INORGANIC CHEMISTRY

(474)
NAME: NUR FARAHAWANI BT MOHD
YUSOFF
PARTNERS: NURUL AMILA BT ARIFF
NAME
COURSE CODE: AS2022M1
LECTURERS: DR YING CHIN LIM
NAME
TILTLE/NO :(6)2 DETERMINATION OF THE
EXPERIMENT PERCENTAGE OF LIGAND IN
THE COORDINATION
COMPOUND

OBJECTIVE
The aim of this experiment is to determine the oxalate content in coordination
compounds.

INTRODUCTION
The volumetric analysis that involve in this experiment is a redox titration where the
potassium permanganate(VII) is used as the titrant that determine can determined the
percentage of the oxalate in analytes involved in this experiment which are the
coordination compound from experiment 3,4 and 5. However, the potassium
permanganate(VII) used must be standardized first by sodium oxalate in order to
determine the exact concentration of it. In the redox reaction, it acts as an oxidising agent
while the analyte as an reducing agent. The endpoint is indicated by the formation of
persistent pale pink colour in the solution in the conical flask. The Mn2+ ions formed are
almost colourless (very pale pink), so the endpoint is the first permanent faint pink due
to the first trace of excess of the purple manganate(VII) ion.
The reaction involve is as shown below:
Half equation of oxalate:
C2O4

CO2 2e

Half equation of potassium permanganate:

8 H MnO4 Mn 2 5e 4 H 2O
Overall equation:

16 H (aq) + 5C2O4 (aq) + 2 MnO4 (aq) 10CO2(g) + 8 H 2O(l) + 2 Mn2 (aq)

2-

There is no indicator is used as the potassium permanganate(VII) itself is an indicator due

to its intensively purple coloured and its high stability. The sulfuric acid is added in order
to prevent the formation of the side reaction which produce MnO 2 , black precipitation or
brown colouration.

CHEMICAL AND APPARATUS

CHEMICALS:

Potassium permanganate(VII) solution

Solid sodium oxalate
Diluted sulfuric acid
Solid potassium tris(oxalato) chromate(III) trihydrate
Solid copper(II) oxalate complex
Solid potassium tris(oxalato) ferrate(III) trihydrate

APPARATUS:
Burette
Conical flask
Laboratory hot plate
Thermometer
Analytical balance
Retort stand

PROCEDURE
PART A
1.
2.
3.

4.
5.

A burette was washed with ditilled water followed by the potassium

permanganate(VII) solution. Then, the burrete was fillled with potassium
permanganate(VII) solution. The initial volume was recorded.
0.20g of dried sodium oxalate was weighed and transferred into a cleaned and dried
conical flask which followed by the addition of 50mL of diluted sulfuric acid.
The mixture was heated to 600C which the temperature was measured with
thermometer. The solution in the conical flask was immediately tiitrated with the
potassium permanganate(VII) solution at 600C until a persistent pale pink colour was
formed. The final volume of the titrant was recorded.
The volume of potassium permanganate(VII) solution used was recorded in the data
sheet given in the laboratory manual.
The titration was repeated for two times.

PART B
1.
2.
3.

A burette was washed with distilled water followed by the potassium

permanganate(VII) solution. Then, the burette was filled with the potassium
perrmanganate(VII) solution and the initial volume was recorded.
0.20g of potassium tris(oxalato) chromium(III) trihydrate was weighed and
transferred into a cleaned and dried conical flask which followed by the addition of
50mL of sulfuric acid.
The mixture was heated to boil and after that, was left to room temperature until the
temperature decreased to 600C. The solution in the conical flask was immediately
titrated with the potassium permanganate(VII) solution at 60 0C until the first

4.
5.
6.

persistent pale pink colour solution formed. The final volume was recorded.
The volume of potassium permanganate(VII) solution used was recorded in the data
sheet given in the laboratory manual.
The titration was repeated for two times.
The steps above was followed by the next titration with different coordinate
compound which were copper(II) oxalate complex and potassium tris(oxalato)
ferrate(III) trihydrate.

