FACULTY OF APPLIED SCIENCES

CHM 474
EXPERIMENT 6
(DETERMINATION OF THE
PERCENTAGE OF LIGANDS IN
COORDINATION COMPOUNDS)
NAME : NUR NABILAH BINTI HAIRMAN
STUDENT’S ID : 2016644614
CLASS : AS2022 M1
TEL NO : 017-7368933
INSTRUCTOR’S NAME : DR. LIM YING CHIN
DATE SUBMITTED : 30 APRIL 2017
INTRODUCTION :

This experiment is about the quantitative analysis in order to determine the oxalate
content in the coordination compounds. A coordination compound is compound that
consisted of a central metal ion chemically bonded to one or more atoms or groups of atoms
known as ligands by coordinate covalent bond. The coordination compounds that were used
in this experiment are the compounds that have been synthesize from experiment 3, 4 and 5.

In this session, we performed two parts, which are part A and part B. The titration
process took place in both part. In part A, we standardised potassium permanganate solution.
This part is important in order to calculate the molarity of the potassium permanganate
solution. In this experiment, potassium permanganate solution was used as the titrant for part
B.

In part B, we performed the titration process for three coordination compound that
have been prepared in previous experiment. The compounds are potassium tris (oxalato)
chromium(III) trihydrate (experiment 3), copper(II)oxalate complexes (experiment 4) and
potassium tris (oxalato) ferrate(III) trihydrate (experiment 5). These three compounds were
titrated with the standard potassium permanganate solution.

Through this experiment, we need to find the percentage of ligands in the

coordination compounds. Other than that, we also need to find the molarity of the potassium
permanganate solution that acts as the titrant in part B, and also the molarity for all the
coordination compounds which later being converted its form from solid to solution form by
adding sulphuric acid to their solid form.

OBJECTIVES :

 To determine the oxalate content in coordination compound.

METHOD :

PART A : STANDARDIZATION OF POTASSIUM PERMANGANATE SOLUTION

1) 0.20 g of dried Na2C204 was weighed and poured into the conical flask.

2) The solid then was dissolved with 50 ml of 1M H2SO4.

3) The solution was heated on the hot plate to 60℃ .

4) Immediately the solution was titrated with potassium permanganate solution , KMnO 4 until
the first persistent pink colour was observed.

5) The initial and the final reading of the burette was recorded.
6) The whole steps were repeated for once more titration.

PART B : DETERMINATION OF THE OXALATE CONTENT IN COORDINATION

COMPOUNDS

1) 0.20 g of coordination compound prepared previously, which is potassium tris (oxalato)

chromium(III) trihydrate was weighed and poured into a conical flask.

2) 50 ml of 1M H2SO4 was added into the same conical flask.

3) The solution was boiled on the hot plate.

4) After the solution had boiled, the flask was removed from the hot plate and was allowed to
cool down to about 60℃ .

5) The solution was titrated with potassium permanganate solution, KMnO4.

6) The titration process was continued until the warm solution retains a light pink colouration
after standing for about 30 seconds.

7) Steps 1-6 were repeated for once more time.

8) Steps 1-7 were repeated by replacing the potassium tris (oxalato) chromium(III) trihydrate
with copper(II)oxalate complexes and potassium tris (oxalato) ferrate(III) trihydrate.

DATA AND RESULTS :

-Part A : STANDARDISATION OF POTASSIUM PERMANGANATE SOLUTION-

MASS OF SAMPLE (Na2C2O4) (g) 0.2161 0.2126

BURETTE READING I II
Final burette reading (ml) 12.10 23.10
Initial burette reading (ml) 0.04 12.10
Volume of KMnO4 (ml) 12.06 11.00

-PART B : STANDARDISATION OF POTASSIUM PERMANGANATE SOLUTION

(potassium tris (oxalato) chromium(III) trihydrate)

