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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:
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 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
2KMnO4(aq)+5H2C2O4(aq) + 3H2SO4 (aq) K2SO4(aq) + 2MnSO4(aq) +8H20(l)
+10CO2(g)
or, in ionic form
2MnO4-(aq) + 5C2O42-(aq) +16H+ (aq) 2Mn2+(aq) + 8H20(l) +10CO2(g)
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, hence, it can be analyzed separately.
H2C2O4 + 2NaOH Na2C2O4 + 2H20
Apparatus and materials:
sample consists of oxalic acid and sodium oxalate, 0.02M of potassium permanganate,
1Msulphuric acid, 0.1M of sodium hydroxide, phenolphthalein indicator, thermometer,pipette
(25ml) , conical flask, hotplate, retort stand, burette, dropper
Procedures
A)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.
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.
Resutlt
Titration 1
Titration number
Initial vol of burette/cm3
Final vol of burette/cm3
Total vol of KMnO4 used/cm3
Average vol of KMnO4 required for titration/cm3

1 rough
3.00
19.30
16.30
16.25

2
19.30
35.60
16.30

3
16.60
32.80
16.20

1
28.00
36.80
8.80
8.25

2
19.10
27.30
8.20

3
27.30
35.60
8.30

Titration 2
Titration number.30
Initial vol of burette/cm3
Final vol of burette/cm3
Total vol of NaOH used/cm3
Average vol of NaOH required for titration/cm3

Calculation:
For titration 1
2MnO4-(aq) + 5C2O42-(aq) +16H+ (aq) 2Mn2+(aq) + 8H20(l) +10CO2(g)
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 16.25) /1000
=0.0325mol
hence, 5/2 x 0.0325 = 0.08125 mol of C2O4 2- ions are reacted .
concentration of the solution with respect to oxalate ions is
n=MV/1000
M= 1000n/V
M=1000(0.08125)/25
M=3.25M
For titration 2
H2C2O4 + 2NaOH Na2C2O4 + 2H20
1mol of oxalic acid is needed to react with 2mol of NaOH
8.25ml of NaOH is used to react with oxalic acid
number of mol of NaOH , n= MV/1000

n=(0.1x8.25) / 1000
n=8.25x10-4 mol
hence, number of mol of oxalic acid is reacted is n= x 8.25 x 10-4
n=4.125x10-4mol
concentration of the oxalic acid in the mixture is
n=MV/1000
M=1000n/V
M=0.0165M
rmm of oxalic acid =90
rmm of sodium oxalate =134.0
n of oxalic acid=4.125x10-4 mol
n of sodium oxalate=0.0808375mol
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 = 3.25M 0.0165M = 3.2335M
Concentration of Na2C2O4 in the mixture = 3.2335M
Concentration of oxalic acid in the mixture = 0.0165M
percentage weight of sodium oxalate = mass of solute/volume x100
=[(0.0808375x134)/25]x100
=43.33%
percentage weight of oxalic acid= mass of solute/volume x100%
=[(4.125x10-4 mol x90)/25]x100
=0.1485%
So that, 43.33grams of sodium oxalate and 0.1485 grams of oxalic acid are in 100ml of sample
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 (C2O42-) first. Hence, titration one can obtain the overall number of mole of the C2O42ions which is 0.08125. 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 a 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
4.125x10-4mole. The overall number of mole of oxalate ions subtract the number of mole of
oxalic acid gives the number of mole of sodium oxalate in the mixture which is equal to
0.0808375mole. The percentage weight of each oxalate can be obtained by simple calculation=
concentration of either oxalic acid or sodium oxalate / total oxalate x100 %
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 a 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. When 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 upto 80 degree Celsius because if the temperature is
too low eg. Below 60degree 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 sulphuric acid is very corrosive to
human skin, do wear glove and handle with extra care. Sodium 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 43.44% while the percentage weight of oxalic acid in mixture
is 0.1485%
Reference
1. Sodium oxalate. [Online] Available at:
http://www.endmemo.com/chem/compound/na2c2o4.php [Accessed on 8/3/15]
2. Redox titration. [Online] Available at: http://www.lahc.edu/classes/chemistry/arias/exp
%208%20-%20redox.pdf [Accessed on 8/3/15]
3.Weight percent. (2003) [Online] Available at: http://dl.clackamas.edu/ch105-04/weight.htm
[Accessed on 8/3/15]
4. Concentration unit. (2010) [Online] Available at :
http://www.ilpi.com/msds/ref/concentration.html [Accessed on 8/3/15]