DATA
Part A ( standardization of potassium permanganate(VII) solution)
Mass of sample(g)
Initial volume (mL)
Final volume (mL)
Volume of KMnO4 (mL)

I
0.2017
25.00
46.90
21.90

II
0.2087
47.50
25.00
22.50

Part B (determination of oxalate compound in potassium tris(oxalato)

chromium(III) trihydrate)
Mass of sample(g)
Initial volume (mL)
Final volume (mL)
Volume of KMnO4 (mL)

I
0.2033
0.50
7.60
7.10

II
0.2060
7.60
13.60
6.00

Part B(determination of oxalate compound in copper(II) oxalate complex)

Mass of sample(g)
Initial volume (mL)
Final volume (mL)
Volume of KMnO4 (mL)

I
0.2052
25.00
41.85
16.85

II
0.2074
25.00
41.35
16.35

Part B(determination of oxalate compound in potassium tris(oxalato) ferrate(III)

trihydrate

Mass of sample(g)
Initial volume (mL)

I
0.2017
0.50

II
0.2087
26.00

Final volume (mL)

Volume of KMnO4 (mL)

15.50
15.00

40.80
14.80

RESULT, CALCULATION AND QUESTION

Part A
The overall reaction:

16 H (aq) + 5C2O4 (aq) + 2 MnO4 (aq) 10CO2(g) + 8 H 2O(l) + 2 Mn2 (aq)

2-

The ratio of manganate(VII) ion and oxalate ion is 2:5.

(SAMPLE I)
molarity of KMnO4 0.2017 g Na2C2O4

1molNa2C2O4
1molC2O2
2molMnO4 1000mL
1

2
134 g Na2C2O4 1molNa2C2O4 5molC2O4
1L
29.10mL

0.02069M

(SAMPLE II)
molarity of KMnO4 0.2087 g Na2C2O4

1molNa2C2O4
1molC2O4
2molMnO4 1000mL
1

2
134 g Na2C2O4 1molNa2C2O4 5molC2O4
1L
22.50mL

0.02676M

The molarity of potassium permanganate(VII) is the average of the I and II samples:

(0.02069) (0.02676)
2
0.02373M

average molarity

Part B

(DETERMINATION
OXALATE
COMPOUND
TRIS(OXALATO) CHROMIUM(III) TRIHYDRATE)
ACTUAL YIELD
(SAMPLE I)

IN

POTASSIUM

mass of oxalate

0.02373molMnO4 5molC2O4
88.02 gC2O4
1L

7.10mL

2
1L
1000mL
2molMnO4
1molC2O4

0.03707 g

0.03707
100
0.2033
18.23%

percentage of oxalate
(SAMPLE II)

0.02373molMnO4 5molC2O4
88.02 gC2O4
1L
mass of oxalate

6.00mL

2
1L
1000mL
2molMnO4
1molC2O4
0.03133g

percentageofoxalate

0.01994
100
0.2060

15.21%
The average percentage of oxalate in potassium tris(oxalato)chromium(III) trihydrate
(18.23) (15.21)
2
16.72%

average percentage
THEORETICAL
YIELD
(SAMPLE I)

1molK 3 [Cr (C2O4 ) 3 ].3H 2O

3molC2O4
88.02 gC2O4
mass of oxalate 0.2033 gK 3 [Cr (C2O4 ) 3 ].3H 2O

487.408 gK 3 [Cr (C2O4 ) 3 ].3H 2O 1molK 3 [Cr (C2O4 ) 3 ].3H 2O 1molC2O4 2

0.1101g

0.1101
100
0.2033
54.16%

percentage of oxalate
(SAMPLE II)

mass of oxalate 0.2060 gK 3 [Cr (C2O4 ) 3 ].3H 2O

0.1116 g

0.1116
100
0.2060
54.17%

percentage of oxalate

The average percentage of oxalate in potassium tris(oxalato)chromium(III) trihydrate

