to assess the normality of oxalic acid solution, an
often used reducing agent.
2. . Background Information
2.1. Redox reaction

A redox reaction, also known as an oxidation-reduction reaction, is a chemical process that


changes the oxidation states of atoms. This is accomplished by the exchange of electrons between
chemical entities. One species is oxidized, which means it loses electrons, while another is reduced,
which means it acquires electrons. The material that loses electrons is referred to as a reducing agent,
while the substance that obtains electrons is referred to as an oxidizing agent. Redox reactions are
ubiquitous and important in many natural processes, such as photosynthesis, respiration, and
combustion. They also have several practical applications, including in batteries, corrosion prevention,
and chemical manufacturing.

Figure 1. Redox reaction between two atoms A and B [1]


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2.2. Redox titration

A redox titration is a form of titration in which the analyte and titrant undergo a redox reaction.
It is used to detect the concentration of an unknown reducing or oxidizing agent solution by reacting it
with a known oxidizing or reducing agent solution.
2.3. Titration’s endpoint

The titration's endpoint is determined by looking for a color change, using an indicator, or
measuring the potential difference between two electrodes. The use of potassium permanganate
(KMnO4) to determine the concentration of iron(II) ions or oxalic acid, and the use of iodine (I2) to
measure the concentration of vitamin C or thiosulfate ions, are two common instances of redox titrations.
Redox titrations are widely used in analytical chemistry and industry for quality control and research
purposes.

Figure 2. Titration's endpoint of diphenylamine in solution 𝐶ⅇ 4+ [2]


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2.4. Gram equivalent weight

Gram equivalent weight (GEW) is a measure of the reactive capacity of a molecule based on
the number of electrons gained or lost in a redox reaction. It is defined as the mass of a substance that
will react with or produce one equivalent of another substance. The formula for gram equivalent weight
is:

Molecular weight
GEW =
Equivalents per mole

2.5. Normality

Normality (N) is a measure of concentration that is used in acid-base and redox reactions. It is
defined as the number of equivalents of solute per liter of solution.[3] To calculate the normality of a
solution, you need to know the molarity of the solution and the number of equivalents per mole of solute.
The formula for normality is:

Molarity
N=
Equivalents per mole of solute
2.6. Overview of today’s experiment.
In the experiment, we standardized the 𝐾𝑀𝑛𝑂4 solution by titrating it against a 0.08N 𝐻2 𝐶2 𝑂4
solution. We recorded the volume of 𝐾𝑀𝑛𝑂4 used and calculated the Normality of the KMnO4 solution
using the appropriate formula.
In the second experiment, we utilized the Normality of 𝐾𝑀𝑛𝑂4 determined in the previous
experiment to standardize an unknown 𝐻2 𝐶2 𝑂4 solution. We gradually added the known Normality
𝐾𝑀𝑛𝑂4 solution into the mixture of the unknown Normality 𝐻2 𝐶2 𝑂4 solution. We waited for the
reaction to complete and recorded the volume of 𝐾𝑀𝑛𝑂4 used. By applying the appropriate formula, we
calculated the Normality of the unknown 𝐻2 𝐶2 𝑂4solution.
Both of these experiments shared the same chemical reaction equation involving the redox
reaction between 𝐾𝑀𝑛𝑂4 and 𝐻2 𝐶2 𝑂4.

2𝐾𝑀𝑛𝑂4 + 5𝐻2 𝐶2 𝑂4 + 3𝐻2 𝑆𝑂4 → 10𝐶𝑂2 + 𝐾2 𝑆𝑂4 + 2𝑀𝑛𝑆𝑂4 + 8𝐻2 𝑂


𝑀𝑛𝑂4− + 5𝐻2 𝐶2 𝑂4 + 6𝐻 + → 10𝐶𝑂2 + 2𝑀𝑛2+ + 8𝐻2 𝑂

In the final experiment, we determined the Normality of 𝑭𝒆𝑺𝑶𝟒 by gradually adding the
previously determined Normality of 𝑲𝑴𝒏𝑶𝟒 solution (from the first experiment) until the reaction was
complete. We observed the color change of the solution to light pink and recorded the amount of
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𝑲𝑴𝒏𝑶𝟒 added. By using the appropriate formula, we calculated the Normality of the 𝑭𝒆𝑺𝑶𝟒 solution
we were trying to find.

