CHM 475: INORGANIC CHEMISTRY

NO. OF EXPERIMENT 6
TITLE Determination of the Percentage of
Ligands in Coordination
Compounds.
NAME Nurul Iman Amani Bt Che Awang
STUDENT NUMBER 2014179961
PARTNER’S NAME Muhamad Nurasyraf Bin Mohd Razip
GROUP 2014532595
LECTURER’S NAME ED247/4A
LAB. INSTRUCTOR Dr Amalina Mohd Tajuddin
DATE OF EXPERIMENT 1st November 2016
DATE OF SUBMITION 8th November 20116
 INTRODUCTION:

There are two sections of this experiment. Part A involves standardization of potassium
permanganate solution which will be used in part B of the experiment. Part B involves
determining the amount of oxalate content in coordination compound of Potassium
Tris(oxalato)chromium(III) Trihydrate, Copper(II) Oxalate and Potassium
Tris(oxalato)ferrate(III) Trihydrate that we have prepared previously. The determination of
oxalate content in coordination compound is further calculated based on stoichiometry
principle.

OBJECTIVE:

The aim of this experiment is to determine the oxalate content in coordination compounds that
we have prepared in experiment 3, 4 and 5.

Apparatus Materials
Conical flask 50 mL of 1M Sulfuric acid
Weighing balance 0.20 g of Na2C2O4
Hot plate 0.20 g of Potassium Tris(oxalato)chromium(III)
Trihydrate
Thermometer 0.20 g of Copper(II) Oxalate
Buret 0.20 g of Potassium Tris(oxalato)ferrate(III)
Trihydrate
Potassium permanganate solution
PROCEDURE:

A. Standardisation of potassium permanganate solution.

1. 0.20 g of dried Na2C2O4 was weighed and it was transferred into conical flask.
2. It was dissolved in 50 ml of 1 M H2SO4.

3. The solution was heated to 60oC.

4. The solution was titrated with KMnO4 solution until the first persistent pink
colour appeared.
5. The volume of KMnO4 solution used or titrated was recorded in the table 6.1.
6. This process was repeated at least one more time utill a consistent values is
obtained.

B. Determination of the oxalate content in coordination compounds.

1. 0.20 g of the crystal Potassium Tris(oxalato)chromium(III) Trihydrate,
K3[Cr(C2O4)3].3H2O prepared previously was weighed and it was
placed in conical flask.
2. It was dissolved in 50 ml of 1 M H2SO4.

3. The solution was heated to 60oC.

4. It was titrated slowly with KMnO4 solution until slightly pink color appeared.
5. The volume of KMnO4 solution used was recorded in the table 6.2.
6. This process was repeated for one more time.
7. The whole steps was repeated with Copper(II) Oxalate,
K2[Cu(C2O4)2(H2O)2] and Potassium Tris(oxalato)ferrate(III) Trihydrate,
K3[Fe(C2O4)3].3H2O.
RESULTS:

Table 6.1: Standardisation of KMnO4 solution.

Trial I II

Mass of Na2C2O4. (g) 0.2100 0.2097

Final volume in burette. (mL) 13.70 26.90

Initial volume in burette. (mL) 0.00 13.70

Volume of KMnO4 used. (mL) 13.70 13.20

Table 6.2a: determination of oxalate content in K3[Cr(C2O4)3].3H2O

Trial I II

Mass of K3[Cr(C2O4)3].3H2O. (g) 0.2048 0.2054

Final volume in burette. (mL) 7.40 7.40

Initial volume in burette. (mL) 0.00 15.80

Volume of KMnO4 used. (mL) 7.40 8.40

Table 6.2b: determination of oxalate content in K2[Cu(C2O4)2(H2O)2]

Trial I II

Mass of K2[Cu(C2O4)2(H2O)2]. (g) 0.2015 0.2088

Final volume in burette. (mL) 7.80 7.80

Initial volume in burette. (mL) 0.00 18.30

Volume of KMnO4 used. (mL) 7.80 10.50

Table 6.2c: determination of oxalate content in K3[Fe(C2O4)3].3H2O.

