LABORATORY REPORT

CHM577
(INORGANIC CHEMISTRY)
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Name : IRFAN NURHADI BIN AZAHAR

Group members :

PROGRAMME: CHM577
GROUP: AS2223A1
EXPERIMENT: SYNTHESIS OF POTASSIUM TRIS(OXALATO)CHROMIUM(III) TRIHYDRATE:
K3[Cr(C2O4)3].3H2O

DATE OF EXPERIMENT: 2 DECEMBER 2021

DATE OF REPORT SUBMISSION: 9 DECEMBER 2021

NAME OF LECTURER: DR ASIAH ABDULLAH

 EXPERIMENT 3

SYNTHESIS OF
POTASSIUM TRIS(OXALATO)CHROMIUM(III) TRIHYDRATE:
K3[Cr(C2O4)3].3H2O

PURPOSE

The purpose of this experiment is to synthesize potassium tris(oxalato)chromium(III) trihydrate,

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

INTRODUCTION

One of the important aspects of any chemical research is the preparation of new compounds. This
process is called synthesis. In this experiment, you will synthesize a special kind of compound
called a coordination compound. A coordination compound consists of a central metal ion
chemically bonded to one or more atoms or groups of atoms (ligands) by coordinate covalent
bonds. Transition metals readily form these coordination compounds, often resulting in bright
colours.

Chromium(III), the most stable oxidation state of chromium, forms a number of complexes, in
which six monodentate ligands surround the cation octahedrally. In the above compound, two
oxalate anions (bidentate ligands) and two water molecules coordinate the chromium cation to
provide oxygen atoms at the corners of the octahedron. Two geometrical isomers exist for the
complex ion, [Cr(C2O4)2(H2O)2], two (C2O4)2- ions [or two H2O molecules] can be on the same
side of octahedron structure of the complex ion giving the cis-isomer or on the opposite sides
giving trans-isomer.

The amount of coordination compound expected from a given mass of reactants can be calculated
and is called the theoretical yield. The actual mass of coordination compound synthesized, called
the actual yield is usually less than the theoretical yield.

Actual yield
% Yield =  100%
Theoretical yield

PROCEDURE

solution of 5.00 g (5.0272 g) of oxalic acid was make in 10 mL of water in a conical flask. Slowly
added 1.8 g (1.8740 g) of potassium dichromate, K2Cr2O7, to the mixture in small portions and
placed the funnel on the conical flask. The orange coloured mixture should spontaneously warm-
up almost to boiling (BE CAREFUL HERE as a vigorous evolution of gas commences). When the
reaction has subsided (about 15 minutes), 2.10 g (2.1085 g) of potassium oxalate monohydrate,
K2C2O4.H2O, was dissolved in the hot green-black liquid and heated to boil for 5 minutes. Cooled
the viscous reaction to room temperature and 10 mL of 95 % ethanol added and cool the beaker
further in ice with frequent stirring. After cooling in ice for 15-30 minutes or when the precipitation
appears complete, the complex by suction filtration was collected. Washed the crystals with two 5
mL portions of 1:1 ethanol/water followed by 13 mL of 95% ethanol. Placed the solid in a beaker
or glass plate and allow it to dry in the oven (about 80 C). Determine the mass of the product, and
hence, the percentage yield. Transfer to a labelled vial. Keep for the next experiment.

RESULT

8H+ +3H2C2O4+6K2C2O4.H2O+K2Cr2O7 → 6CO2+9H2O+8K+ + 2K3[Cr(C2O4)3].3H2O

The number of moles H2C2O4 : = 5.02720 / (2+24+64) =0.05636 mol

The number of moles K2Cr2O7 =1.8740 / 294 =0.00637 mol

The limiting reactant is K2Cr2O7

1 mol of K2Cr2O7 = 2 mol of K3[Cr(C2O4)3].3H2O

0.0637 mol K2Cr2O7 = 0.01274 mol of K3[Cr(C2O4)3].3H2O

Molar mass of K3[Cr(C2O4)3].3H2O = 487

The theoretical yield = 0.01274(487) = 6.20438 g

Mass of K3[Cr(C2O4)3].3H2O obtained is = 4.6887g

Percentage yield of K3[Cr(C2O4)3].3H2O is = 4.6887g / 6.20438 g x 100% = 75.6%

DISCUSSION

In this experiment , we haves tudied how to synthesis coordination compound . Coordination