10𝐹ⅇ𝑆𝑂4 + 8𝐻2 𝑆𝑂4 + 2𝐾𝑀𝑛𝑂4 → 𝐾2 𝑆𝑂4 + 5𝐹ⅇ2 (𝑆𝑂4 )3 + 2𝑀𝑛𝑆𝑂4 + 8𝐻2 𝑂

At the end of the titration, three of the four variables were known, and the unknown variable
could be determined. The formula used to calculate the Normality for all three experiments remained
the same.
𝑽𝒐𝒙𝒊𝒅𝒊𝒛𝒊𝒏𝒈 × 𝑵𝒐𝒙𝒊𝒅𝒊𝒛𝒊𝒏𝒈 = 𝑽𝒓𝒆𝒅𝒖𝒄𝒊𝒏𝒈 × 𝑵𝒓𝒆𝒅𝒖𝒄𝒊𝒏𝒈

where V is the volume of oxidizing or reducing agents used in titrations and N is the normality
of oxidizing or reducing agents.

Part 2. Materials and Methods


1. Materials
● 3 Beakers (100mL, 200mL, 250mL)
● 2 Erlenmeyer Flasks (250mL)
● Cylinder (100mL)
● Pipette (10mL)
● Burette (50mL)
● Funnel
● Water Bath
Experiment 1: Handling with burette
● Distilled water
● KMnO4: ~65mL
Experiment 2: Standardization of prepared KMnO4 solution
● 0.08N H2C2O4: ~25mL
● 6N H2SO4: 40mL
● Distilled water: 80mL
Experiment 3: Determination of unknown concentration H2C2O4 solution
● Unknown normality H2C2O4: ~25mL
● 6N H2C2O4: 40mL
● Distilled water: 80mL
Experiment 4: Determination of unknown concentration FeSO4 solution
● Unknown normality FeSO4: ~25mL
● 6N H2C2O4: 40mL
● Distilled water: 80mL
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Figure 3. Equiment and materials were used for the experiments, A) Tools needed for the experiment,
B) Burette, C) 0.05N KMnO4, D) 6N H2C2O4, E) 0.08N H2C2O4, F) Unknown normality H2C2O4,
G) Unknown normality FeSO4, H) Water Bath.

2. Methods
Experiment 1: Handling with burette
● Step 1: Rinsed the burette 3 times with distilled water then rinsed 3 times with ~5mL KMnO4
to remove the wastes.
● Step 2: Filled with KMnO4 and let it flow over the top of the burette tip and took care not to
have air bubbles.
● Step 3: Record the starting point (ideally up to the level of the average eye), and then read the
burette at the top of the meniscus since the KMnO4 solution is dark in color.
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Figure 4. The process of conducting Experiment 1, A) Rinsed the burette with distilled water, B)
Discarded the waste, C) Rinsed the burette with ~5mL KMnO4.
Experiment 2: Standardization of prepared KMnO4 solution
● Step 1: Prepared 2 erlenmeyer flasks, each flask added 10mL 0.08N H2C2O4, add 40mL
distilled water and add 20mL 6N H2SO4.
● Step 2: Heated the flask to ~85 – 90oC and recorded the initial point (Vi).
● Step 3: The initial indication of a color shift (light pink) and the ultimate point (Vf) were
stopped titration and recorded after adding KMnO4 slowly and swirled the flask continuously.
● Step 4: Calculated the normality of KMnO4, the average normality and standard deviation.

Figure 5. The process of conducting Experiment 2, A) Measured 10mL 0.08N H2C2O4 to put in the
flask, B) Put 10mL 0.08N H2C2O4 into the flask, C) Added KMnO4 slowly and swirled the flask
continuously, D) Prepared the necessary solutions into the flask, E) The flask was submerged in a water
bath to warm it up.
Experiment 3: Determination of unknown concentration H2C2O4 solution
● Step 1: Prepared 2 erlenmeyer flasks, each flask added 10mL unknown H2C2O4, add 40mL
distilled water and add 20mL 6N H2SO4.
● Step 2: Heated the flask to ~85 – 90oC and recorded the initial point (Vi).
● Step 3: The initial indication of a color shift (light pink) and the ultimate point (Vf) were
stopped titration and recorded after adding KMnO4 slowly and swirled the flask continuously.
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● Step 4: Calculated the normality of unknown concentration H2SO4, the average normality and
standard deviation.