Trial I II

Mass of K3[Fe(C2O4)3].3H2O. (g) 0.2053 0.2066

Final volume in burette. (mL) 7.60 7.60

Initial volume in burette. (mL) 0.00 14.00

Volume of KMnO4 used. (mL) 7.60 6.40

CALCULATION:

Standardisation of KMnO4 solution.

Trial 1 Trial 2
Number of moles of Na2C2O4 Number of moles of Na2C2O4
0.2100g Na2C2O4 x 1 mol Na2C2O4 0.2054g Na2C2O4 x 1 mol Na2C2O4
134.0 g Na2C2O4 134 g Na2C2O4
-3 -3
= 1.567 x10 mol Na2C2O4 = 1.5328 x10 mol Na2C2O4
Number of moles of KMnO4 solution
Number of moles of KMnO4 solution
1.5328 x10-3 mol Na2C2O4 x 2 mol KMnO4
1.567 x10-3 mol Na2C2O4 x 2 mol KMnO4
5 mol Na2C2O4
5 mol Na2C2O4
= 6.1312 x 10-4 mol KMnO4
-4
= 6.268 x 10 mol KMnO4
Concentration of KMnO4
Concentration of KMnO4
= 6.1312 x 10-4 mol KMnO4
-4
= 6.268 x 10 mol KMnO4
0.0132 L
0.0137 L
= 0.04645 M KMnO4
= 0.04588 M KMnO4

Average concentrate KMnO4 = 0.04588 M + 0.04645 M = 0.04617 M

2
Determination of oxalate content in K3[Cr(C2O4)3].3H2O

Trial 1 Trial 2

Number of moles of KMnO4 Number of moles of KMnO4

-4
0.04617 M x 0.0078 L = 3.6013 x 10 mol 0.04617 M x 0.01050 L = 4.848 x 10-4 mol
Number of moles of MnO4- Number of moles of MnO4-
3.6013 x 10-4 mol KMnO4 x 1 mol MnO4- 3.00 x 10-4 mol KMnO4 x 1 mol MnO4-
1 mol KMnO4 1 mol KMnO4
= 3.6013 x 10-4 mol MnO4- = 3.00 x 10-4 mol MnO4-
Number of moles of C2O42- Number of moles of C2O42-
3.6013 x 10-4 mol MnO4- x 5 mol C2O42- 3.00 x 10-4 mol MnO4- x 5 mol C2O42-
2 mol MnO4- 2 mol MnO4-
2-
2- = 7.500 x 10-4 mol C2O4
= 9.0033 x 10-4 mol C2O4
Mass of oxalate
Mass of oxalate 2- -1
-4
2- -1 7.500 x 10-4 mol C2O4 x 88.0 g mol
9.0033 x 10 mol C2O4 x 88.0 g mol
= 0.0660 g C2O42-
= 0.07923 g C2O42-
Percent of oxalate
Percent of oxalate
2- 0.0660 g C2O42- x 100
0.07923 g C2O4 x 100
0.2540 g
0.2048 g
= 25.98 %
= 38.69 %

Average percent of Oxalate = 38.69 + 25.98 = 32.34 %

2
Theoretical percentage oxalate in complex
3 x 88.0 g mol-1 = 54.17 %
-1
487.36 g mol
Percentage purity of complex.
32.34 X 100 = 59.70 %
54.17
Determination of oxalate content in K2[Cu(C2O4)2(H2O)2]

