Title: Determination of Oxalic Acid and Sodium Oxalate in a Mixture Solution

Objective: To determine the percentage of oxalic acid and sodium oxalate in a mixture

Introduction:
A laboratory method used in quantitative analysis is titration. Thus, titrimetric analysis plays
a vital role in the determination of concentration of analyte in a given solution, the
stoichiometry of a reaction, the number of accepted or donated in a redox reaction, the
solubility of products an so on and so forth. Usually, two solutions known as the analyte
solution and a standard solution is used in titration. The solution that is to be studied is called
as the analyte of which the concentration is usually unknown. The standard solution is usually
a solution of which the concentration and identity are known.

The equivalence point or endpoint is observed in a titration, indicating that the chemical
reaction is complete. Equivalence point and endpoint are different terms. The theoretical
completion of a reaction is known as the equivalence point whereas endpoint is the point in a
titration which a reaction is complete which is to be determined experimentally.

In this experiment, both oxalic acid and sodium oxalate react with potassium permanganate:
2 KMnO4 + 5 H2C2O4 + 3 H2SO4 K2SO4 + 2 MnSO4 + 8 H2O + 10 CO2
or, ionically
2 MnO4- + 5 C2O42- + 16 H+ 2 Mn2+ + 8 H2O + 10 CO2

Both oxalic acid and sodium oxalate contain one oxalate ion in a molecule; so the volume
of potassium permanganate can be separated into the portions reacting with oxalic acid and
sodium oxalate.

Only oxalic acid will react with sodium hydroxide, thus can be determined separately:
H2C2O4 + 2 NaOH Na2C2O4 + 2 H2O

Apparatus and Materials:

Sample consists of oxalic acid and sodium oxalate, 0.02 M potassium permanganate, 1 M
sulphuric acid, 0.1 M sodium hydroxide, phenolphthalein indicator, burette, conical flask, hot
plate, retort stand and thermometer.
Procedure:
There were two parts of titration in this experiment. In the first part, 25cm3 of the sample
was pipetted into a conical flask. It was acidified with about 15cm3 of dilute sulphuric acid.
The flask was heated until it was too hot to touch (~80oC), and was titrated with potassium
permanganate. The titration was repeated twice.
In the second part, 25cm3 of the sample was pipetted into a conical flask. A few drops of
phenolphthalein indicator was added and was titrated with sodium hydroxide until the colour
of the solution just turned pink. The titration was repeated twice as well.

Results and Calculations:

Titration 1:
Titration number 1 (rough) 2 3
Initial volume of 0.00 14.70 30.00
burette (cm3)
Final volume of 14.70 30,00 45.20
burette (ml)
Total volume of 14.70 15.30 15.20
KMnO4 used (cm3)
Average volume of 15.25
KMnO4 required for
titration (cm3)

Titration 2:
Titration number 1 (rough) 2 3
Initial volume of 30.30 39.20 40.00
burette (cm3)
Final volume of 39.20 46.90 47.20
burette (cm3)
Total volume of 8.90 7.70 7.20
NaOH used (cm3)
Average volume of 7.45
NaOH required for
titration (cm3)
From the results of titration 1,
Molarity of KMnO4, M1 = 0.02M
Volume of KMnO4 used, V1 = 15.25cm3
Volume of sample used, V2 = 25cm3

2 MnO4- + 5 C2O42- + 16 H+ 2 Mn2+ + 8 H2O + 10 CO2

Since 2 moles of MnO4- ions react with 5 moles of C2O42- ions, thus M1V1 / M2V2 = 2/5

[(0.02M)(15.25cm3)] / [M2(25cm3)] = 2/5

M2 = 0.0305M

From the results of titration 2,

Molarity of NaOH, M1 = 0.1M
Volume of NaOH used, V1 = 7.45cm3
Volume of sample used, V2 = 25cm3

H2C2O4 + 2 NaOH Na2C2O4 + 2 H2O

Since 2 moles of NaOH react with 1 mole of oxalic acid, thus M1V1 / M2V2 = 2

[(0.1M)(7.45cm3)] / [M2(25cm3)] = 2
M2 = 0.0149M

Concentration of oxalate ions = 0.0305M = 0.0305mol / dm3

Concentration of oxalic acid = 0.0149M = 0.0149mol / dm3

Concentration of sodium oxalate Na2C2O4 = Conc. of oxalate ions – Conc. of oxalic acid
= 0.0305 – 0.0149
= 0.0156mol / dm3

Concentration of oxalic acid = 0.0149mol/dm3 x [2(1.00794) + 2(12.0107) + 4(15.9994)]g/mol

= 1.3415g / dm3
Concentration of sodium oxalate = 0.0156mol/dm3 x [2(23) +2(12.0107) + 4(15.9994)] g/mol
= 2.0907g / dm3

Percentage of oxalic acid = [(1.3415g / dm3 ) / (1.3415 + 2.0907)g / dm3 ] x 100%

= 39.09%

Percentage of sodium oxalate = [(2.0907g / dm3 ) / (1.3415 + 2.0907)g / dm3 ] x 100%

= 60.91%

Discussion:
An experiment was set up to determine the concentration of the oxalate anion in a mixture,
through which the percentages of sodium oxalate and oxalic acid can be calculated. Through
the first titration, the molarity of oxalate ions with a value of 0.0305M was obtained. This value
is the concentration of the oxalate ion for the overall mixture. Therefore, it is necessary to have
the second titration. Since the second titration is an acid base neutralisation (Tan, 2013)
reaction, only the oxalic acid will be reacted and thus, the molarity of oxalic acid was obtained
as 0.0149M. the molarity of sodium oxalate was obtained by subtracting the molarity of oxalic
acid from the molarity of the overall oxalate ions. Since the molarity of oxalic acid and sodium
oxalate is known, the percentages of it were obtained to be 39.09% and 60.91% respectively.
For both titration 1 and titration 2, the titration was done thrice. This was because the first
titration was a rough estimation while the second and third titrations were more accurate and
an average is obtained from the two readings to ensure accuracy. Phenolphthalein is an acid-
base reaction indicator. Hence, in titration 2, phenolphthalein is added to indicate the endpoint
of the reaction. For titration 1, the potassium permanganate itself acts as an indicator by
reducing to colourless Mn2+. The solutions were heated at 80 oC to fasten the rate of reaction
(Yip, 2013)
Conclusion:
The percentage of sodium oxalate and oxalic acid in the mixture was successfully determined.
The mixture contained 60.91% of sodium oxalate and 39.09% of oxalic acid.

References
1. Tan, 2013. Ace AHead STPM Text Chemistry Second Term. In: Selangor Darul Ehsan:
Oxford Fajar.
2. Yip, 2013. Pre-U STPM Text Chemistry Term 2. In: Selangor Darul Ehsan: Pelangi.