INORGANIC CHEMISTRY (CHM 577)

LABORATORY REPORT
EXPERIMENT 3: SYNTHESIS OF POTASSIUM
TRIS(OXALATO) CHROMIUM (III) TRIHYDRATE
EXPERIMENT 4: PREPARATION OF COPPER(II)
OXALATECOMPLEX
EXPERIMENT 5: SYNTHESIS OF POTASSIUM
TRIS(OXALATO)FERRATE(III) TRIHYDRATE

NAME NURUL NAJWA NABILA BINTI AHMAD SHAHIR

STUDENT ID 2022608166

GROUP AS2223M2

LECTURER NAME DR. MOHD AZIZI NAWAWI

SUBMISSION 15TH NOVEMBER 2023

DATE
OBJECTIVE
1. To synthesis potassium tris(oxalate) chromium(iii)trihydrate.
2. To prepare copper (ii) oxalate complex.
3. To synthesize potassium tris (oxalate) ferrate (iii) trihydrate.

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 suppliesone
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 existfor 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 oppositesides
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 acid 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 (C2O4)2- 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 and universities 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 = x 100%
𝑡ℎ𝑒𝑜𝑟𝑖𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
PROCEDURE

Experiment 3

1. 5.00 g of oxalate acid was dissolved in 10 ml distilled water in a conical flask. 1.8g of
potassium dichromate was added into the mixture in small portions and the funnel was
placedon 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
Precipitatewas 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 untilthe solid dissolves.
2. 6.20 g of potassium oxalate monohydrate was dissolved in 30 ml of distilled
waterin another flask.
3. The heated CuSO4 solution was added into the flask contained potassium
4. oxalateMonohydrate slowly. The flask was swirled slowly to mix.
5. The mixture was cooled in ice bath for 30 minutes. Blue crystals were formed.
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 5
Procedure A

1. 5.00 g of ferrous ammonium sulphate was dissolved in 25 ml distilled

waterContaining 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
intothe 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
oxalateMonohydrate. It was heated to approximately 40oC. 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 ofdistilled 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 the Buchner funnel. 30 mL of 95% ethanol was added slowly to
the solution. Any crystals that were formed were re-dissolved. 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
with10 ml of 1:1 ethanol/distillation water for two times. The crystals were
washed withCold 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 AND CALCULATION
Experiment 3: mass of K3 [Cr(C2O4)3].3H2O

Mass of watch glass and filter 33.8024 g

paper
Mass of watch glass and filter 38.9122 g
paper + crystals
Mass of crystals 5.1098 g
Theoretical yield 5.6046 g
Percent yield 91.17 %

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

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

1mol H2C2O4 2 mol K3[Cr(C2O4)3.3H2O

5.0096 g H2C2O4 x ( )x( )
90.02 g H2C2O4 7 mol H2C2O4
= 0.0159 mol K3[Cr(C2O4)3]. 3H2O

1mol K2Cr2O7 2 mol K3[Cr(C2O4)3.3H2O

1.8096 g K2Cr2O7 x ( )x( )
294.2 g K2Cr2O7 1 mol K2Cr2O7
= 0.0123 mol K3[Cr(C2O4)3]. 3H2O

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

2.1090 g K2C2O4.H2O x ( )x( )
184.22g 2K2C2O4.H2O 2 mol 2K2C2O4.H2O
= 0.0114 mol K3[Cr(C2O4)3]. 3H2O

So, K2C2O4.H2O is limiting reactant.

Molar mass of K3[Cr(C2O4)3].3H2O = 487.36 g

The theoretical yield of K3[Cr(C2O4)3].3H2O = (0.0114 mol) (487.36 g)

= 5.5559 g

5.1098 g
Percentage yield of K3[Cr(C2O4)3].3H2O = x 100%
5.6046 g
= 91.17 %
 Experiment 4: mass of K2 [Cu(C2O4)2(H2O2)

Mass of watch glass and 33.8024 g

filter paper
Mass of watch glass and 36.339 g
filter paper + crystals
Mass of crystals 2.5366 g
Theoretical yield 2.8567 g
Percent yield 88.52 %

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

Theoretical mass of K2C2O4.H2O

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

2.0236 g of CuSO4.5H2O x ( )x( )
249.61 g H2C2O4 1mol CuSO4.5H2O
= 0.0081 mol K2 [Cu(C2O4)2(H2O)2

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

6.2260 g K2C2O4.H2O x ( )x( )
184.22 g K2C2O4.H2O 2 mol K2C2O4.H2O
= 0.0169 mol K2 [Cu(C2O4)2(H2O)2]

So, CuSO4.5H2O is limiting reactant.