Trial 1 Trial 2

Number of moles of KMnO4 Number of moles of KMnO4

-4
0.075 M x 0.0078 L = 5.85 x 10 mol 0.075 M x 0.0105 L = 7.875 10-4 mol
Number of moles of MnO4- Number of moles of MnO4-
5.85 x 10-4 mol KMnO4 x 1 mol MnO4- 7.875 x 10-4 mol KMnO4 x 1 mol MnO4-
1 mol KMnO4 1 mol KMnO4
= 5.85 x 10-4 mol MnO4- = 7.875 x 10-4 mol MnO4-
Number of moles of C2O42- Number of moles of C2O42-
5.85 x 10-4 mol MnO4- x 5 mol C2O42- 7.875 x 10-4 mol MnO4- x 5 mol C2O42-
2 mol MnO4- 2 mol MnO4-
2- 2-
= 1.4625 x 10-3 mol C2O4 = 1.9688 x 10-3 mol C2O4
Mass of oxalate Mass of oxalate
2- -1 2- -1
1.4625x 10-3 mol C2O4 x 88.0 g mol 1.9688 x 10-3 mol C2O4 x 88.0 g mol
= 0.1287 g C2O42- = 0.1733 g C2O42-
Percent of oxalate Percent of oxalate
0.1287 g C2O42- x 100 0.1733 g C2O42- x 100
0.2015g 0.2088g
= 63.87 % = 83.00 %

Average amount of Oxalate = 63.87 + 83.00 = 73.35 %

2
Theoretical percentage oxalate in complex
2 x 88.0 g mol-1 = 49.75 %
-1
353.79 g mol
Percentage purity of complex.
73.35 % = 147.44 %
49.75 %
Determination of oxalate content in K3[Fe(C2O4)3].3H2O.

Trial 1 Trial 2

Number of moles of KMnO4 Number of moles of KMnO4

-4
0.0750 M x 0.0076 L = 5.700 x 10 mol 0.0750 M x 0.0064 L = 4.800 x 10-4 mol
Number of moles of MnO4- Number of moles of MnO4-
5.700 x 10-4 mol KMnO4 x 1 mol MnO4- 4.800 x 10-4 mol KMnO4 x 1 mol MnO4-
1 mol KMnO4 1 mol KMnO4
= 5.700 x 10-4 mol MnO4- = 4.800 x 10-4 mol MnO4-
Number of moles of C2O42- Number of moles of C2O42-
5.700 x 10-4 mol MnO4- x 5 mol C2O42- 4.800 x 10-4 mol MnO4- x 5 mol C2O42-
2 mol MnO4- 2 mol MnO4-
2-
= 1.425 x 10-3 mol C2O42- = 1.200 x 10-3 mol C2O4
Mass of oxalate Mass of oxalate
2- -1 2- -1
1.425 x 10-3 mol C2O4 x 88.0 g mol 1.200 x 10-3 mol C2O4 x 88.0 g mol
= 0.1254 g C2O42- = 0.1056 g C2O42-
Percent of oxalate Percent of oxalate
0.1254 g C2O42- x 100 0.1056 g C2O42- x 100
0.2053g 0.2066g
= 61.08 % = 51.11 %

Average amount of Oxalate = 61.08 + 51.11 = 56.10 %

2
Theoretical percentage of oxalate
3 x 88.0 g mol-1 = 53.74 %
-1
491.21 g mol

Percentage purity of complex

56.10 % = 104.39 %
53.74 %
DISCUSSION:

The experiment is conducted based on the principle of standardization and redox

titration method. The experiment is divided into parts, part A and B; where each part
discussed each principle.
Standardization process is defined as “the process of determining the exact
concentration (molarity) of a solution. Titration is one type of analytical procedure often used
in standardization. In a titration, an exact volume of one substance is reacted with a known
amount of another substance”. The titration process is performed using burette. The reactants
called as titrant is hold by burette. It will be titrated into a reaction vessel containing another
reactant. The titrant is KMnO4, while Na2C2O4 solution will be in the reaction vessel. The
unbalanced equation of the reaction is as follow:

MnO4- (aq) + C2O42- aq) Mn2+ aq) + CO2 (g)

Aqueous solution of permanganate ion is not stable over a long period of time. Thus,
the exact concentration of KMnO4 must be determined by titration with a known amount of
odium oxalate, Na2C2O4.
In order to determine the oxalate content in the coordination compound, first we have
to determine the mass percent of oxalate ion in the salt by titration with a standard KMnO4.
The process is called oxidation-reduction titration. The KMnO4 will oxidize all the oxalate to
carbon dioxide which escapes. The oxalate is oxidized and the permanganate is reduced.

