LABORATORY REPORT

COURSE CODE

CHM475 (INORGANIC CHEMISTRY)

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EXPERIMENT 3: SYNTHESIS OF POTASSIUM

TRIS(OXALATO)CHROMIUM (III) TRIHYDRATE
EXPERIMENT 4: SYNTHESIS OF COPPER(II)
OXALATE COMPLEXES
EXPERIMENT 5: SYNTHESIS OF POTASSIUM
TRIS(OXALATO)FERRATE(III) TRIHYDRATE

Experiment 3: Synthesis Of Potassium Tris(Oxalato)chromium(III) Trihydrate:

Cr 3 H 2 O

K3
Experiment 4: Synthesis Of Copper(II) Oxalate Complexes
Experiment 5: Synthesis Of Potassium Tris(Oxalato)ferrate(III) Trihydrate

Introduction
The synthesis process is used in the preparation of new compounds or complexes. This
experiment focused on the preparation of coordination compound which consists of a central
metal ion chemically bonded to ligands by coordinate covalent bonds. The transition metals
that form coordination compound with ligands have special characteristics in which they
form colored compound. In this experiment, the transition metals involved are chromium(III),
copper(II) and ferrous(III). The amount of compound used in this experiment is used to
calculate the theoretical yield which then is compared with the actual yield to get the
percentage yield.
Percentage yield=

Actual yield
100%
T h eoretical yield

Objective
1. To synthesize three different compounds which are potassium tris(oxalato)
chromium(III) trihydrate, copper(II) oxalate complex and potassium tris(oxalato)
ferrate(III) trihydrate.
2. To determine the percentage yield of each compound.

Apparatus and Equipment

Oxalic Acid
H2O
Potassium dichromate, K2Cr2O7
Potassium oxalate monohydrate, K2C2O4.H2O
Ethanol
1:1 ethanol/water
Copper(II) sulphate pentahydrate, CuSO4.5H2O
Ferrous ammonium sulfate
Dilute sulfuric acid
6% H2O2
Filter paper
Beaker
Ice cube
Glass rod
Funnel
Conical flask
Beaker
Measuring cylinder
Dropper

Hot plate
Weighing boat

Procedure
Experiment 3
1. 5.00 g of oxalic acid was dissolved in 10 mL of distilled water in the conical flask.
2. 1.8 g of potassium dichromate, K 2 Cr 2 O7 was added to the solution and the funnel
was placed on the conical flask.
3. After about 15 minutes, 2.10 g of potassium oxalate monohydrate,
4.
5.
6.
7.
8.

K2C2O4. H2 O

was dissolved in the hot green-black solution.

The mixture was heated to boiling for 5 minutes.
The solution was cooled to room temperature and 10 mL of 95% ethanol was added.
The flask was cooled in the ice bath with frequent stirring.
After 15-30 minutes, the suction filtration was conducted to collect the complex.
The crystal complex obtained was washed twice with 5 mL portions of 1:1

ethanol/water followed by 13 mL of 95% ethanol.

9. The solid was dried in the oven and the mass was obtained.
Experiment 4
1. 2.00 g of copper(II) sulphate pentahydrate,

CuSO 4 . 5 H 2 O

was dissolved in 30 mL

of distilled water in a conical flask.

2. The solution was heated on the hot plate until the solids dissolved.
3. 6.20 g of potassium oxalate monohydrate, K 2 C 2 O 4 . H 2 O was dissolved in 3040 mL distilled water.
4. The heated copper(II) sulphate solution was added to the solution and the flask was
5.
6.
7.
8.

swirled slowly to mix.

The flask was placed in the ice bath for 30-60 minutes.
Then, the suction filtration was conducted.
The crystal was washed twice with 3 mL portions of cold water.
The crystal was dried in the oven and the mass was obtained.

Experiment 5
1. 5.00 g of ferrous ammonium sulfate was dissolved in the beaker containing 20 mL of
distilled water and 1 mL of dilute sulfuric acid.
2. In a separate beaker, 2.50 g of oxalic acid was dissolved in 25 mL of distilled water.