Experiment 4: Determination of unknown concentration FeSO4 solution


● Step 1: Prepared 2 erlenmeyer flasks, each flask added 10mL unknown FeSO4, add 40mL
distilled water and add 20mL 6N H2SO4.
● Step 2: Heated the flask to ~85 – 90oC and recorded the initial point (Vi).
● Step 3: The initial indication of a color shift (light pink) and the ultimate point (Vf) were
stopped titration and recorded after adding KMnO4 slowly and swirled the flask continuously.
● Step 4: Calculated the normality of unknown concentration FeSO4, the average normality and
standard deviation.
Part 3. Results and Discussion
1. STANDARDIZATION OF PREPARED KMnO4 SOLUTION
Calculation:
Normality of the standard H2C2O4 solution, N(H2C2O4) = 0.08 N

Volume of the standard H2C2O4 solution used, V(H2C2O4) = 10 mL


Burette reading Volume of Normality of
Trial # Results
(mL) KMnO4 (mL) KMnO4 (N)

1 22 - 37.3 15.3 mL 0.0523 N


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2 25 - 40 15 mL 0,0533 N

Table 1. The results table of Experiment 1

VH2C2O4  N H 2C2O4 10  0.08


Normality of KMnO4 in trial 1 = =  0.0523N
VKMnO4 15.3

VH2C2O4  N H 2C2O4 10  0.08


Normality of KMnO4 in trial 2 = =  0.0533N
VKMnO4 15

0.0523 + 0.0533
Average Normality of KMnO4 = = 0.0528 N
2
Discussion:
In the first experiment, the color of the solution was darker than in the second one because we
accidentally added an excessive amount of KMnO4, resulting in a darker pink color. However, in the
second trial, we were aware of the limit for reducing KMnO4, which was found to be below 15.3 mL of
KMnO4 solution. Therefore, we carefully added KMnO4 gradually and achieved a very pale pink
solution, without it becoming as dark as in the first trial. In this experiment, an oxidation-reduction
reaction occurred between KMnO4 and H2C2O4. When that reaction was fully completed, the solution
appeared very pale pink due to the excess amount of KMnO4 added.
𝟐𝑲𝑴𝒏𝑶𝟒 + 𝟓𝑯𝟐 𝑪𝟐 𝑶𝟒 + 𝟑𝑯𝟐 𝑺𝑶𝟒 → 𝟏𝟎𝑪𝑶𝟐 + 𝑲𝟐 𝑺𝑶𝟒 + 𝟐𝑴𝒏𝑺𝑶𝟒 + 𝟖𝑯𝟐 𝑶
+7 +2
Mn+ 5e − → Mn  2 (reduction)
+3 +4
2C → 2C + 2e −  5 (oxidation)
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2. DETERMINATION OF UNKNOWN CONCENTRATION H2C2O4 SOLUTION


Calculation:
Normality of the standard KMnO4 solution, N(KMnO4) = 0.0528 N

Volume of the unknown H2C2O4 solution used, V(H2C2O4) = 10 mL

Volume of
Burette Normality of
Trial # KMnO4 Results
reading (mL) H2C2O4 (N)
(mL)