compound formed when lewis acid that is cu2+ are reacted with lewis base that is C2O4 and
H2O. Potassium dichromate , K2Cr2O7 dissoved slightly acid solution , excess oxalic acid ,
H2C2O4 is added and the following reactiion take place:

8H+ +3H2C2O4+6K2C2O4.H2O+K2Cr2O7→ 6CO2+9H2O+8K+ +2K3[Cr(C2O4)3].3H2O

Vigorouly orange solution was formed and filtered then leaves for crystallization. Potassium
oxalate , K2C2O4.H2O was added . Dark green solution was formed and was heated for five
minutes.
After that we allowed the solution cool at room temperature.The dark green crystal was was
filtered and washed with 1:1 ethanol/water and followed by 13 ml of acetone. The mass of the
dark green crystal obtained is 4.6887 g .The theoretical yield obtained is 6.20438 g.So the
percentage yield is 75.6 % .There is large different to achieve 100% of theoretical yield.There
maybe error occur when we are doing an experiment.So there is some precaution that we must
take care while we are doing an experiment .
First we need to makesure our conical flask is cleaned before we are using it, this is important
because there maybe left other substance left in the conical flask and cause our product was
contaminated.We also need to becareful when heating oxalic acid , potassium chromate and
potassium oxalate as it will bump when we heat too long.

CONCLUSION

Potassium tri(oxalato)chromium(III)trihydrate , K3[Cr(C2O4)3].3H2O was synthesize.The actual

mass obtained was 4.6887 g while the theoretical yield obtained was 6.20438 g . So the
theoretical yield is 75.6%

REFERENCES

1) Duward F. Shiver , Inorganic syntheses , copyright 1979 , published by John Wiley & Sons,
Inc. Page : 127

2) Raymond Chang and Kenneth A.Goldsby , Chemistry , eleventh edition published by Mc

Graw Hill copyright 2013 , page 103 and 104

QUESTION

1. What is the oxidation state of chromium in K2Cr2O7 and in the product?

2. Write two half-equations for each reaction involved in the preparation of the complex using
oxalic acid dihydrate, H2C2O4.2H2O, and potassium dichromate, K2Cr2O7, and a balanced
equation for the overall reaction.

Oxidation state of chromium in K2Cr2O7 : +1(2) + 2x -2(7) =0

2x =12

X= +6

Oxidation state of chromium in product: x + 0(2) + 0(2) = -1

x= -1

Two half equations:

Oxalic acid dehydrate: H2C2O4 → 2CO2 + 2H+ + 2e- ( Oxidation reaction)

Potassium dichromate: Cr2O72−(aq) + 14H+ + 6e− → 2Cr3+(aq) + 7H2O

(Reduction reaction)
 Balanced equation for overall equation: K2[Cr207] + 7H2C204*2H20
→2{K[Cr(H20)2(C204)2].2H20} + 6CO2 + 13H2O

DATA SHEET FOR EXPERIMENT 3

POTASSIUM TRIS(OXALATO)CHROMIUM(III) TRIHYDRATE SYNTHESIS

Name: IRFAN NURHADI BIN AZAHAR

UiTM ID No.: 2020819572

Date of Experiment: 2 DECEMBER 2021

RESULTS

1. Theoretical yield of K3[Cr(C2O4)3].3H2O (mass) ______6.20438 g_____

4.6887 g
2. Mass of K3[Cr (C2O4)3].3H2O obtained ____________________

3. Percent yield of K3[Cr(C2O4)3].3H2O _______75.6%________