3. Then, the second solution was added to the first solution.

4. The mixture was heated to boiling.
5. 15 mL hot water was added to the yellow precipitate and the solution was stirred. The
supernatant was decanted.
6. Another 15 mL hot water was added to the precipitate.
7. 3.50 g solid potassium oxalate monohydrate was added and the solution was heated to
approximately 40 .
8. At 40 , 10 mL of 6%

H 2 O2 was added dropwise and the solution was stirred

continuously. During this step, the temperature was maintained at

40

or above

but not exceed 50 .

9. The solution was heated to boiling.
10. A solution of 2.00 g of oxalic acid dihydrate in 30 mL of distilled water was prepared.
20 mL of this solution was added initially to the mixture. The rest was added until the
brown precipitate dissolved.
11. The clear solution was boiled. Then, the suction filtration was conducted. 30 mL of
95% ethanol was added.
12. The filtrate was further heated to redissolve any crystal and the solution was left to
crystallize for one week.
13. After one week, suction filtration was performed again. The crystal was washed twice
with 1:1 ethanol/water. Then, the crystal obtained was dried and weighed.

Data and Results

Experiment 3
Chemical
Oxalic acid
Potassium dichromate
Potassium oxalate monohydrate

Theoretical yield of product (g)

Actual yield of product (g)
Percent yield of product (%)

Mass (g)
5.0020
1.8005
2.1005

5.8490
4.6215
79.01%

8H+ + 3H2C2O4 + 6K2C2O4.H2O + K2Cr2O7 6CO2 + 9H2O + 8K+

+ 2K3[Cr (C2O4)3].3H2O
Molar mass of H2C2O4 = 2(1.008) + 2(12.01) + 4(16)
= 90.036 g/mol
Molar mass of K2Cr2O7 = 2(39.10) + 2(52.01) + 7(16)
= 294.22 g/mol
Molar mass of K3[Cr (C2O4)3].3H2O = 3(39.10) + 52.01 + 6(12.01) + 6(12.01) + 12(16.00)
+ 12(16.00) + 6(1.008) + 3(16.00)
= 487.418 g/mol

No. of mole of H2C2O4 = mass (g)

molar mass (g/mol)
= 5.0020g
90.036 g/mol
= 0.056 mol

No. of mole of K2Cr2O7 = mass (g)

molar mass (g/mol)
= 1.8005g
294.22g
= 0.006 mol

From the equation:

3mol of H2C2O4 2mol of K3[Cr (C2O4)3].3H2O
0.056 x
x = 0.056 x 2
3
x = 0.0373mol of K3[Cr (C2O4)3].3H2O

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

0.006 x
x = 0.006 x 2
x = 0.012mol of K3[Cr (C2O4)3].3H2O

#The limiting reactant is K2Cr2O7

Mass of K3[Cr (C2O4)3].3H2O = 0.012mol x 487.418g/mol

= 5.8490g
Percentage yield =

actual yield

x 100%

theoretical yield
= 4.6215g
5.8490g
= 79.01 %

x 100%

Experiment 4
Chemical
Copper(II) sulphate pentahydrate
Potassium oxalate monohydrate

Theoretical yield of product (g)

Actual yield of product (g)
Percent yield of product (%)

Mass (g)
2.0064
6.2172

2.8305
1.1717
41.40%

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

Molar mass of CuSO4.5H2O = 63.54 + 32.07 + 4(16) + 5[2(1.008) + 16]
= 249.69g/mol
Molar mass of K2C2O4.H2O = 2(39.10) + 2(12.01) + 4(16) + 2(1.008) + 16
= 184.236g/mol
Molar mass of K2[Cu(C2O4)2(H2O)2] = 2(39.10) + 63.54 + 4(12.01) + 8(16) + 4(1.008)
+ 2(16)
= 353.812g/mol

No. of mole of CuSO4.5H2O =

Mass (g)
Molar mass (g/mol)
= 2.0046g
249.69g/mol
= 0.0080mol

No. of mole of K2C2O4.H2O = Mass (g)

Molar mass (g/mol)

