Objective

1. To synthesize Potassium Tris(oxalato) Chromium(iii) Trihydrate, K3[Cr(C2O4)3]·3H2O

2. To prepare a Copper(ii) Oxalate Complexes
3. To synthesize Potassium Tris(oxolato) Ferrate(iii) Trihydrate, K3[Fe(C2O4)3]·3H2O

Introduction

The important aspects in any chemicals research is the preparation of the new compounds and
this process called synthesis. A synthesis reaction or direct combination reaction is one most
common types of chemicals reactions. In a synthesis reaction there is two or more chemicals
combine to form a more complex product. In this experiment we are going to synthesizing
coordination compound. Coordination compound is the product of a lewis acid-base reaction in
which natural molecules or anions bond to central metal ion by coordinate covalent bonds. A
coordinate covalent bond is a covalent bond in which one atom supplies both electrons. This
type of bonding is different from a normal covalent bond in a bond which is each atom supplies
one electron. Transition metal readily formed coordination compound and resulting in bright
colour.

In this experiment, we performed three experiment related to synthesis of crystals. The crystal
that we prepared were Potassium Tris(oxalato) Chromium(iii) Trihydrate, Copper(ii) Oxalate
Complexes and Potassium Tris(oxalato) Ferrate(iii) Trihydrate.

In experiment 3, chromium(iii) is the most stable oxidation state of chromium and tend to form
octahedral complexes. The colour of these complex is determined by the ligands attached to the
Chromium centre. Two oxalate anions 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)2H2O2], two (C2O4)2- ion or two H2o molecules can be on the
same side of octahedron structure of the complex ion giving the cis-isomers or on the opposite
sides giving trans-isomers.

In experiment 4, copper is transition metal when potassium oxalate solution was added to Cu+
aqeous solution copper(ii) oxalate was formed. Oxalate complexes are coordination compounds
produced by reacting oxalic aicd with a transition metal. For copper(ii) oxalate K2[Cu(C2O4)2
(H2O)2] complexes, copper is a transition metal that acts as Lewis acid while the oxalate ion as
well as water act as Lewis bases.
In experiment 5, Potassium tris(oxalato)ferrate (III) is a metal complex of iron with three
oxalate ligands (C2O42-) bonded to every central metal atom.These ligands are bidentate,
meaning that each of them binds to the metal atom at 2 different places. It has the chemical
formula K3[Fe(C2O4)3]·3H2O, and the three-dimensional structure. Such complexes are often
utilized in schools anduniversities to introduce various concepts such as ligand strength,metal
complexes, and ligand replacement. Potassium tris(oxalato)ferrate (III) is hygroscopic and light
sensitive in nature.

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. The actual mass of coordination compound synthesized,
called the actual yield is usually less than the theoretical yield.

𝐴𝑐𝑡𝑢𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
% Yield = 𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑 x 100%
PROCEDURE

Experiment 3:
Experiment 4 :
Experiment 5 :
QUESTION

Experiment 3:

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

Chromium in K2Cr2O7 Chromium in K3[Cr(C2O4)3]·3H2O

K+, O2- K+, (C2O4)-2

K2Cr2O7 = neutral, 0 K3[Cr(C2O4)3] = 0
(2*+1) + (2*Cr) + (7*-2) = 0 (3*+1) + Cr + (3* -2) = 0
(2) + (2Cr) – 14 = 0 (3) + Cr + (-6) = 0
2Cr – 12 = 0 Cr = +3
Cr = +6 Oxidation state for Chromium ions is +3
Oxidation state for Chromium ions is
+6

2. Write two half equations for each reaction involved in the preparation of the complex
using oxalic acid dihydrate, K2C2O4.H2O, and potassium dichromate, K2Cr2O7, and a
balanced equation for the overall reaction.

5C2O42-  10 CO2 + 10e

Cr2O72- + 14H+ +10e  2Cr2+ + 7H2O

5C2O42- + 14H+ + Cr2O72-  10CO2 + 2Cr2- + 7H2O

RESULTS

Experiment 3: mass of K3[Cr(C2O4)3]·3H2O

Mass of filter paper 0.3357 g

Mass of filter paper + crystals 5.5295 g
Mass of crystal 5.1938 g
Theoretical yield 5.6051 g
Percent yield 92.66 %