The reaction takes place in acidic medium (H2SO4) as the reaction required the
dissociation of the reacting ion. Sulfuric acid is added to sodium oxalate to produce H2C2O4,
or oxalic acid plus sodium chloride. The H2C2O4 oxalate in an acidic environment dissociates
into C2O4 plus two H+ ions. Potassium permanganate in an acidic environment dissociates
into the potassium or K+ ions and permanganate or MnO4- ions. The process is quite slow;
therefore the salt compound is heated at 60-70 degree centigrade to speed up the reaction.

The ion C2O42- and Mn2+ are colorless while the MnO4- has a deep purple color. Until
all the oxalate salt is consumed in the reaction, the titrated solution will remain colorless.
When the reaction is complete, the solution will be a light pink color.
 Before reaching the endpoint, we will momentarily see a spot of pink color, but it
will disappear as you swirl. As more and more persistent color occurs, we slowed down the
addition of the titrant. This is important to ensure we obtained a preliminary final volume
reading and did not overshoot with one more drop. The presence of excess unreacted
permanganate ion can be detected by the appearance of the first consistent pink color (for
about 30 seconds). This is considered as the endpoint of titration. Endpoint or also called as
equivalence point is the point at which there will be equal number of moles of KMnO4 and
Na2C2O4 in the solution.

At the completing of the reaction, the moles of KMnO4 which are added from the
burette can be determined from the grams of Na2C2O4 by using the calculated moles of
Na2C2O4, using the concept of stoichiometry. The calculation will be shown in the result and
analysis. The balance equation of the reaction is as follow:

2 MnO4- + 5 H2C2O4 + 6 H + 10 CO2 + 2 Mn2+ + 8 H2O

The results we collected show the concentration of standardized KMnO4 solution was
0.04617 M. Then, we had determined amount of oxalate ions in coordination compounds by
titrating with standardized KMnO4 solution. After calculation using stoichiometry method
from balanced half chemical equation, we know that the ratio of the reaction in this

experiment was 2 mol of MnO4- reacted with 5 mol C2O4 produce Mn2+,CO2 and water.
The percentage of oxalate in coordination compounds were 54.17 %% in
K3[Cr(C2O4)3].3H2O, 49.75 % in K2[Cu(C2O4)2(H2O)2] and 53.74 %in
K3[Fe(C2O4)3].3H2O. The percentage purity of complex for K2[Cu(C2O4)2(H2O)2] and
K3[Fe(C2O4)3].3H2O exceeded 100%. This may be due to uncomplete drying of the
complex. This will cause the increase of sample’s weigh due to the presence of additional
water. Another reason could be the presence of contaminants, side-products, and/or unreacted
reagent during conducting the experiment.
 Precaution
There are some precautionary steps need to be considered during the experiment. Safety
goggles, aprons, and gloves must be worn in lab at all times. This is because the materials that
are used need to be handled properly. Oxalate is very toxic via oral and inhalation routes and
severe kidney damage is possible if oxalate salts are taken internally. Oxalate compounds can
be absorbed through the skin; gloves and washing affected areas with cold water are required. 1
M sulfuric acid is slightly corrosive. Wear gloves when handling these compounds and wash
any affected areas thoroughly with cold water. KMnO4 is a very strong oxidizing agent and
must not be poured into the organic collection bottles.
During the titration, KMnO4 must not be added or swirled rapidly as it may result in
brown coloration in your solution. This is due to the formation of manganese (IV) oxide
(MnO2). If you have not added any more KMnO4 than needed to reach the endpoint, the excess
oxalate should reduce the MnO2 momentarily. However, if you fail to swirl the sample and
overshoot the endpoint while MnO2 is formed, the titration is ruined and must be performed
again. The apparatus especially burette must be rinsed properly to ensure there is no
contaminants present that will affect our data. When you remove the thermometer to perform
the titration, be sure to rinse the thermometer into the flask since you do not want to lose any of
the sodium oxalate.