= 6. 2172g
184.236g/mol
= 0.0337mol

From the equation:

1mol of CuSO4.5H2O 1mol of K2[Cu(C2O4)2(H2O)2]
0.0080mol x
x = 0.0080 mol of K2[Cu(C2O4)2(H2O)2]

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

0.0337mol x
x = 0.0337
2
x = 0.01685mol of K2[Cu(C2O4)2(H2O)2]
# The limiting reagent is CuSO4.5H2O

Mass of K2[Cu(C2O4)2(H2O)2] = 0.0080mol x 353.812g/mol

= 2.8305g

Percentage yield = Actual yield

x 100%

Theoretical yield
= 1.1717g
2.8305g
= 41.40 %

Experiment 5

x 100%

Chemical
Ferrous ammonium sulfate
Oxalic acid dihydrate
Solid potassium oxalate monohydrate

Theoretical yield of product (g)

Actual yield of product (g)
Percent yield of product (%)

Mass (g)
5.0236
2.5008
3.5080

6.2881
6.0800
96.69%

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

Fe3+ + 3OH- Fe(OH)3(s)
Overall chemical equation:
3K2C2O4 + 2Fe(OH)3(s) + 3H2C2O4 2K3[Fe(C2O4)3].3H2O + 3H2O

Molar mass of Fe(NH4)2(SO4)2.6H2O

= 55.85 + 2(14.01) + 8(1.008) + 2(32.07) + 8(16.00) + 12(1.008) + 6(16.00)
= 392.17g/mol
Molar mass of K2C2O4
= 2(39.10) + 2(12.01) + 4(16)
= 166.22g/mol
Molar mass of H2C2O4
= 2(1.008) + 2(12.01) + 4(16)
= 90.036g/mol

No. of mole of Fe(NH4)2(SO4)2.6H2O =

mass (g)
molar mass (g/mol)

= 5.0236g
392.17 g/mol
= 0.0128mol
No. of mole of Fe(NH4)2(SO4)2.6H2O = No. of mole of Fe(OH)3
#No. of mole of Fe(OH)3= 0.0128mol

No. of mole of K2C2O4 = mass (g)

molar mass (g/mol)
= 3.5080g
166.22g/mol
= 0.0211mol
No. of mole H2C2O4 = mass (g)
molar mass (g/mol)
= 2.5008g
90.036g/mol
= 0.0278mol

From equation:
2mol of Fe(OH)3 2mol of K3[Fe(C2O4)3].3H2O
0.0128mol x
x = 0.0128mol of K3[Fe(C2O4)3].3H2O
3mol of K2C2O4 2mol of K3[Fe(C2O4)3].3H2O
0.0211mol x

x = 0.0211 x 2
3
x = 0.0141mol of K3[Fe(C2O4)3].3H2O

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

0.0278mol x
x = 0.0278 x 2
3
x = 0.0185mol of K3[Fe(C2O4)3].3H2O
#The limiting reactant is Fe(OH)3

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

= 3(39.10) + 55.85 + 6(12.01) + 12(16) + 6(1.008) + 3(16)
= 491.258g/mol

Mass of K3[Fe(C2O4)3].3H2O
= 0.0128mol x 491.258g/mol
= 6.2881g

Percentage yield = actual yield

theoretical yield

x 100%

= 6.0800
6.2881
= 96.69%

x 100%

Discussion
Experiment 3
In this experiment, the coordination compound formed by the combination of Lewis acid
which is chromium(III),

3+

Cr

and Lewis bases or ligands (oxalate and water). As oxalic

acid dihydrate and potassium dichromate were mixed, the chromium ion was reduced (
6+

Cr

to

3+

Cr

by reduction process. In the same time, oxidation process occurred where

carbon dioxide gas was released. The two half equations are:
++Cr 2 O7
14 H

2-

+ 6 C2 O 4

3 C2 O 4

2-

2+ 6 e

2Cr

3-

+ 7 H2O

(reduction process)