7H2C2O4 + 2K2C2O4.H2O + K2Cr2O7  4CO2 + 3H2O + 2K3[Cr(C2O4)3].3H2O

1 𝑚𝑜𝑙 H2C2O4 2 𝑚𝑜𝑙 K3[Cr(C2O4)3].3H2O

5.0031 g of H2C2O4 × ×
90.03 𝑔 H2C2O4 7 𝑚𝑜𝑙 H2C2O4

= 0.0159 mol K3[Cr(C2O4)3].3H2O

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

1.8014 g of K2Cr2O7 × ×
294.18 𝑔 K2Cr2O7 1 𝑚𝑜𝑙 K2Cr2O7

= 0.0122 mol K3[Cr(C2O4)3].3H2O

1 𝑚𝑜𝑙 K2C2O4.H2O 2 𝑚𝑜𝑙 K3[Cr(C2O4)3].3H2O

2.1111g of K2C2O4.H2O × ×
184.22 𝑔 K2C2O4.H2O 2 𝑚𝑜𝑙 K2C2O4.H2O

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

The limiting reactant is K2C2O4.H2O

Molar mass of K3[Cr(C2O4)3].3H2O = 487.4 g

The theoretical yield of K3[Cr(C2O4)3].3H2O = (0.0115 mol) (487.4 g)

= 5.6051 g

5.1938 g
Percentage yield of K3[Cr(C2O4)3].3H2O = × 100%
5.6051 g

= 92.66 %
Experiment 4: mass of K2[Cu(C2O4)2 (H2O)2]

Mass of filter paper 0.3357g

Mass of filter paper + crystals 2.6824 g
Mass of crystal 2.3467 g
Theoretical yield 2.8304 g
Percent yield 83.54 %

CuSO4.5H2O + 2K2C2O4.H2O  K2[Cu(C2O4)2 (H2O)2] + K2SO4 + 5H2O

1 𝑚𝑜𝑙 CuSO4.5H2O 1 𝑚𝑜𝑙 K2[Cu(C2O4)2 (H2O)2]

2.0034 g of CuSO4.5H2O × ×
249.61 𝑔 CuSO4.5H2O 1 𝑚𝑜𝑙 CuSO4.5H2O

= 0.0080 mol K2[Cu(C2O4)2 (H2O)2]

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

6.2042 g of K2C2O4.H2O × ×
184.22 𝑔 K2C2O4.H2O 2 𝑚𝑜𝑙 K2C2O4.H2O

= 0.0168 mol K2[Cu(C2O4)2 (H2O)2]

The limiting reactant is CuSO4.5H2O

353.81 𝑔 K2[Cu(C2O4)2 (H2O)2]

0.0080 mol K2[Cu(C2O4)2 (H2O)2] ×
1 mol K2[Cu(C2O4)2 (H2O)2]

= 2.8304 g K2[Cu(C2O4)2 (H2O)2]

2.3467 𝑔
Percentage yield of K2[Cu(C2O4)2 (H2O)2] = 2.8304 𝑔 × 100%

= 83.54 %
Experiment 5: mass of K3[Fe(C2O4)3]·3H2O

Mass of filter paper 0.3357 g

Mass of filter paper + crystals 4.8643 g
Mass of crystal 4.5286 g
Theoretical yield 6.2875 g
Percent yield 72.03 %

Fe(NH4)2(SO4)2· 6H2O + H2C2O4  FeC2O4+ H2SO4 + (NH4)2SO4 + 6H2O

Fe3+ + 3OH-  Fe(OH)3

3K2C2O4 + 2Fe(OH)3 + 3H2C2O4  2K3[Fe(C2O4)3]·3H2O + 3H2O

1 𝑚𝑜𝑙 Fe(NH4)2(SO4)2· 6H2O O

5.0196 g of Fe(NH4)2(SO4)2· 6H2O × 392.02 𝑔 Fe(NH4)2(SO4)2· 6H2O

1 𝑚𝑜𝑙 𝐹𝑒 2+ 2 𝑚𝑜𝑙 𝐹𝑒 3+ 1 𝑚𝑜𝑙 Fe(OH)3

= 0.0128 mol FeC2O4 × × ×
1 𝑚𝑜𝑙 FeC2O4 2 𝑚𝑜𝑙 Fe2+ 1 𝑚𝑜𝑙 Fe3+

2 𝑚𝑜𝑙 K3[Fe(C2O4)3]·3H2O
= 0.0128 mol Fe(OH)3 × 2 𝑚𝑜𝑙 Fe(OH)3

= 0.0128 mol K3[Fe(C2O4)3]·3H2O

1 𝑚𝑜𝑙 K2C2O4 2 𝑚𝑜𝑙 K3[Fe(C2O4)3]·3H2O

3.509 g K2C2O4 × ×
166.23 𝑔 K2C2O4 3 𝑚𝑜𝑙 K2C2O4

= 0.0140 mol K3[Fe(C2O4)3]·3H2O

1 𝑚𝑜𝑙 H2C2O4 2 𝑚𝑜𝑙 K3[Fe(C2O4)3]·3H2O

2.0263 g H2C2O4 × ×
90.03 𝑔 H2C2O4 3 𝑚𝑜𝑙 H2C2O4

= 0.0150 mol K3[Fe(C2O4)3]·3H2O

The limiting reactant is Fe(NH4)2(SO4)2· 6H2O

491.21 𝑔 K3[Fe(C2O4)3]·3H2O
0.0128 mol K3[Fe(C2O4)3]·3H2O × 1 𝑚𝑜𝑙 K3[Fe(C2O4)3]·3H2O

= 6.2875 g

4.5286 𝑔
Percentage yield K3[Fe(C2O4)3]·3H2O = 6.2875 𝑔 × 100%

= 72.03 %
DISCUSSION

In this experiments, we had to prepared and synthesized Potassium Tris(oxalato) Chromium(iii)

Trihydrate, K3[Cr(C2O4)3]·3H2O, Copper(ii) Oxalate Complex ,and Potassium Tris(oxolato)
Ferrate(iii) Trihydrate, K3[Fe(C2O4)3]·3H2O. Transition metals have high tendency to form
complex ions or coordination compound. Complex ions are a central metal cation bonded to
one or more molecules or ions. They typically consist of a complex and a counter ion. Those
compounds undergoes a crystallisation process to synthesis crystal. The results that we obtained
from these experiment were 5.1938 g grey solid of K3[Cr(C2O4)3]·3H2O , 2.3467 g of blue
solid of K2[Cu(C2O4)2 (H2O)2], 4.5286 g fluorescent green solid of K3[Fe(C2O4)3]·3H2O. The
percentage yield we get after calculation were 92.66% of K3[Cr(C2O4)3]·3H2O, 83.54% of
K2[Cu(C2O4)2 (H2O)2], and 72.03% of K3[Fe(C2O4)3]·3H2O.

In experiment 3, 10 ml of water was added to 5.0031 g of oxalic acid. After that 1.8014 g of
potassium dichromate, K2Cr2O7 was added to mixture and dissolved slightly in the acid solution.
And this reaction take place,

K2Cr2O7 + H2C2O4  H2Cr2O7 + K2C2O4

The orange coloured mixture vigorously formed and a funnel was used to prevent the vigorous
gases out from the conical flask, let the mixture sit for 15 minutes. Then 2.10 g of potassium
oxalate monohydrate, K2C2O4.H2O, was weigh and added to the hot green-black mixture.

K2Cr2O7 + 3H2C2O4 + 6K2C2O4.H2O  2K3 [Cr2(C2O4)3].H2O + 6CO2 + 9H2O

The mixture then was put on the hot plate to boil for 5 minutes. Let the mixture to cool at the
room temperature and add 10 ml of 95% of ethanol. The mixture then was let to cool in ice for
15-30 minutes or when the precipitate completely appears with frequent stirring. To collect the
formation of crystal or complex, we use suction filtration process. The precipitate was washed
with two portion of 5 ml 1:1 ethanol/water then followed by 95% ethanol to wash out all the
precipitate from the conical flask. Then, the solid was placed in a watch glass and allow it to
dry in oven. The mass of the product that we get is 5.1938 g of K3[Cr(C2O4)3]·3H2O which is
in dark grey colour. The dark gery colour represent formation of chromium metal. The crystal
was keep for the next experiment.
In experiment 4, oxalate complexes produced by oxalic acid and transition metal. Copper act
as a lewis acid while oxalate ions and water act as lewis bases. We had prepared copper(ii)
oxalate complexes, it was formed when copper(ii) sulphate pentahydrate CuSO4.5H2O, reacted
with potassium oxalate monohydrate, K2C2O4.H2O. First, copper(ii) sulphate pentahydrate was
dissolved in 30 ml of distilled water and heated on hot plate. After that, dissolved potassium
oxalate monohydrate with 30 ml distilled water. By using funnel, copper(ii) sulpahate was heat
earlier and added into potassium oxalate solution and swirled. Then, the solution chilled in an
ice bath for 30-60 minutes. Blue crystals formed in the cooling process. The solid was collected
through suction filtration and washed the crystal twice with 3 ml portion of cold water. Then,
the crystal was put in the oven to dry. The crystal was keep after the drying process to use in
the next experiment. Blue solid represent formation of copper(ii) in the solution.

