CHM 474: INORGANIC

CHEMISTRY AS
202

NO. OF EXPERIMENT

3, 4 & 5

TITLE

Synthesis of potassium
tris(oxalate)chromium(III) trihydrate,
copper(II) oxalate complex and

NAME

potassium tris(oxalate)ferrate(III)
MOHAMAD
trihydrate. ZULFIKRI BIN MAT JUSOH

STUDENT NUMBER

2014910247

PARTNERS NAME

AMIRUL IMRAN BIN IDOPI

GROUP

AS2022M1

LECTURERS NAME

DR. LIM YING CHI N

LAB. INSTRUCTOR

MISS SARAH

DATE OF EXPERIMENT

15th &22nd. OCT. 2015

DATE OF SUBMITION

30th OCT. 2015

OBJECTIVE:
1. To synthesis potassium tris(oxalate)chromium(III) trihydrate.
2. To prepare a copper(II) oxalate complex.
3. To synthesis potassium tris(oxalate)ferrate(III) trihydrate.

INTRODUCTION:
One of important aspects of any chemical research was the preparation of new
compound. This process called as synthesis. In this experiment we will synthesised a special
kind of compound called as a coordination compound. A coordination compound consisted of
a central metal ion chemically bonded to one or more atoms or groups of atoms known as
ligands by coordinate covalent bond. Transition metal readily formed these coordination
compound, often resulting in bright colour.
In this experiment we performed three experiment was about preparation of crystals.
The crystal that we prepared were potassium tris(oxalate)chromium(III) trihydrate, copper(II)
oxalate complex and potassium tris(oxalate)ferrate(III) trihydrate.
The amount of coordination compound expected from given mass of reactants can be
calculated and it was called theoretical yield. The actual mass of the coordination compound
synthesised was called actual yield and it was usually less than the theoretical yield.

PROCEDURE:
Experiment 3
1. 5.00 g of oxalate acid was dissolved in 10 ml distilled water in a conical flask. 1.8 g
of potassium dichromate was added into the mixture in small portions and the funnel
was placed on the mouth of conical flask.
2. After the reaction had subsided, 2.10 g of potassium oxalate monohydrate was
added into the hot green-black liquid and it was heated until boiling for 5 minutes.
3. The flask was cooled down at room temperature and 10 ml 95% ethanol was
added into the flask and it was cooled in ice bath with frequent stirring.
4. After cooling in ice for 15 minutes or when the precipitate completely formed, the
precipitate was collected by suction filtration.
5. The crystals were washed with 5 ml portion 1:1 ethanol/distilled water and
followed by 13 ml of 95% ethanol.
6. The crystals were placed on the watch glass and it was allowed to dry in the oven.
7. The mass of the synthesis crystals and percentage yield were determined.
8. The crystals were transferred into a plastic packet. It was kept for next experiment.
Experiment 4
1. 2.00 g copper(II) sulphate was weighed and it was placed in conical flask. 30 ml of
distilled water was added in the flask. The flask was heated slowly on a hot plate until
the solid dissolves.
2. 6.20 g of potassium oxalate monohydrate was dissolved in 30 ml of distilled water
in another flask.
3. The heated CuSO4 solution was added into the flask contained potassium oxalate
monohydrate slowly. The flask was swirled slowly to mix.
4. The mixture was cooled in ice bath for 30 minutes. Blue crystals were formed.
5. The crystals were placed on the watch glass and it was allowed to dry in the oven.
6. The mass of the synthesis crystals and percentage yield were determined.
7. The crystals were transferred into a plastic packet. It was kept for next experiment.

Experiment 5
Procedure A
1. 5.00 g of ferrous ammonium sulphate was dissolved in 25 ml distilled water
containing 1 ml of diluted sulphuric acid in the beaker.
2. 2.50 g of oxalate acid dihydrate was dissolved in 25 ml of distilled water in
another beaker. Then it was added into the beaker containing ferrous ammonium
sulphate.
3. The mixture was heated slowly until boiling and then it was allowed the yellow
precipitate to settle. The supernatant was discarded. 15 ml hot water was added into
the yellow precipitate. It was stirred and the supernatant was discarded.
4. 15 ml of hot water was added to precipitate. 3.5 g of solid potassium oxalate
o

monohydrate. It was heated to approximately 40 C. Then immediately 10 ml of 6%

H2O2 was added drop wisely and it was stirred continuously.
5. It was heated to boiling and the dissolved solution of 2.0 g of oxalic acid in 30 ml of
distilled water was added into the mixture until the brown precipitate was dissolved.
6. It was boiled until the solution was clear. The solution was filtered through Buchner
funnel. 30 ml of 95% ethanol was added slowly to the solution. Any crystals were
formed was redissolved. Then, it was leaved in not direct light to crystallise for a
week.
Procedure B
1. The crystals were collected by suction filtration process. The beaker was rinsed with
10 ml of 1:1 ethanol/distillation water for two times. The crystals were washed with
cold acetone.
2. The crystals were placed on the watch glass and it was allowed to dry on air.
3. The mass of the synthesis crystals and percentage yield were determined.
4. The crystals were transferred into a plastic packet. It was kept for next experiment.

RESULTS:
Experiment 3: mass of K2[Cr(C2O4)3].3H2O
Mass of watch glass and filter paper

35.1230 g

Mass of watch glass and filter paper + crystals

40.0201 g

Mass of crystals

4.8971 g

Theoretical yield

5.6046 g

Percent yield

87.38 %

Experiment 4: mass of K2[Cu(C2O4)2.(H2O)2

Mass of watch glass and filter paper

31.5282 g

Mass of watch glass and filter paper + crystals

34.1391 g

Mass of crystals

2.6109 g

Theoretical yield

2.8657 g

Percent yield

91.11 %

Experiment 5: mass of K3[Fe(C2O4)3].3H2O

Mass of filter paper

0.3337 g

Mass of filter paper + crystals

4.7415 g

Mass of crystals

4.4078 g

Theoretical yield

6.2851 g

Percent yield

70.13 %

CALCULATION:
Experiment 3:
7H2C2O4 + K2Cr2O7 + 2K2C2O4.H2O

2K3[Cr(C2O4)3]. 3H2O + 4CO2 + 3H2O

Theoretical mass of K2[Cr(C2O4)3].3H2O

5.0123 g H2C2O4

1 mol H2C2O4

2 mol K3[Cr(C2O4)3. 3H2O

90.02 g H2C2O4
=

7 mol H2C2O4

0.0159 mol K3[Cr(C2O4)3. H2O

1.8273 g K2Cr2O7

1 mol K2Cr2O7

2 mol K3[Cr(C2O4)3. 3H2O

294.2 g K2Cr2O7
=

1 mol K2Cr2O7

0.0124 mol K3[Cr(C2O4)3. H2O

2.1111 g K2C2O4.H2O

1 mol 2K2C2O4.H2O
184.22 g 2K2C2O4.H2O

2 mol K3[Cr(C2O4)3. 3H2O

2 mol 2K2C2O4.H2O

0.0115 mol K3[Cr(C2O4)3. H2O

So, K2C2O4.H2O is limiting reactant

0.0115 mol K3[Cr(C2O4)3. 3H2O

487.36 g K3[Cr(C2O4)3].3 H2O

1 mol K3[Cr(C2O4)3. 3H2O

5.6046 g K3[Cr(C2O4)3. 3H2O

Percent yield of K3[Cr(C2O4)3. 3H2O

4.8971g
5.6046 g
= 87.38 %

100

Experiment 4:
CuSO4.5H2O +

2K2C2O4.H2O

K2[Cu(C2O4)2(H2O)2]

+ K2SO4 + 5H2O

Theoretical mass of K2[Cu(C2O4)2.(H2O)2]

2.0236 g CuSO4.5H2O x

1 mol CuSO4.5H2O

1mol K2[Cu(C2O4)2(H2O)2]

249.62 g CuSO4.5H2O
=

0.0081 mol K2[Cu(C2O4)2(H2O)2]

6.2260 g K2C2O4.H2O

1 mol K2C2O4.H2O
184.22 g K2C2O4.H2O

1 mol CuSO4.5H2O

1 mol K2[Cu(C2O4)2(H2O)2]
2 mol K2C2O4.H2O

0.0169 mol K2[Cu(C2O4)2(H2O)2]

So, CuSO4.5H2O is limiting reactant

0.0081 mol K2[Cu(C2O4)2(H2O)2]

353.79 g K2[Cu(C2O4)2(H2O)2]
1 K2[Cu(C2O4)2(H2O)2]

2.8657 g K2[Cu(C2O4)2(H2O)2]

Percent yield of K2[Cu(C2O4)2(H2O)2]

2.6109 g
x
2.8657 g
=

91.11 %

100

Experiment 5:
3K2C2O4 + 2Fe(OH)3 + 3H2C2O4

2K3[Fe(C2O4)3].3H2O

3H2O

Theoretical mass of K3[Fe(C2O4)3].3H2O

5.0064 g Fe(NH4)2(SO4). 6H2O

1 mol Fe(NH4)2(SO4). 6H2O

392.02 g Fe(NH4)2(SO4). 6H2O

2+

= 0.0128 mol FeC2O4 x 1 mol Fe

1 mol FeC2O4
= 0.0128 mol Fe(OH)3

3+

2 mol Fe

1 mol Fe(OH)3

2+

2 mol Fe

3+

1 mol Fe

2 mol K3[Fe(C2O4)3].3H2O
2 mol Fe(OH)3

0.0128 mol K3[Fe(C2O4)3].3H2O

3.5004 g K2C2O4

1 mol K2C2O4

166.22 g K2C2O4
=

3 mol K2C2O4

0.0140 mol K3[Fe(C2O4)3].3H2O

2.0024 g H2C2O4

1 mol H2C2O4

90.02 g H2C2O4
=

2 mol K3[Fe(C2O4)3].3H2O

2 mol K3[Fe(C2O4)3].3H2O
3 mol H2C2O4

0.0148 mol K3[Fe(C2O4)3].3H2O

So, K2C2O4 is limiting reactant.

0.0128 mol K3[Fe(C2O4)3].3H2O

491.21 g K3[Fe(C2O4)3].3H2O
1 mol K3[Fe(C2O4)3].3H2O

6.2851 g K3[Fe(C2O4)3].3H2O

Percent yield of K3[Fe(C2O4)3].3H2O

Actual yield
X
Theoretical yield
4.4078 g
X
6.2851 g
=
%

100

100

70.13

DISCUSSION:
In

this

experiment,

tris(oxalate)chromium(III)

we

had

trihydrate,

prepared

copper(II)

crystals

oxalate

such

complex

as

potassium

and

potassium

tris(oxalate)ferrate(III) trihydrate. The process to synthesis the crystals were known as

crystallisation. The results of the experiment that we obtained were 4.8971 g emerald green
solid K3[Cr(C2O4)3. 3H2O, 2.6109 g blue solid K2[Cu(C2O4)2(H2O)2] and 4.4078 g green
solid K3[Fe(C2O4)3].3H2O. The percent yield that we get after the calculation were 87.36 %
of

K3[Cr(C2O4)3.

3H2O,

91.11

of

K2[Cu(C2O4)2(H2O)2]

and

70.13

of

K3[Fe(C2O4)3].3H2O.
The error may be occurred when we run this experiment that will affect the result of
experiment. The error was there may be had some product remained at the Buchner funnel
when we collected the product after suction filtration to transferred it into watch glass.
Besides that, the product may dissolve when we washed the product with ethanol and cold
water. The precautions that we must take in the experiment, we must always were wearing
gloves to protect our hand from exposed to acid. Then, we must be careful handling hot plate
when we heated the mixture.

CONCLUSION:
The

conclusion

in

tris(oxalate)chromium(III)

the

experiment

trihydrate,

was

copper(II)

the

oxalate

crystals
complex

of

potassium

and

potassium

tris(oxalate)ferrate(III) trihydrate were synthesised by crystallisation process. The percent

yield of the crystals obtained were 87.36 % of K 3[Cr(C2O4)3. 3H2O, 91.11 % of
K2[Cu(C2O4)2(H2O)2] and 70.13 % of K3[Fe(C2O4)3].3H2O.

REFERENCES:
1. Hadariah Bahron, Kamariah Muda, Sharifah Rohaiza Syed Omar, Karimah
Kassim/2015/Inorgani Chemistry: Experiment for Undergraduates/UiTM PRESS.
2.

th

Silberberg, Amateis/2015/Chemistry: The Molecular Nature of Matter and Change 7

edition/Mc Graw Hill Education.

ANSWERS THE QUESTIONS:

1.

Oxidation state of chromium in K2Cr2O7 and in the product.

K2Cr2O7 = 0
(+1)(2) + (X)(2) + (-2)(7) = 0
2X = +14 2
X = +6

K3[Cr(C2O4)3]. 3H2O = 0
(+1)(3) + (X) + (-2)(3) + 3(0) = 0
X = +6 3
X = +3

2. Half equation reaction involved in preparation

2-

of the complex. 5C2O4

2-

Cr2O7

5C2O4

2-

14H

+ 14H

+ 10e

10CO2
2Cr

+ Cr2O7

2-

2+

10CO2

+ 10e
+

7H2O
+ 2Cr

2+

+ 7H2O

Figure 1: flow chat for Experiment 3

Figure 2: flow chat for Experiment 4

nm

Figure 3: flow chat for Experiment 5