MASS OF SAMPLE (K3[Cr(C2O4)3].3H2O) (g) 0.2052 0.2038

BURETTE READING I II
Final burette reading (ml) 28.20 33.50
Initial burette reading (ml) 23.10 28.20
Volume of KMnO4 (ml) 5.10 5.30
-PART B : STANDARDISATION OF POTASSIUM PERMANGANATE SOLUTION
(copper(II)oxalate complexes)

MASS OF SAMPLE (K2[Cu(C2O4)2(H2O)2] (g) 0.2036 0.2016

BURETTE READING I II
Final burette reading (ml) 25.70 26.50
Initial burette reading (ml) 17.20 18.10
Volume of KMnO4 (ml) 8.50 8.40

-PART B : STANDARDISATION OF POTASSIUM PERMANGANATE SOLUTION

(potassium tris (oxalato) ferrate(III) trihydrate)

MASS OF SAMPLE (K3[Fe(C2O4)3].3H2O (g) 0.2045 0.2078

BURETTE READING I II
Final burette reading (ml) 35.30 36.20
Initial burette reading (ml) 25.70 26.50
Volume of KMnO4 (ml) 9.60 9.70

CALCULATIONS :

-Part A : STANDARDISATION OF POTASSIUM PERMANGANATE SOLUTION-

[ MnO4- (aq) + 8H+(aq) + 5e Mn2+(aq) + 4H2O(l) ] x 2

[ C2O42- (aq) 2CO2(g) + 2e ] x 5

2MnO4- (aq) + 16H+ (aq) + 5C2O42- (aq) 2 Mn2+ (aq) + 8H2O(l) + 10CO2 (g)

1st trial :

Number of moles of Na2C2O4 = 0.2161g / 134gmol-1

= 1.6127 x 10-3 mol

5 mol C2O42- : 2 mol MnO4-

∴ 1.6127 x 10-3 mol C2O42- : 6.4508 x 10-4 mol MnO4-

∴ molarity of potassium permanganate :

6.4508 x 10−4 mol

M=
(12.06 /1000)

= 0.0535 M
2nd trial :

Number of moles of Na2C2O4 = 0.2126 g / 134gmol-1

= 1.5866 x 10-3 mol

5 mol C2O42- : 2 mol MnO4-

∴ 1.5866 x 10-3 mol C2O42- : 6.3464 x 10-4 mol MnO4-

∴ molarity of potassium permanganate :

6.3464 x 10−4 mol

M=
(11.00 /1000)

= 0.0577 M

∴ average molarity of potassium permanganate solution :

= (0.0535 + 0.0577) M

= 0.0556 M

-PART B : STANDARDISATION OF POTASSIUM PERMANGANATE SOLUTION

(potassium tris (oxalato) chromium(III) trihydrate)

[ MnO4- (aq) + 8H+(aq) + 5e Mn2+(aq) + 4H2O(l) ] x 2

[ C2O42- (aq) 2CO2(g) + 2e ] x 5

2MnO4- (aq) + 16H+ (aq) + 5C2O42- (aq) 2 Mn2+ (aq) + 8H2O(l) + 10CO2 (g)

1st trial :

Number of moles of MnO4- = 0.0556 M x (5.10/1000) L

= 2.8356 x 10-4 mol

2 mol MnO4- : 5 mol C2O42-

∴ 2.8356 x 10-4 mol MnO4- : 7.089 x 10-4 mol C2O42-

Mass of oxalate in potassium tris (oxalato) chromium(III) trihydrate :

= 7.089 x 10-4 mol C2O42- x 88.018 gmol-1

= 0.0624 g

Percentage by weight of oxalate in potassium tris (oxalato) chromium(III) trihydrate :

0.0624 g
= x 100%
0.2052 g

= 30.41 %

2nd trial :

Number of moles of MnO4- = 0.0556 M x (5.30/1000) L

= 2.9468 x 10-4 mol

2 mol MnO4- : 5 mol C2O42-

∴ 2.9468 x 10-4 mol MnO4- : 7.367 x 10-4 mol C2O42-

Mass of oxalate in potassium tris (oxalato) chromium(III) trihydrate :