6 CO2 + (oxidation process)

6e

In this step, orange colored mixture was formed with the evolution of carbon dioxide gases.
After 15 minutes of reaction, hot green-black liquid was formed.
As a result, the dark-green crystal of potassium tris(oxalate)chromium(III) trihydrate was
formed. The balanced equation is:
C
Cr .3 H 2 O

++ 2 K 3
++3 H 2 C 2 O 4 +6 K 2 C 2 O 4 . H 2 O+ K 2 Cr 2 O7 6 CO 2 +9 H 2 O+8 K
8H
As the mass of product was weighed, the actual yield is obtained. The theoretical yield is
calculated by using the number of moles of product from the limiting reactant. In this
experiment, the limiting reactant is potassium dichromate. The percentage yield is calculated
by using this formula:
Percentage yield=

Actual yield
100%
T h eoretical yield

The percent yield of the product obtained is 79.01% . It shows that there might some errors
while conducting this experiment as there is mass loss of the product as we compared to the
expected theoretical value. The errors will be discussed later.

Question
1. What is the oxidation state of chromium in

K 2 Cr 2 O7

and in the product?

K 2 Cr 2 O7 :

In

2 (+1 ) +2 x+ 7 (2 ) =0
2+2 x 14=0

2 x =12
x=+6

Oxidation state of chromium in

K 2 Cr 2 O7

is +6 .

In the product:
3 (+ 1 )+ x +3 (2 )+ 3 ( 0 )=0
+3+ x6=0

x3=0
x=+3

Oxidation state of chromium in the product is +3 .

2. Write two half-equations for each reaction involved in the preparation of the
complex using oxalic acid dehydrate,
dichromate,
st

1 half equation :

K 2 Cr 2 O7

K2C2O4. H2 O

and potassium

and a balanced equation for the overall reaction.

++Cr 2 O7
14 H

2-

+ 6 C2 O4

2+ 6 e

2Cr

3-

+ 7 H2O

2nd half equation :

3 C2 O 4

2-

6 CO2

+ 6 e

Overall equation:
C
Cr .3 H 2 O

++ 2 K 3

++3 H 2 C 2 O 4 +6 K 2 C 2 O 4 . H 2 O+ K 2 Cr 2 O7 6 CO 2 +9 H 2 O+8 K
8H

Experiment 4
Oxalic acid acts as bidentate ligand with many transition metal ions such as copper(II). In this
experiment, copper(II) functions as a Lewis acid while oxalate ion and water act as Lewis
bases (ligands) which bound to the metal ion thus forming a complex. The preparation of
copper(II) oxalate complex involved several steps. Firstly, copper(II) sulfate pentahydrate
was dissolved in water and heated. This is the source of copper(II) ions. In another flask,
potassium oxalate monohydrate was dissolved with water which is the source of oxalate ions
As both solution was mixed, copper(II) oxalate complex was formed. The full equation is:
C

O
CuSO 4 .5 H 2 O +
+ K 2 SO 4 +5 H 2 O
Cu

2 K 2 C 2 O4 . H 2 O K 2
As a result, blue salt of copper(II) oxalate complex was formed. After weighing, the actual
yield was obtained while the theoretical yield was determined from the calculation which
involves limiting reactant and the full equation. The limiting reactant in this experiment is

CuSO 4 .5 H 2 O

which produces the fewest number of moles of product. From the limiting

reactant, the theoretical yield was obtained. Then, the percentage yield was obtained which is
41.40%. This value is quite low which also showed that there must be some errors while
conducting this experiment.
Experiment 5
In this experiment, potassium tris(oxalato)ferrate(III) trihydrate was formed by conducting

two processes. Firstly, ferrous ammonium sulfate,

produced iron(II) oxalate,

NH

SO
. 6 H2O

Fe

NH

SO

was reacted with oxalic acid which

Fe

FeC 2 O 4 indicated by yellow precipitate. The equation is:

H2C2O4

FeC 2 O 4 (s ) +

H 2 SO 4 +

NH

+ 6 H 2 O(l)

By decantation, the iron oxalate was separated. During this step, heating helps to facilitate the
separation of yellow precipitate from other products. In the second process, potassium
tris(oxalato)ferrate(III) trihydrate was formed after addition of potassium oxalate, hydrogen
peroxide and oxalic acid.
Upon addition of potassium oxalate and hydrogen peroxide, oxidation of
has occurred. The equation involve is:
H 2 O+ HO 2

2+
+ 2 Fe

3++3 OH
2 Fe

2+
Fe

to

3+
Fe


Because of high concentration of OH

ions

Fe(OH )3 (brown precipitate) was formed.