(54.16) (54.17)
2
54.17%

average percentage
PERCENTAGE
PURITY :

percentage purity

16.72
100
54.17
30.87%

(DETERMINATION OF
OXALATE COMPOUND IN COPPER(II) OXALATE COMPLEX)
ACTUAL YIELD
(SAMPLE I)

0.02373molMnO4 5molC2O4
88.02 gC2O4
1L
mass of oxalate

16.85mL

2
1L
1000mL
2molMnO4
1molC2O4
0.08799 g

0.08799
100
0.2052
42.88%

percentage of oxalate
(SAMPLE II)
mass of oxalate

0.02373molMnO4 5molC2O4
88.02 gC2O4
1L

16.35mL

2
1L
1000mL
2molMnO4
1molC2O4

0.08538 g

1molK 3 [Cr (C2O4 ) 3 ].3H 2O

3molC2O4
88.02 gC2O4

487.408 gK 3 [Cr (C2O4 ) 3 ].3H 2O 1molK 3 [Cr (C2O4 ) 3 ].3H 2O 1molC2O4 2

0.08538
100
0.2074
41.17%

percentage of oxalate

The average percentage of oxalate in copper(II) oxalate complex:

(42.88) (41.17)
2
42.03%

average percentage
THEORETICAL
YIELD
(SAMPLE I)
mass of oxalate 0.2052 gK 2 [Cu (C2O4 ) 2 ( H 2O) 2 ]

1molK 2 [Cu (C2O4 ) 2 ( H 2O) 2 ]

2molC2O4
88.02 gC2O4

353.82 gK 2 [Cu (C2O4 ) 2 ( H 2O) 2 ] 1molK 2 [Cu (C2O4 ) 2 ( H 2O) 2 ] 1molC2O4 2

0.1021g

0.1021
100
0.2052
49.76%

percentage of oxalate
(SAMPLE II)
mass of oxalate 0.2074 gK 2 [Cu (C2O4 ) 2 ( H 2O) 2 ]

1molK 2 [Cu (C2O4 ) 2 ( H 2O) 2 ]

2molC2O4
88.02 gC2O4

353.82 gK 2 [Cu (C2O4 ) 2 ( H 2O) 2 ] 1molK 2 [Cu (C2O4 ) 2 ( H 2O) 2 ] 1molC2O4 2

0.1032 g

0.1032
100
0.2074
49.76%

percentage of oxalate

The average percentage of oxalate in copper(II) oxalate complex:

(49.76) (49.76)
2
49.76%

average percentage

\PERCENTAGE PURITY :

percentage purity

42.03
100
49.76
84.47%

(DETERMINATION
OXALATE
COMPOUND
TRIS(OXALATO) FERRATE(III) TRIHYDRATE)

IN

POTASSIUM

ACTUAL YIELD
(SAMPLE I)
mass of oxalate

0.02373molMnO4 5molC2O4
88.02 gC2O4
1L

15.00mL

2
1L
1000mL
2molMnO4
1molC2O4

0.07833 g

0.07833
100
0.2022
38.74%

percentage of oxalate
(SAMPLE II)
mass of oxalate

0.02373molMnO4 5molC2O4
88.02 gC2O4
1L

14.80mL

2
1L
1000mL
2molMnO4
1molC2O4

0.07728 g

0.07728
100
0.2077
37.21%

percentage of oxalate

The average percentage of oxalate in potassium tris(oxalato)chromium(III) trihydrate

(38.74) (37.21)
2
37.98%

average percentage
THEORETICAL
YIELD
(SAMPLE I)

mass of oxalate 0.2022 gK 3[ Fe(C2O4 )3 .3H 2O]