= 7.367 x 10-4 mol C2O42- x 88.018 gmol-1

= 0.0648 g

Percentage by weight of oxalate in potassium tris (oxalato) chromium(III) trihydrate :

0.0648 g
= x 100%
0.2038 g

= 31.8 %

∴Average percentage by weight of oxalate in potassium tris (oxalato) chromium(III)

trihydrate :

= ( 30.41 % + 31.8 % )

= 31.11 %
-PART B : STANDARDISATION OF POTASSIUM PERMANGANATE SOLUTION
(copper(II)oxalate complexes)

[ MnO4- (aq) + 8H+(aq) + 5e Mn2+(aq) + 4H2O(l) ] x 2

[ C2O42- (aq) 2CO2(g) + 2e ] x 5

2MnO4- (aq) + 16H+ (aq) + 5C2O42- (aq) 2 Mn2+ (aq) + 8H2O(l) + 10CO2 (g)

1st trial :

Number of moles of MnO4- = 0.0556 M x (8.50/1000) L

= 4.726 x 10-4 mol

2 mol MnO4- : 5 mol C2O42-

∴ 4.726 x 10-4 mol MnO4- : 1.1815 x 10-3 mol C2O42-

Mass of oxalate in copper(II)oxalate complexes :

= 1.1815 x 10-3 mol C2O42- x 88.018 gmol-1

= 0.104 g

Percentage by weight of oxalate in copper(II)oxalate complexes :

0.104 g
= x 100%
0.2036 g

= 51.08 %

2nd trial :

Number of moles of MnO4- = 0.0556 M x (8.40/1000) L

= 4.6704 x 10-4 mol

2 mol MnO4- : 5 mol C2O42-

∴ 4.6704 x 10-4 mol MnO4- : 1.1676 x 10-3 mol C2O42-

Mass of oxalate in copper(II)oxalate complexes :

= 1.1676 x 10-3 mol C2O42- x 88.018 gmol-1

= 0.1028 g

Percentage by weight of oxalate in copper(II)oxalate complexes :

0.1028 g
= x 100%
0.2016 g

= 50.99 %

∴ Average percentage by weight of oxalate in copper(II)oxalate complexes :

= ( 51.08 % + 50.99 % )

= 51.04 %

-PART B : STANDARDISATION OF POTASSIUM PERMANGANATE SOLUTION

(potassium tris (oxalato) ferrate(III) trihydrate)

[ MnO4- (aq) + 8H+(aq) + 5e Mn2+(aq) + 4H2O(l) ] x 2

[ C2O42- (aq) 2CO2(g) + 2e ] x 5

2MnO4- (aq) + 16H+ (aq) + 5C2O42- (aq) 2 Mn2+ (aq) + 8H2O(l) + 10CO2 (g)

1st trial :

Number of moles of MnO4- = 0.0556 M x (9.60/1000) L

= 5.3376 x 10-4 mol

2 mol MnO4- : 5 mol C2O42-

∴ 5.3376 x 10-4 mol MnO4- : 1.3344 x 10-3 mol C2O42-

Mass of oxalate in potassium tris (oxalato) ferrate(III) trihydrate :

= 1.3344 x 10-3 mol C2O42- x 88.018 gmol-1

= 0.1175 g

Percentage by weight of oxalate in potassium tris (oxalato) ferrate(III) trihydrate :

0.1175 g
= x 100%
0.2045 g

= 57.46 %

2nd trial :

Number of moles of MnO4- = 0.0556 M x (9.70/1000) L

= 5.3932 x 10-4 mol

2 mol MnO4- : 5 mol C2O42-

∴ 5.3932 x 10-4 mol MnO4- : 1.3483 x 10-3 mol C2O42-

Mass of oxalate in potassium tris (oxalato) ferrate(III) trihydrate :