The equation is:

Fe(OH )3 (s)

3++3 OH
Fe
After that, more oxalic acid was added which caused the brown precipitate to dissolve and the
soluble complex was formed. The full equation is:
C
Fe .3 H 2 O+ 3 H 2 O

3 K 2 C 2 O 4 + 3 Fe (OH )3(s )+3 H 2 C2 O 4 2 K 3

As a result after one week of crystallization, a bright green crystal was formed. From this, the
actual yield is obtained after weighing while theoretical yield is calculated from the equation.
The percentage yield obtained is 96.69% which is quite close to 100% yield. However, there
must be some errors while conducting this experiment which has caused the mass loss of the
product.
The errors that might have occurred during the preparation of the compounds in experiments
3, 4 and 5 were almost similar as all experiments involved similar steps such as weighing,
dissolving, heating and filtration. All results showed that the expected colored compound in
crystals form was obtained but these errors might affect on how much the mass of product
loss if compared to the expected theoretical mass. The errors were:
1. While transferring the salt, there might be some salt left in the weighing boat which
leads to inaccurate mass. This affect on the actual and theoretical yields obtained.
2. The compound was not completely dissolved in the solvent before mixing with other
solution because of improper stirring condition.
3. The weighing boat might be contaminated with other chemicals as it was not cleaned
and dried enough before weighing.
4. There was error while transferring the mixture into the Buchner funnel during suction
filtration. For example, the filter paper was not wet with a small amount of solvent
first before the mixture is transferred onto the filter paper. This may cause the mixture
passing under filter paper during filtration. Moreover, the mixture was not poured

carefully onto the very center of filter paper which may cause the sample to be under
the edges of filter paper.

During this experiment, there are several safety precautions needed such as:
1. While handling the hot glassware, use tongs to hold and white tile to place the
glassware after heating.
2. Do not use thermometer to stir the solution.
3. Pour acid into water, not water into acid.
4. Do not point the mouth of conical flask containing chemicals to others especially after
heating the chemicals.
5. Wear gloves as some chemicals such as concentrated acid is corrosive to skin.
6. Do not leave the glassware and hot plate unattended.
7. Use the glassware such as beaker and conical flask with Pyrex or Kimax labels for
heating.
In order to improve the accuracy of the result, there are several suggestions for this
experiment such as:
1. Instead of using the glass rod to stir, we can also use the magnetic stirrer to ensure
that all salts are completely dissolved in the solvent.
2. The apparatus such as conical flask and measuring cylinder can be calibrated with
distilled water followed by the solvent being used.

Conclusion
Coordination compound is formed between metal ion and ligands by coordinate covalent
bonding. The results in the form of crystal can be further analyzed by determine the
percentage yield which shows the ratio of actual yield and theoretical yield. In all
experiments, the colored crystal was formed which indicate that the reactions have occurred.
Meanwhile, experiment 5 shows the closest value to the theoretical yield with high
percentage yield if compared to experiment 3 and 4.

References
1. Hadariah Bahron, Kamariah Muda, Sharifah Rohaiza, Karimah Kassim. (2008).
Inorganic Chemistry: Experiments for Undergraduates. Kuala Lumpur: UiTM Press.
2. Experiment 2: Synthesis of Potassium tris(oxalato)ferrate(III) trihydrate. Retrieved
from: http://coursehero.com/file/5648535/Expt2-IronIIIOxalate/ on 29 Oct 2015
3. Exp

1:

Synthesis

of

an

Iron

coordination

www.chem.umass.edu/chem112/ on 29 Oct 2015

complex.

Retrieved

from: