UNIVERSITI PUTRA MALAYSIA
CHY3401
ANALYTICAL CHEMISTRY
EXPERIMENT: 1
EXPERIMENT TITLE: REDOX TITRATION
EXPERIMENT DATE: 31st MARCH & 7th APRIL 2022
SUBMITTION DATE: 12/04/2022
: PROF. DR. NOR AZAH BINTI YUSOF
LAB INSTRUCTOR:
NO. NAME STUDENT ID.
1. NUR AQILAH NAJIHAH BINTI MUSLIMIN 209985
2. ABDUL MUKMIN BIN BAGIS 210823
Results
A. Standardization of Potassium Permanganate Solution
Weight of FeSO4(NH4)2.SO4.6H2O = 2.000 g
Titration 1 2 3
Initial reading (mL) 5.6 24.7 0.2
End reading (mL) 24.7 44.2 19.4
Volume (mL) 19.1 19.5 19.2
Average volume of MnO4- =
= 19.3 mL
B. Determination of Molecular Weight of Oxalic Acid
1 2 3
Weight of Oxalic Acid (g) 0.100 0.100 0.100
Average weight of Oxalic Acid = 0.100 g
Titration 1 2 3
Initial reading (mL) 11.8 16.1 18.1
End reading (mL) 39.1 44.0 46.1
Volume (mL) 27.3 28.1 28.0
Average =
= 27.8 mL
Calculation
A. Standardization of Permanganate solution
Molecular weight of FeSO4(NH4)2.SO4.6H2O = 392 g/mol
Concentration of Ferrous ion = ×
= ×
= 5.10 x 10-2 M
Equation: 5Fe2+ + MnO4- + 8H+ 2+ + 5Fe3+ + 4H2O
Oxidation equation: 5Fe2+ (s) 5Fe3+ (aq) + 5e
Reduction equation: MnO4- (aq) + 8H+ (aq) + 5e Mn2+ (aq) + 4H2O (l)
Concentration of MnO4- :
M1V1 = 5 M1 = [Fe2+]
M2V2 1 V1 = Volume of Fe2+
(5.10 x 10-2)(25.00) = 5 M2 = [MnO4-]
M2 (19.3) 1 V2 = Volume of MnO4-
M2 = 1.32 x 10-2 M
B. Determination of molecular weight of oxalic acid
Equation: 2MnO4- + 5C2O42- + 16H+ 2 + 2Mn2+ + 8H2O
Oxidation equation: C2O42- (s) 2CO2 (g) +2e
Reduction equation: MnO4- (aq) + 8H+ (aq) + 5e 2+ (aq) + 4H2O (l)
Molecular weight of oxalic acid:
mole of oxalic acid = 5
mole of MnO4- 2
W/MW = 5 W = mass of oxalic acid
M2V2 2 MW = molecular weight of oxalic acid
MW = 2W
5M2V2
Sample 1, MW = 2(0.100) .
5(1.32×10-2)(0.0273)
= 111.00 g/mol
Sample 2, MW = 2(0.100) .
-2
5(1.32×10 )(0.0281)
= 107.84 g/mol
Sample 1, MW = 2(0.100) .
-2
5(1.32×10 )(0.0280)
= 108.22 g/mol
Sample 1 2 3
Molecular weight (g/mol) 111.00 107.84 108.22
Average = 109.02 g/mol
Molecular formula = H2C2O4.nH2O
Molecular weight = 2(1) + 2(12) + 4(16) + 18(n) = 121.71
Formula = H2C2O4.2H2O
Theoretical Molecular Weight = 126
(based on molecular formula)
Percentage of error = (Theoretical value experiment value) x 100%
Theoretical value
= (126 109.02) x 100%
109.02
= 15.58%
Discussion
Redox titration is a laboratory method of determining the concentration of a given
analyte by causing a redox reaction between the titrant and the analyte. This experiment
consists of two part which is part A, standardization of permanganate solution and part B,
determination of molecular weight of oxalic acid. This experiment did not require an indicator
as potassium permanganate, KMnO4 acts as self-indicator of where the permanganate ions are
a deep purple color. The color change from colorless solution to faint pink solution shown that
the reaction is reaching the endpoint which is the point shows that the amount of reactant
necessary for a complete reaction has been added to a solution. Moreover, sulfuric acid, H2SO4
was used in this experiment to increase the acidic content of the solution to prevent the MnO4-
(purple) to reduce to MnO2 (dark brown) and as catalyse to speed the reaction.