= 1.3483 x 10-3 mol C2O42- x 88.018 gmol-1

= 0.1187 g

Percentage by weight of oxalate in potassium tris (oxalato) ferrate(III) trihydrate :

0.1187 g
= x 100%
0.2078 g

= 57.12 %

∴ Average percentage by weight of oxalate in potassium tris (oxalato) ferrate(III) trihydrate :

= ( 57.46 % + 57.12 % )

= 57.29 %
DISCUSSION:

The purpose of this experiment is to determine the oxalate content in coordination

compound. In order to measure the oxalate content in the coordination compound, titration
process called as redox titration process need to be performed. By performing this type of
titration, we can measure the amount of the oxalate ligands that are bound to each of the
metal centre. The titrant that was used in this experiment is potassium permanganate solution.

In part A, we standardised the potassium permanganate solution. A solution of

sulphuric acid with dried Na2C2O4 was titrated with the potassium permanganate solution
until first persistent light pink colour occured. Because the mass of Na2C2O4 is known, we
can calculate the amount of Na2C2O4 that will react with potassium permanganate solution.

2MnO4- (aq) + 16H+ (aq) + 5C2O42- (aq) 2 Mn2+ (aq) + 8H2O(l) + 10CO2 (g)

From this equation, the number of moles of potassium permanganate solution that
react with Na2C2O4 are 6.4508 x 10-4 mol MnO4- and 6.3464 x 10-4 mol MnO4- for first and
second trial respectively. Then, the calculated molarity of potassium permanganate in first
trial is 0.0535 M. For second trial, the molarity is 0.0577 M. So, the average molarity for
the potassium permanganate solution is 0.0556 M.

For part B, the first coordination compound involved in this reaction is potassium tris
(oxalato) chromium (III). This compound was titrated with the standardised potassium
permanganate solution which its concentration is 0.0556 M. The percent by weight of oxalate
content in this coordination compound is 30.41% for first trial and 31.8% for second trial.
The average percent of weight of oxalate content is found to be 31.11%.

The second coordination compound used in this experiment is copper (II) oxalate
complexes. This compound also being titrated with the standardised potassium permanganate
solution until a solution retains a slight pink colouration after standing for about 30 seconds.
The percent by weight of oxalate content in this coordination compound is 51.08 % for first
trial and 50.99% for second trial. The average percent of weight of oxalate content is found to
be 51.04%.

The last coordination compound is potassium tris (oxalato) ferrate (III) trihydrate.
This compound was dissolved in sulphuric acid and placed on the hot plate until boil, then
was allowed to cool down to 60℃. This warm solution then was titrated with potassium
permanganate solution. The percent by weight of oxalate content in this coordination
compound is 57.46% for first trial and 57.12% for second trial. The average percent of weight
of oxalate content is found to be 57.29%.

No additional indicator is needed in this experiment because the reduction of

permanganates only requires strong acidic condition. This explain why the solution that need
to be titrated with potassium permanganate solution contain sulphuric acid. Permanganate
will be reduced by oxalate, C2O42- in acidic condition. Oxalate reacts very slowly at room
temperature so the solutions are titrated hot to make the procedure practical.

CONCLUSION :

We had successfully determine the oxalate content in these three coordination

compound, potassium tris (oxalato) chromium (III), copper (II) oxalate complexes and
potassium tris (oxalato) ferrate (III) trihydrate. The average molarity for the potassium
permanganate solution is 0.0556 M. The average percent of weight of oxalate content in
potassium tris (oxalato) chromium (III) is found to be 31.11%. The average percent of weight
of oxalate content in copper (II) oxalate complexes and potassium tris (oxalato) ferrate (III)
trihydrate are 51.04% and 57.29% respectively.

REFERENCES :

 www.lahc.edu
 www.classes.colgate.edu>chem102>week3
 www.christineloehr.org>2014>project4final
 https://www.coursehero.com>file>experiment6>determination_of_percentage_of_lig
ands_in_coordination_compound