1molK 3 [ Fe(C2O4 ) 3 .3H 2O]

3molC2O4
88.02 gC2O4

491.248 gK 3 [ Fe(C2O4 ) 3 .3H 2O] 1molK 3[ Fe(C2O4 )3 .3H 2O] 1molC2O4 2

0.1087 g

0.1087
100
0.2022
53.76%

percentage of oxalate
(SAMPLE II)

1molK 3 [ Fe(C2O4 ) 3 .3H 2O]

3molC2O4
88.02 gC2O4
mass of oxalate 0.2077 gK 3[ Fe(C2O4 )3 .3H 2O]

491.248 gK 3 [ Fe(C2O4 ) 3 .3H 2O] 1molK 3[ Fe(C2O4 )3 .3H 2O] 1molC2O4 2

0.1116 g

0.1116
100
0.2077
53.73%

percentage of oxalate

The average percentage of oxalate in copper(II) oxalate complex:

(53.76) (53.73)
2
53.75%

average percentage

\PERCENTAGE PURITY :
percentage purity
(STRUCTURE OF THE
SYNTHESIZED COMPOUND)

37.98
100
53.75
70.66%

POTASSIUM TRIS(OXALATO) CHROMIUM(III) TRIHYDRATE

COPPER(II)
COMPLEX

OXALATE

POTASSIUM
TRIS(OXALATO)
FERRATE(III)
TRIHYDRATE

DISCUSSION
This experiment is conducted in
order
to
determine
the
composition of oxalate in the coordinate by using a standardized potassium
permanganate(VII) solution. The potassium permanganate(VII) act as an oxidising agent
and indicator itself. It can act as an indicator as its intensively purple coloured solution
and with high stability has make it suitable to be an indicator for this redox titration. The
manganate(VII), MnO4- ion will be reduced to Mn2+ while the oxalate will be oxidised to
carbon dioxide gas. The overall ionic equation is as followed:

16 H (aq) + 5C2O4 (aq) + 2 MnO4 (aq) 10CO2(g) + 8 H 2O(l) + 2 Mn2 (aq)

2-

After all the oxalate ion has been oxidised to carbon dioxide, an excessive one drop of
potassium manganate(VII) solution will formed a pale pink solution which indicate the
end point of the titration. The addition of sulfuric acid to dissolved the solid samples is
used to prevent any side reaction during titration MnO which formed a black precipitate
or brown colour solution.
In part A, the exact molarity of the potassium permanganate(VII) solution is 0.02373M
where the molarity is calculate based on the ratio of manganate(VII) ion with oxalate ion
which is 2:5. After standardized, it is used to determine the percentage of oxalate
compound
in
the
coordination
compounds
which
are
K3[Cr(C2O4)3.3H2O] ,K2[Cu(C2O4)3(H2O)2] and K3[Fe(C2O4)3.3H2O] in part B.
The actual percentage wight per weight of the oxalate compound in the potassium
tris(oxalato) chromium(III) trihydrate is 16.72% which is calculated from the average of
the percentage weight per weight of titration trial I and II. The percentage weight per
weight in first trial is 18.23% while the second trial is 15.21%. However, the theoretical
value for the percentage weight e weight is 54.17% that will give the percentage purity
equal to 30.87%. This percentage indicates that the result of the titration is not reliable as
the actual percentage of the oxalate compound in the coordination compound has a very
distinct different between the theoretical value and it is below 50%. This is due to the
errors happened in the experiment.