1 23.3 - 24.7 1.4 mL 0.007392 N

2 25 - 26.4 1.4 mL 0.007392 N

Table 2. The results table of Experiment 2


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VKMnO4  N KMnO4 1.4  0.0528


Normality of H2C2O4 in trial 1 = = = 0.007392 N
VH 2C2O4 10

VKMnO4  N KMnO4 1.4  0.0528


Normality of H2C2O4 in trial 2 = = = 0.007392 N
VH 2C2O4 10

0.007392 + 0.007392
Average Normality of H2C2O4 = = 0.007392 N
2
Discussion:
In this experiment, both trial runs yielded the same volume result for KMnO4, which was 1.4 mL.
The resulting solution obtained had the same light pink color. This outcome was achieved because we
were more careful while adding KMnO4 and promptly stopped adding it when the solution turned light
pink. The reaction in this experiment was similar to the one in the previous experiment, but the amount
of H2C2O4 was unknown in terms of normality, so the amount of KMnO4 required to be added was
different.
𝟐𝑲𝑴𝒏𝑶𝟒 + 𝟓𝑯𝟐 𝑪𝟐 𝑶𝟒 + 𝟑𝑯𝟐 𝑺𝑶𝟒 → 𝟏𝟎𝑪𝑶𝟐 + 𝑲𝟐 𝑺𝑶𝟒 + 𝟐𝑴𝒏𝑺𝑶𝟒 + 𝟖𝑯𝟐 𝑶
+7 +2
Mn+ 5e − → Mn  2 (reduction)
+3 +4
2C → 2C + 2e −  5 (oxidation)
3. DETERMINATION OF UNKNOWN CONCENTRATION FeSO4 SOLUTION
Calculation:
Normality of the standard KMnO4 solution, N(KMnO4) = 0.0528 N
Volume of the unknown FeSO4 solution used, V(FeSO4) = 10 mL
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Burette reading Volume of Normality of


Trial # Results
(mL) KMnO4 (mL) FeSO4 (N)

1 27 - 31 4 mL 0.02112 N

2 31 - 35 4 mL 0.02112 N

Table 3. The results table of Experiment 3

VKMnO4  N KMnO4 4  0.0528


Normality of FeSO4 in trial 1 = = = 0.02112 N
VFeSO4 10

VKMnO4  N KMnO4 4  0.0528


Normality of FeSO4 in trial 2 = = = 0.02112 N
VFeSO4 10

0.02112 + 0.02112
Average Normality of FeSO4 = = 0.02112 N
2
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Discussion:
In the final experiment, FeSO4 was used to replace oxalic acid as the reducing agent in this reaction.
A redox reaction occurred between FeSO4 and KMnO4. When the reaction was complete, the solution
exhibited a pale pink color due to the excess KMnO4, similar to the previous two experiments. In both
instances, we obtained 4 mL of KMnO4, indicating that we conducted the experiment carefully,
especially during the step of adding KMnO4. Consequently, we achieved the expected outcome of a pale
pink solution.
𝟏𝟎𝑭𝒆𝑺𝑶𝟒 + 𝟖𝑯𝟐 𝑺𝑶𝟒 + 𝟐𝑲𝑴𝒏𝑶𝟒 → 𝑲𝟐 𝑺𝑶𝟒 + 𝟓𝑭𝒆𝟐 (𝑺𝑶𝟒 )𝟑 + 𝟐𝑴𝒏𝑺𝑶𝟒 + 𝟖𝑯𝟐 𝑶
+7 +2
Mn+ 5e− → Mn 2 (reduction)
+2 +3
2 Fe → 2 Fe+ 2e −  5 (oxidation)

Part 4. Conclusions
In conclusion, the utilization of the titrating method and burette in this lab experiment proved to
be invaluable in determining the normality of KMnO4, as well as the normality of H2C2O4 and FeSO4
through oxidation-reduction reactions. The resulting pale pink solutions provided crucial insights into
the accurate quantification of these substances.
This lab not only enhanced our understanding of oxidation-reduction reactions but also
emphasized the significance of careful experimental procedures and precise measurements. The skills
acquired, including the use of the burette and meticulous recording of data, will undoubtedly benefit us
in future scientific endeavors.
Overall, this lab served as an enriching learning experience. It underscored the importance of
reliable analytical techniques and provided us with practical knowledge in titration, oxidation-reduction
reactions, and the determination of substance concentrations. The acquired skills and insights from this
experiment will undoubtedly contribute to our growth as aspiring scientists.
References
[1] Encyclopædia Britannica, inc. (n.d.). Spiritualism. Encyclopædia Britannica.
https://www.britannica.com/topic/spiritualism-philosophy
[2] Selecting an indicator for a redox titration: Image and Video Exchange Forum. Image and
Video Exchange Forum | A place to share ideas! (2013, November 5).
https://asdlib.org/imageandvideoexchangeforum/selecting-an-indicator-for-a-redox-titration/
END.

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