Experiment 11: 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
The method of titration is used widely for quantitative analysis. Thus, titrimetric analysis is very
essential for chemists to analyst the concentration of analyst in a given solution, the stoichiometry of a
reaction, the number of electrons accepted or lost in a redox reaction, the solubility of products and so
on. Basically, titration contains the use of two solution which are an analyst solution and a standard
solution. An analyst solution is the constituent of interest that is to be learned. The concentration of the
analyst is actually not known. However, standard solution is known as the solution which the
characteristic, identity and concentration of the solution are identified.
During a reaction of titration, the endpoint is a point which the reaction is ended to be observed,
indicating or observing that the chemical reaction is finished. In this experiment, both oxalic acid and
sodium oxalate are mixed and reacted with potassium permanganate. The equation of the reaction is
written as:

2 KMnO4 + 5 H2C2O4 + 3 H2SO4  K2SO4 + 2 MnSO4 + 8 H2O + 10 CO2

Or, in ionic form

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

Both sodium oxalate and oxalic acid have one oxalate ion in a molecule. So, the volume of potassium
permanganate can be divided into the portions reading with oxalic acid and sodium oxalate.
Only oxalic acid will react with sodium hydroxide, thus it can be analyzed separately.

H2C2O4 + 2 NaOH  Na2C2O4 + 2 H2O

Apparatus and materials
Sample consists of oxalic acid and sodium oxalate, 0.02M of potassium permanganate, 1M of sulphuric
acid, 0.1M of sodium hydroxide, phenolphthalein indicator, thermometer, pipette (25ml), conical flask,
hotplate, retort stand, burette, and dropper.

Procedures
Titration 1
25ml of the sample was pipetted into a conical flask. 15ml of dilute sulphuric acid was used to acidify
the sample. The mixture was heated until the flask was too hot to touch which was around 80 degree
Celsius. The mixture then was titrated by potassium permanganate. The titration was repeated twice and
the result was recorded.
Titration 2
25ml of the sample was pipette into a conical flask. Few drops of phenolphthalein was added into it and
the mixture was titrated with sodium hydroxide until the colour of the solution just turned into pink
color. The titration was repeated twice and the result was recorded.

Collected data
Titration 1
Titration number 1 (rough) 2 3
Initial volume of burette (cm3) 0.00 15.00 31.70
Final volume of burette (cm3) 15.90 31.70 48.30
Total volume of KMnO4 used (cm3) 15.90 16.70 16.60

Average volume of KMnO4 required for titration = 16.65 cm3

Titration 2
Titration number 1 (rough) 2 3
Initial volume of burette (cm3) 0.00 7.50 14.80
Final volume of burette (cm3) 7.50 14.80 22.10
 Total volume of NaOH used (cm3) 7.50 7.30 7.30

Average volume of NaOH required for titration = 7.30 cm3

Calculation
For titration 1
2 KMnO4 + 5 H2C2O4 + 3 H2SO4  K2SO4 + 2 MnSO4 + 8 H2O + 10 CO2
2 mol of potassium permanganate is needed to react with 5 mol of oxalate ions
Number of mol of MnO4- used = MV/1000
= (0.02M x 16.65)/1000
= 0.0003 mol
Hence, 5/2 x 0.0003mol = 0.0008 mol of C2O42- ion was reacted.
Concentration of the solution with respect to oxalate ions is
N = MV/1000
M = 1000n/V
M = 1000(0.0008)/25
M = 0.032 M

For titration 2
H2C2O4 + 2 NaOH  Na2C2O4 + 2 H2O
1 mol of oxalic acid is needed to react with 2 mol of NaOH
n(NaOH) = MV/1000
= 0.1 x 7.30 /1000
= 0.0007 mol
Therefore, number of mole of oxalic acid is reacted is = 0.0007/2
= 0.0004 mol
Concentration of oxalic acid = 1000(0.0004)/25.0
= 0.016 M
RMM of oxalic acid = 90
RMM of sodium oxalate = 134
To get the concentration of Na2C2O4, we subtract the total oxalate concentration which is from titration
1 by the concentration of oxalic acid which is from titration 2.
Hence concentration of Na2C2O4 = 0.032 M – 0.016 M = 0.016 M
Percentage weight of sodium oxalate = mass of solute/volume x 100
= [(0.0008 x 134)/25] x 100
= 0.43%
Percentage weight of oxalic acid = mass of solute/volume x 100
= [(0.0004 x 90)/25] x 100
= 0.14%

Discussion
In order to determine the percentage of oxalic acid and sodium oxalate in a mixture which have same
anions, we have to construct an experiment to determine the overall concentration of the anion (C2O42-)
first. Hence, titration one can obtain the overall number of mole of the C2O42- ions which is 0.0008 mole.
However this value is the value of overall number of mole of oxalate ions only, so that titration 2 is
needed. We used NaOH which is a base to neutralize the oxalic acid in the sample. As we have stated
that this is an acid base neutralization, only oxalic acid in the mixture will be reacted with NaOH. By
this way, only oxalic acid is reacted. Then, the result of titration 2 can be used to obtain the number of
mole of oxalic acid in the mixture which is 0.0004 mole. The overall concentration of oxalate ions
subtract the concentration of oxalic acid gives the concentration of sodium oxalate in the mixture which
is equal to 0.016 M. The percentage weight of each oxalate can be obtained by simple calculation =
concentration of either oxalic acid or sodium oxalate/total oxalate x 100
For each titration, the titration number 1 usually is a rough value to determine the rough range of volume
to be used for the reaction. Hence, titration number 2 and 3 are more accurate. Then, titration number 2
and 3 are used to get an average value instead of just using one value in order to enhance and increase
the accuracy of the experimental value. Phenolphthalein is an acid base reaction indicator. It has a ph
range of 8.3-10.0. It turns to colorless if the solution is acidic and it turns into pink if the solution is
alkali. For the reaction between potassium permanganate and the oxalate sample with dilute sulphuric
acid, the color of the potassium permanganate is dark purple in colour. Then it is reacted with oxalate
ions, it is reduced into colourless Mn2+. So, if all oxalate ions are reacted, the solution in conical will
turn pink if the potassium permanganate is in excess. Thus, the color of pink appear can be an indication
of endpoint of a reaction. In titration 1, the temperature of the mixture is heated up to 80 degree Celsius
because if the temperature is too low eg. Below 60 degree Celsius, the interaction between the oxalate
with potassium permanganate will be too slow to be titrated.
Potassium permanganate is dark in color, handle with care, wear glove while handling in order to
prevent the color stick onto hand or lab coat. 1M of sulphuric acid is very corrosive to human skin, do
wear glove and handle with extra care. 0odium hydroxide is alkali and corrosive to human skin too
handle with care and wear glove.

Conclusion
The percentage of oxalic acid and sodium oxalate in the mixture is determined, the percentage weight of
Na2C2O4 in mixture is 0.43% while the percentage weight of oxalic acid in mixture is 0.14%.

Reference
1. Sodium oxalate. [Online] Available at:
http://www.endmemo.com/chem/compound/na2c2o4.php [Accessed on 10/3/2018]
2. Redox titration. [Online] Available at:
http://www.lahc.edu/classes/chemistry/arias/exp%208%20-%20redox.pdf [Accessed on 10/3/2018]
3. Weight percent. (2003) [Online] Available at:
http://dl.clackamas.edu/ch105-04/weight.htm [Accessed on 10/3/2018]
4. Concentration unit. (2010) [Online] Available at:
http://www.ilpi.com/msds/ref/concentration.html [Accessed on 10/3/2018]