Errors
There are some random, systematic and human error may occurred throughout the
experiment. During transferring compounds from, some of it left in the weighing boat, leading
to inaccuracy of the compounds’ mass. In this experiment, the limited time and little amount of
apparatus limit us to collect two readings of very consistent values.
The compound may not completely dissolve in the solvent before mixing with other
solution because of improper stirring condition. During the titration, the titrant or reactant in the
conical flask may contain some impurities that may cause inaccuracy of the data.
The apparatus such as conical flask and burette might be contaminated with other chemicals as
it was not cleaned and dried enough before being used.
Future recommendations
The random errors that are resulted from inaccuracy of measurements can be reduced by
taking more measurements with high consistent values and take the average of the data. During
transferring the compound from the weighing boat, rinsing can be done to ensure the entire
compound is successfully transferred. Instead of using the glass rod to stir, we can also use the
magnetic stirrer to ensure that all salts are completely dissolved in the solvent.
Lastly, It is useful to run what is called a blank for this titration since the sulphuric acid solution
may contain some impurities that would react with the potassium permanganate and bring error
to your data.
To correct for this a blank containing only the solvent must be titrated. The "corrected
volume" is equal to the volume of KMnO4– required to titrate oxalate ion in solvent minus the
volume required to titrate the solvent alone.

CONCLUSION:

The conclusions were we had standardized the KMnO4 solution by titrating against
Na2C2O4. The concentration of KMnO4 solution was 0.04617 M. The oxalate content in each
coordination compound is determined by calculating theoretical percentage of oxalate and the
percentage purity of complex. the percentage of oxalate in coordination compounds were
54.17 %% in K3[Cr(C2O4)3].3H2O, 49.75 % in K2[Cu(C2O4)2(H2O)2] and 53.74 %in
K3[Fe(C2O4)3].3H2O.
ANSWERS FOR QUESTIONS:

1. 16 H+ + 2MnO4- + 10e- 2Mn2+ + 8H2O

5C2O4 10CO2 + 10e-

16 H+ + 2MnO4 + 5C2O4 2Mn2+ + 8H2O + 10CO2

2. Based on the calculation:

Experimental Percentage oxalate in K3[Cr(C2O4)3].3H2O is 32.34
%% Experimental Percentage oxalate in K2[Cu(C2O4)2(H2O)2] is ,
73.35 % Experimental Percentage oxalate in K3[Fe(C2O4)3].3H2O is
56.10 % Theoretical percentage in oxalate in K3[Cr(C2O4)3].3H2O is
54.17 % Theoretical percentage in oxalate in K2[Cu(C2O4)2(H2O)2] is
49.75 % Theoretical percentage in oxalate in K3[Fe(C2O4)3].3H2O is
53.74 % Percentage purity of K3[Cr(C2O4)3].3H2O is 59.70 %
Percentage purity of K2[Cu(C2O4)2(H2O)2 is 147.44 %
Percentage purity of K3[Fe(C2O4)3].3H2O is 104.39 %
REFERENCES:

1. Hadariah Bahron, Kamariah Muda, Sharifah Rohaiza Syed Omar, Karimah

Kassim/2015/Inorgani Chemistry: Experiment for
Undergraduates/UiTM PRESS.
2. Silberberg, Amateis/2015/Chemistry: The Molecular Nature of Matter and
Change 7thedition/Mc Graw Hill Education.

3. Wasserman, R.,(2015). Does Sodium Oxalate React With Potassium

Permanganate? Retrieved from

http://www.livestrong.com/article/286203-does- sodium-

oxalate-react-with-potassium-permanganate/