Then, determination of oxalate compound in the copper(II) oxalate complex shows result
where the percentage weight per weight of oxalate is equal to 42.03% while the
theoretical percentage is actually 49.76% which will gives the percent purity equals to
84.47%. According to the percentage of the purity, the result shown is acceptable and
nearly accurate as the percentage purity is high. The percentage weight per weight at first
trial of titration is 42.88% while the second trial is 41.17% and thus, the average of these
percentages is equal to 42.03% for the actual yield.
Next, the percentage of oxalate compound in the potassium tris(oxalato)
ferrate(III)trihydrate is 37.98% which is the actual yield of the percentage weight per
weight while the theoretical value for percentage weight per weight of the oxalate
compound is 53.75%. Therefore, the percentage purity is 70.66%. The percentage weight
per weight of oxalate compound in the first trial of titration is 37.21% while the second
trial is 38.74% so the average percentage is equal to 37.98% which is the actual yield of
percentage of oxalate in the coordination compound involve.
The errors that involves in this experiment are contamination of sample, the actual
endpoint is not reached and the loss of samples.
First error is contamination of the samples. This is due to improper method of cleansing
the apparatus. Before the apparatus is used, it should be rinsed thoroughly by distilled
water and followed by the solution to be filled in the apparatus. For example, before
using the burette, it must be washed by the tap water. Then , distilled water and followed
by the potassium permanganate(VII) solution. After that, the burette can be filled with the
new potassium permanganate(VII) solution. This is order to prevent any contamination to
the chemicals that are used in the experiment as it might effect the accuracy of the result.
If the apparatus is not properly washed, there might be a presence of unknown substances
that can cause any side reaction which is unnoticeable.
Second error is the actual endpoint is not reached. This is due to the colour of the solution
masked the pale pink colour which indicate the end point of the titration. For example,
the colour of the potassium tris(oxalato) chromium(III) trihydrate is dark green.
Therefore, the formation of pale pink colour is barely hard to be seen so the endpoint is
not accurately determined.
Third error is loss of samples. When the weighed sample is transferred, there is some of
the sample that is stick to the weighing board. Therefore the mass that recorded in the
data sheet is not fully used as some of the sample is left in the weighing board which
make the exact mass of the sample used is not the same as the mass recorded. For
example, after weighing the solid sodium oxalate and the three coordianate compound ,
they are transferred into the conical flask to dissolved with the sulfuric acid. However,
there are some of the samples are stick to the weighing board after being transferred.
As for precaution to reduce the errors of the experiment, the apparatus must be properly
rinsed by distilled water and the solution to be filled into the apparatus to prevent
contamination of the chemicals that are used in the experiment. The endpoint of the

titration must be properly observed in order to get an accurate reading of the volume of
titrant used so the result of the experiment will be more accurate and close to the
theoretical value. The weighing by difference is the most suitable technique that can be
used for weighing the samples in order to accurately determine the exact mass of the
samples that have been used in the experiment.

CONCLUSION
The percentage weight per weight of oxalate compound in the three coordination
compound which are potassium tris(oxalato) chromium (III)trihydrate, copper(II) oxalate
complex and potassium tris(oxalato) ferrate(III) trihydrate are 16.72%, 42.03% and
37.98% respectively. These percentages are determine through titration with the
standardized potassium permanganate(VII) solution and thus, these are the actual yield of
percentage of oxalate in the coordination compounds. The theoretical percentage weight
per weight of the oxalate in the potassium tris(oxalato) chromium(III) trihydrate , copper
oxalate complex and potassium tris(oxalato) ferrate (III) trihydrate are 54.17%, 49.76%
and 53..75% respectively. Next , the percentage purity of the complexes are 30.87% for
potassium tris(oxalato)chromium (III)trihydrate , 84.47% for copper(II) oxalate complex
and 70.66% for potassium tris(oxalato)ferrate(III)trihydrate.

REFRENCE
1.
2.
3.

http://www.docbrown.info/page07/SSquestions/redox_vol_calcs1ANS.htm
http://www.docbrown.info/page07/transition05Mn.htm
Inorganic Chemistry Experiments for Undergraduates, Hadariah Bahron,Kamariah
Muda,Sharifah Rohaiza Syed Omar and Kamariah Kassim, published by Penerbit
Press UITM.

DATASHEET

JOTTER