CuSO4.5H2O + 2K2C2O4.H2O  K2[Cu(C2O4)2 (H2O)2] + K2SO4 + 5H2O

In experiment 5, potassium tris(oxalato) ferrate(iii) trihydrate is hygroscopic and sensitive in
nature. Ferum act as lewis acid that react with neutral molecule and C2O4 act as lewis bases and
H2O act as ligands. Ferrous ammonium sulfate was dissolved in the oxalic acid and formed
yellow precipitate. The chemical equation was shown belown:

Fe(NH4)2(SO4)2.6H2O + H2C2O4 → FeC2O4 (s) + H2SO4 + (NH4)2SO4 + 6H2O

After that the solution was heated to boiling , FeC2O4 is finely divided precipitate and tend to
colloid. But by heating the solution cause to coagulate and seperating the precipitate from the
solution. The supernatant is decanted. Potassium oxalate was added to the FeC2O4 precipitate
which is produce a slightly basic solution for oxidation ferrous ion to ferric ion by dropwise of
hydrogen peroxide and the solution was turn to dark brown with precipitate. The dark brown
colour occur when OH- ion concentration was high enough to react with Fe3+ to form ferric
hydroxide The below reation take placed:

H2O + HO2- + 2Fe2+  2Fe3+ 3OH-

Fe3+ + 3OH-  Fe(OH)3

Oxalic acid was added until excess, the solution turn colourless solution. Because oxalic acid
dissolved the Fe(OH)3 and the soluble complex is formed

3K2C2O4 + 2Fe(OH)3 + 3H2C2O4 → 2K3[Fe(C2O4)3].3H2O + 3H2O

The colourless solution was turn to grey green solution. The solid or the crystal was obtaian by
suction filtration process which the solution was washed with 30ml 95% ethanol slowly and
leave the solution to recrystallize. After the green crystal is filtered and washed with 1:1
ethanol/water and cooled acetone. Let the solution for several days and the green flourecent
crystal formed.
There are some error may be occur during run the experiments that will be effect the result.
There may be some product remianed in the Buchner funnel when we collect the product afer
suction filtration process and transfered to watch glass. Also the product may be dissolved when
we washed the product with ethanol and cold water. And we misread the instruction where it
say to drowise 10 ml of H2O2 but we only do 5 drop not 10ml wisedrop. The precaution step
that need to take to prevent any injured or any mistake that effect our result. Make sure the
glassware that we use is cleaned first with distilled water to prevent the contaminated to our
pproduct. Next, wearing golves to handle high concentrated solution because the chemical
cloud absorbed into our skin and can cause serve damage. Next, when we heat the solution of
ferrous ammonium sulphate and oxalic acid dihydrate we need to slow the hot plate to avoid
the bumping of the solution.

CONCLUSION

In conclusion, Potassium tri(oxalato)chromium(III)trihydrate ,K3[Cr(C2O4)3].3H2O was

synthesize.The actual mass obtained was 5.1938 g while the theoretical yield obtained was
5.6051 g . So the theoretical yield is 92.66%. Copper(II)oxalate complexes, K2[Cu(C2O4)2
(H2O)2] was synthesize.The actual mass obtained was 2.3467 g while the theoretical yield
obtained was 2.8304 g . So the theoretical yield is 83.54 %. Potassiumtris
(oxalato)Ferrate(III)Trihydrate , was K3[Fe(C2O4)3].3H2O synthesize.The actual mass obtained
4.5286 g was while the theoretical yield obtained was . So 6.2875 g the theoretical yield is
72.83%

REFERENCE

1. https://www.academia.edu/11002377/Title_Preparation_And_Studies_of_Potassium
2. https://pubs.acs.org/doi/pdf/10.1021/ed061p1098
3. https://www.researchgate.net/publication/263032238_The_crystal_structures_of_potas
sium_Trisoxalato-chromateIII_and_-aluminateIII_trihydrate_A_reinvestigation
4. https://www.chegg.com/homework-help/questions-and-answers/-synthesis-potassium-
tris-oxalato-chromate-iii-hydrated-b-synthesis-tris-acetylacetonato-i-q4368280
5. https://www.scribd.com/document/329497428/Lab-Report-Experiment-3-4-and-5