Name Teoh Song Yu

Student ID 1606421
Partner's name and 1. Chong Jen Kai (1607128)
ID 2. Lee Pui Yi (1606655)
3. Ooi Jason (1504540)
No of Experiment 11
Experiment title Determination of Oxalic Acid and Sodium Oxalate in a Mixture
Solution
Date of Experiment 1 March 2017
Practical group 3
Practical subgroup 1
Date of submission 15 March 2017
Lecturer's name Dr. Ooi Zhong Xian
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:
Oxalic acid is an organic compound with the formula C2H2O4. It is a colorless
crystalline solid that forms a colorless solution in water. Its condensed formula is HOOCCOOH,
reflecting its classification as the simplest dicarboxylic acid. Its acid strength is much greater
than that of acetic acid. Oxalic acid is a reducing agent and its conjugate base, known as oxalate
(C2O42-), is a chelating agent for metal cations. Typically, oxalic acid occurs as the dihydrate with
the formula C2H2O42H2O. Excessive ingestion of oxalic acid or prolonged skin contact can be
dangerous.
Sodium oxalate, or disodium oxalate, is the sodium salt of oxalic acid with the formula
Na2C2O4. It is usually a white, crystalline, odorless powder, that decomposes at 250270 C.
Disodium oxalate can act as a reducing agent, and it may be used as a primary standard for
standardizing potassium permanganate (KMnO4) solutions.
In this experiment, a mixture of oxalic acid and sodium oxalate is presented and test is
carried out to determine the percentage of oxalic acid and sodium oxalate in a mixture. The
method of titration is used widely for quantitative analysis. Thus, titrametric analysis is very
essential for chemists to analyze the concentration of analyte 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 analyte solution and a standard solution. an analyte solution is the constituent of interest that
is to be learned. The concentration of the analyte is not known. However, standard solutions
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.
Apparatus:
Pipette, conical flask, hotplate, retort stand, burette, dropper
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
Procedure:
a) Titration 1
25ml of the sample was pipetted into a conical flask. 4-ml 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 23 degree Celsius. The mixture then was titrated by potassium permanganate. The
titration was repeated twice and the result was recorded.
b) Titration 2
25ml of the sample was pipette into a conical flask. A 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.
Results:
a) Titration 1
Titration number 1 2 3
(Rough)
Initial volume of 0 0 16.5
burette (cm3)
Final volume of 16.6 16.5 32.9
burette (cm3)
Total volume of 16.6 16.5 16.4
KMnO4 used (cm3)

Average volume of KMnO4 required for titration = 16.5cm3

b) Titration 2
Titration number 1 2 3
(Rough)
Initial volume of 0 10 18.1
burette (cm3)
Final volume of 8.1 18.1 26.2
burette (cm3)
Total volume of 8.1 8.1 8.1
NaOH used (cm3)
 Average volume of NaOH required for titration = 8.1cm3

Calculations:
For titration 1,
2 MnO4-(aq) + 5 C2O42-(aq) + 16 H+(aq) 2 Mn2+(aq) + 8 H2O() + 10 CO2(g)
2 mol of potassium permanganate is needed to react with 5 mol of oxalate ions
MV
number of mol of (MnO4) used,n = 1000

( 0.02 M ) (16.5 cm 3)
= 1000

= 3.3x10-4 mol
5
Hence x 3.3 x 104=8.25 x 104 mol
2

0.0825 mol of C2O42- ions reacted

Molarity of the solution with respect to oxalate ions is
MV
n=
1000

1000 n
M=
V

1000 x 8.25 x 104 mol

M=
25 ml

M =0.03 3 M

For titration 2,
H2C2O4 + 2 NaOH Na2C2O4 + 2 H2O
1 mol of oxalic acid is needed to react with 2 mol of NaOH
8.1m of NaOH is used to react with oxalic acid
MV
Number of mol of NaOH ,n = 1000
 ( 0.1 M ) ( 8.1 cm3 )
= 1000

= 8.1x10-4mol

1 4
Therefore, number of mol of oxalic acid reacted, n = x 8.1 x 10 mol
2

= 4.05 x 10-4 mol

Molarity of oxalic acid in the mixture,
1000 n
M=
V

( 1000 ) (4.05 x 104 mol)

M=
25 ml

M =0.0162 M =0.0162 mol dm3

Molarity of Na2C2O4 = molarity of oxalate ions - Concentration of oxalic acid

0.033 M 0.0162M = 0.0168M = 0.0168 mol dm-3
Concentration of oxalic acid = 0.0162 mol dm-3 x 90 g/mol
= 1.458 g dm-3
Concentration of sodium oxalate = 0.0168 mol dm-3 x 134 g/mol
= 2.2512 g dm-3
1.458
Percentage of oxalic acid = x 100 = 39.3%
1.458+ 2.2512

2.2512
Percentage of sodium oxalate = x 100 =60.7%
1.458+ 2.2512

Discussion:
In order to determine the percentage of oxalic acid and sodium oxalate in a mixture
which have same anions, we have to construct a experiment to determine the overall
concentration of the anion first. Hence, titration one can obtain the overall molarity of the C 2O42-
ions which is 0.033M. However, this value is the value of overall molarity 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 molarity of oxalic acid in the mixture which is 0.0162 M.
The overall molarity of oxalate ions subtract the molarity of oxalic acid gives the molarity of
sodium oxalate in the mixture which is equal to mole. 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 first titration usually is a rough value to determine the rough range
of volume to be used for the reaction. Hence, second and third titration are more accurate. Then,
both titration 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. Then it is reacted with oxalate ions and it is reduced into colourless Mn 2+. 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 first titration, the
temperature of the mixture is heated up to 80C because if the temperature is too low, the
interaction between the oxalate with potassium permanganate will be too slow to be titrated.
Precaution:
1. Parallax error
2. Potassium permanganate is dark in color, handle with care, wear glove while handling to
prevent the color stick onto hand or lab coat.
3. Sulphuric acid is very corrosive to human skin, do wear glove and handle with extra
care.
4. Sodium hydroxide is alkali and corrosive to human skin too, handle with care and wear
glove.
Conclusion:
The percentage unknown amount of oxalic acid and sodium oxalate in the sample solution was
calculated. The percentage of oxalic acid was 39.3% and the percentage of sodium oxalate was
60.7%.

References:
1. UTAR (2017) Experiment 2, in Lab manual UDEC 1134 Chemistry Laboratory 1. pp. 21-22.
2. Vlab.amrita.edu,. (2011). Acid Base Titration. Retrieved 5 March 2017, from
vlab.amrita.edu/?sub=2&brch=193&sim=352&cnt=1
3. Satyajit Sarker, Lutfun Nahar, Chemistry for Pharmacy Students: General, Organic and
Natural Product Chemistry, pp. 14