The theoretical yield of K2 [Cu(C2O4)2(H2O)2]

353.79 g K2[Cu(C2O4)2 (H2O)2]
0.0081 mol K2 [Cu(C2O4)2(H2O)2 x ( 1mol K2[Cu(C2O4)2(H2O)2 )
= 2.8657 g K2 [Cu(C2O4)2(H2O)2]

2.5366 g
Percentage yield of K2 [Cu(C2O4)2(H2O)2] = x 100%
2.8657 g
= 88.52 %
 Experiment 5: mass of K3[Fe(C2O4)3].3H2O

Mass of watch glass and 33.8024 g

filter paper
Mass of watch glass and 38.2118 g
filter paper + crystals
Mass of crystals 4.4094 g
Theoretical yield 6.2875 g
Percent yield 70.10 %

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

Fe3+ + 3OH- → Fe (OH)3

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

1mol Fe (NH4)2(SO4)2.6H2O
5.0264 g Fe (NH4)2(SO4)2. 6H2O x ( )
392.02 g Fe (NH4)2(SO4)2.6H2O

1 mol Fe2+ 2 mol Fe3+ 1 mol Fe(OH)3

= 0.0128 mol FeC2O4 x (1 mol FeC2O4 ) x ( )x( )
2 mol Fe2+ 1 mol Fe3+

2 mol K3[Fe(C2O4)3].3H2O
= 0.0128 mol Fe (OH)3 x ( 2 mol Fe(OH)3
)
= 0.0128 mol K3[Fe(C2O4)3].3H2O

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

3.5004 g K2C2O4 x ( )x( 3 mol K2C2O4
)
166.23 g K2C2O4
= 0.0140 mol K3[Fe(C2O4)3].3H2O

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

2.0024 g H2C2O4 x (90.02 g H2C2O4 ) x ( )
3 mol K2C2O4
= 0.0184 mol K3[Fe(C2O4)3].3H2O

So, Fe (NH4)2(SO4)2. 6H2O is limiting reactant.

The theoretical yield of K3[Fe(C2O4)3].3H2O 0.0128 mol

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

= 6.2875 g K3[Fe(C2O4)3].3H2O
 4.4094 g
Percentage yield of K3[Fe(C2O4)3].3H2O = x 100%
6.2875 g

= 70.13 %

DISCUSSION
In this experiment, 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 under goes a crystallization process to synthesis crystal. The result we obtained
from this experiment were 5.1098 g grey solid of K3[Cr(C2O4)3] ·3H2O, 2.5366 g of blue
solid of K2 [Cu(C2O4)2 (H2O)2], 4.4078 g fluorescent green solid of K3[Fe(C2O4)3] ·3H2O.
The percentage yield we get after calculation were 91.17 % of K3[Cr(C2O4)3] ·3H2O,
88.52% of K2 [Cu(C2O4)2 (H2O)2], and 70.10% of K3[Fe(C2O4)3] ·3H2O.

In experiment 3, 10 ml of water was added to 5.0096 g of oxalic acid. After that 1.8096 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 mass of the product that we get is 5.1098 g of K3[Cr(C2O4)3] ·3H2O which is in dark
grey colour. The dark grey colour represent formation of chromium metal. The crystal was
keeps 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, react with potassium oxalate monohydrate, K2C2O4.H2O.

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 below:

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 separating 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 reaction 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 obtain by
suction filtration process which the solution was washed with 30 ml 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.

CONCLUSION

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

synthesize. The actual mass obtained was 5.1098 g while the theoretical yield obtained was
5.6046 g. So, the percentage yield is 91.17 %. Copper (II) oxalate complexes, K2 [Cu(C2O4)2
(H2O)2] was synthesize. The actual mass obtained was 2.5366 g while the theoretical yield
obtained was 2.8567 g. So, the percentage yield is 88.52 %. Potassium tris(oxalato)
Ferrate(III) trihydrate, K3 [Fe(C2O4)3].3H2O was synthesize. The actual mass obtained was
4.4094 g while the theoretical yield obtained was 6.2875 g. So, the percentage yield is
70.13%.
QUESTIONS
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
complexusing oxalic acid dihydrate, K2C2O4.H2O, and potassium dichromate,
K2Cr2O7, and a balanced equation for the overall reaction.

5C2O42- → 10CO2 + 10e-

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

REFERENCES
1. Hadariah Bahron Kamariah Muda, Sharifah Rohaiza Syed Omar,
Karimah/2015/Inorganic Chemistry: Experiment for Undergraduate/UITM
PRESS.
2. Silberberg, Amaties/2015/chemistry: The molecular nature of matter and
change 7thedition/Mc Graw Hill education.
JOTTER

EXPERIMENT 3
EXPERIMENT 4
EXPERIMENT 5