In the part A of this experiment, the potassium permanganate, KMnO4 is standardized
by titration using ferrous ammonium sulphate, FeSO4(NH4).SO4.6H2O as
the source of Fe2+. During the reaction, the Fe+2 is oxidized to Fe+3 while the MnO4- is reduced
to Mn+2. Then the exact molarity of the KMnO4 was determined which is 1.32×10-2 M. The
equation for this reaction is shown below:
Overall equation: 5Fe2+ + MnO4- + 8H+ 2+ + 5Fe3+ + 4H2O
Oxidation equation: 5Fe2+ 3+ (aq) + 5e
Reduction equation: MnO4- (aq) + 8H+ 2+ (aq) + 4H2O (l)
When weighting the FeSO4(NH4).SO4.6H2O, the weight has to be accurate to obtain a valid
result. Then, the pipette and volumetric flask should not be used for the dilution of the
permanganate solution as pipetting from a volumetric flask is not a safe laboratory practice due
to the volumetric flask are likely to tip and break when a pipette is inserted into the neck of the
flask. The average amount of potassium permanganate, KMnO4 that been used to titrate the
analyte is 19.3 mL. Based on the balance equation, the concentration of MnO4- was calculated
by using this formula:
M1V1 = 5
M2V2 1
Where, M1 = [Fe2+]
M2 = [MnO4-]
V1 = Volume of Fe2+
V2 = Volume of MnO4-
Therefore, based on the calculation the concentration of the potassium permanganate solution
is 1.32×10-2 M.
In the part B of this experiment, the titration between oxalic acid solution with
potassium permanganate, KMnO4 is conducted to determine the molecular weight of oxalic
acid. The volume of all chemicals needs to be exact to obtain accurate, valid result. The oxalic
acid solution needs to be heated to 80°C. If the solution is titrated cold, the faint pink titrated
solution turns brown soon and the reaction takes longer times. Meanwhile, when the oxalic
solution is overheated, it will cause decomposition of oxalic acid as CO 2. Then, the result obtain
is not accurate. During the reaction, the C2O4-2 is oxidized to CO2 while the MnO4- is reduced
to Mn+2. Then the theoretical molecular weight of oxalic acid is determined which is
109.02g/mol. The equation for this reaction is shown below:
Equation: 2MnO4- + 5C2O42- + 16H+ 2 + 2Mn2+ + 8H2O
Oxidation equation: C2O42- (s) 2CO2 (g) +2e
Reduction equation: MnO4- (aq) + 8H+ (aq) + 5e 2+ (aq) + 4H2O (l)
Based on the balance equation of the reaction, the experimental molecular weight of oxalic acid
was calculated by using this formula:
W/MW = 5
M2V2 2
MW = 2W .
5M2V2
Where, W = mass of oxalic acid
MW = molecular weight of oxalic acid
Then the percentage error for this experiment is identified which is 15.58% due to several errors
that have occurred while conducting this experiment causing the experimental molecular
weight oof oxalic acid is less that theoretical value. Some errors that happen while running this
experiment is the loss of ferrous ammonium sulphate or oxalic acid when transferred it to
another apparatus. This causing the weight of oxalic acid decrease from 0.1 g while ferrous
ammonium sulphate decreases from 2.0 g. Next, misreading of the volume on the burette as
the eyes level are not perpendicular with the reading scale on the burette due to the burette was
placed too high. Moreover, overheating the oxalic acid solution more than 80°C cause the
volume of the solution decrease as decomposition of oxalic acid to CO2 was occurred. All this
error will lead to inaccurate and less precise results.
Conclusion
In conclusion the redox reaction is a laboratory method of determining the
concentration of a given analyte by causing a redox reaction between the titrant and the analyte.
The reducing agents in this experiment is ferrous ammonium sulphate and oxalic acid while
the oxidizing agent is potassium permanganate. The balance redox equation for this experiment
is;
A. Standardization of Permanganate solution:
5Fe2+ + MnO4- + 8H+ 2+ + 5Fe3+ + 4H2O
B. Determination of molecular weight of oxalic acid:
2MnO4- + 5C2O42- + 16H+ 2 + 2Mn2+ + 8H2O
Finally, the concentration of Fe2+ is 5.10 x 10-2 M, MnO4- is 1.32 × 10-2 M, and the
experimental molecular weight of oxalic acid was successfully calculated which is 109.02
g/mol.
Precaution steps
Use the full personal protective equipment (PPE) and goggles while conducting the
experiment.
Rinse the burette first before starting the titration so that we can reduce the risk of any
contamination and miscalculation during the titration.
The eyes level must be perpendicular to the reading scale of the apparatus which is
burette, pipette, measuring cylinder, etc.
Heat the solution at constant temperature, make sure it not overheating.
References
Vikram R. Jadhav, October 2020, A Procedure Employing for Redox Titration:
Balancing the Redox Chemical Equation in Acidic or Basic Medium.
https://papers.ssrn.com/sol3/papers.cfm?abstract_id=3684260
Robert M. Fowler, Harry A. Bright, November 1935, Standardization of permanganate
solution with sodium oxalate.
https://nvlpubs.nist.gov/nistpubs/jres/15/jresv15n5p493_A1b.pdf
Joshua Halpern, November 2021, Concentration of Solution.
https://chem.libretexts.org/Bookshelves/General_Chemistry/Map%3A_Chemistry_-
