CHM 474

INORGANIC CHEMISTRY

EXPERIMENT 3, 4, 5 :
SYNTHESIS OF POTASSIUM TRIS (OXALATO)
CHROMIUM(III) TRIHYRATE, COPPER(II) OXALATE
COMPLEXES, POTASSIUM TRIS (OXALATO) FERRATE(III)
TRIHYDRATE

NAME :

NUR SYAFIQAH BT CHE KAMARUDIN

ID : 2015247498
GROUP : AS2022M2
LAB PARTNER : AMIRAH FARZANA BT AZMAN
LECTURERS NAME : DR. AMALINA BT MOHD TAJUDDIN
DATE OF EXPERIMENT : 7 APRIL 2016

OBJECTIVES :
1. To synthesize the Potassium Tris (oxalato) Chromium(III) Trihydrate.
2. To prepare Copper(II) Oxalate complex
3. To synthesize Potassium Tris (oxalato) Ferrate(III) Trihydrate

INTRODUCTION :
Synthesis is a process where the substances are combined in order to form a new substances.
For this experiment, there are three synthesis of compound is being conducted. That is
synthesizing of the Potassium Tris(oxalato) Chromium(III) Trihydrate, Copper (II) Oxalate
Complex and Potassium Tris (oxalato) Ferrate(III) Trihydrate.
Firstly, for the potassium tris(oxalato) chromium(III) Trihydrate synthesis, basically a
chromium is one metal that have many oxidation numbers. Among all, chromium(III) is the
most suitable metal that have the most stable oxidation state forming the number of
complexes, whereas the six monodentate ligands will surround the cation in octahendral
shape. Based on the compound, two molecules of water with two anions of oxalate that
monitor the cation of chromium in order to drive oxygen atom at corner of octahedron. The
chemical equation for this synthesis :2 K2C2O4 . H2O + 7H2C2O4 + K2Cr2O4 2K2[Cr(C2O4)2] . 3H2O + 6CO2 + 3H2O
For experiment synthesising the copper(II) oxalate complex, this experiment are involving a
coordination compound. Theoretically, coordination compound is the product of a lewis acidbase reaction in which neutral molecules of anions was bonded to central metal. Ligands, a
type of lewis base in metal complexes, that range from monoatomic ions to complex ligands
in which it can bind the metal more than one metal in order to be in neutral or anionic. For
the oxalate complex, each oxalate ligand will create bond to the copper in which two oxygen
atom that donates a pair of electron to the copper. This is also known as coordinate covalent
bond where one atom donate both electrons.
CuSO4 .5H2O + 2 K2C2O4. H2O = K2[Cu(C2O4)2(H2O2)2] + 5 H2O + K2SO4
For experiment synthesis of potassium tris(oxalato) ferrate(III) Trihydrate, as it is a known as
a metal complex iron combined with the three oxalate ligands of C2O42- that are bonded to
every central atom. Each ligands are bonded to the metal atom in two different places, called
as bidentate. In this experiment, the compound was synthesised through the addition of oxalic
acid to form potassium oxalate based on the chemical equation :H2C2O4 + 2KOH K2C2O4 . 5H2O + H2O

Then, the ferrous ammonium sulphate was added with the potassium oxalate to form the
desired product, the potassium tris(oxalato) Ferrate (III) Trihdydrate where the product are in
the form of green crystal.
3K2C2O4 + 2Fe(OH)3 + 3H2C2O4 2K3[Fe(C2O4)3]. 3H2O + 3H2O
Overall for this three synthesising of experiment, the theoretical yield, actual yield as well as
the percentage yield of the product can be calculated throughout these experiment.
Theoretical yield is the amount of coordination compound product from a known mass of
reactant while the actual yield is the actual mass of the coordination compound synthesised.
The percentage yield can be calculated when both actual and theoretical value obtained and
the formula in order to calculate the percentage yield as shown :% yield =

act ual yield

x 100
theoretical yield

PROCEDURES :
A. Synthesize of Potassium (oxalate) Chromium(III) Trihydrate
1. A solution of 5.00g of oxalic acid in 10ml water was made in a conical flask.
2. 1g of potassium dichromate was added into the mixture in small portion and the
funnel was placed on the conical flask. The orange coloured mixture should
spontaneously was warmed up almost to boiling.
3. When reaction has subsided in 15 minutes, 2.10g of potassium oxalate monohydrate
was dissolved in the hot green-black liquid and was heated to boiling 5 minutes.
4. The viscous was then cooled to room temperature.
5. 10ml of 95% ethanol was added and the beaker was cooled further in ice with
frequent stirring.
6. After cooling for 15-30 minutes or when precipitation appear completed, the complex
was collected by suction filtration.
7. The crystal was washed with two 5ml 1:1 portion ethanol/water followed by 13ml of
95% ethanol.
8. The solid in a beaker was placed and allowed to dry in the oven.
9. The mass of the product was determined, and the percentage yield was calculated.
10. The sample was transferred to a labelled vial and kept for next experiment.
B. Synthesize of Copper(II) oxalate Complexes
1. 2.00g of copper(II) sulphate pentahydrate was weighed and was added to 30ml of
water in a small conical flask.
2. The mixture was slowly heated to the hot plate until the solids dissolved.
3. 6.20g of potassium oxalate monohydrate was weighed and added into a small conical
flask, dissolved with 30-40ml distilled water at room temperature.
4. By using funnel, the heated copper(II) sulphate was added to the potassium oxalate
solution, by swirled the flask slowly to mix.

5. The mixture was then chilled in ice bath for 30-60minutes. The blue crystals
precipitated after cooling process.
6. The complex was then collected by suction filtration and the crystal was washed twice
with 3ml portion of cold water.
7. The crystal was allowed to dry in the oven.
8. The percentage yield was determine and being transferred to a labelled vial. The
complex was kept for next experiment .
C. Synthesis of Potassium Tris(oxalato) Ferrate (III) Trihydrate
1. 5.00g of ferrous ammonium sulphate was dissolved in 20ml of water containing 1ml
of dilute sulphuric acid and being well stirred.
2. A solution of 2.50g of oxalic acid in 25ml of water was prepared.
3. The mixture was slowly heated to boiling and yellow precipitate was allowed to settle.
4. The supernatant was decant. 15ml of hot water was added to yellow precipitate and
stirred and the supernatant was decant.
5. 15ml of hot water was added to the precipitate.
6. 3.50 g of solid potassium oxalate monohydrate was added and was heated to
approximately 40oC .
7. While temperature at 40oC, 10ml of 6% H2O2 was added using dropper into it and
being stirred continuously.
8. Periodically, the temperature of solution was checked atleast 40oC during addition of
H2O2 .
9. The mixture was heated to boiling and a solution of 2.00g of oxalic acid dehydrate in
30ml of water portion was added along with 20ml initially until all has dissolved.
10. The clear solution was boiled, filtered through a Bunchner funnel with well flitting
paper.
11. 30ml of 95% ethanol was added slowly to the solution.
12. Any crystal was redissolve by heating and leave to crystallize.
Procedure B:The crystal was obtained using suction filtration. The crystal was washed with a
cooled 1:1 ethanol/ water mixture and with cooled acetone. Then the crystal was dried
and weighed. Then it was stored in a sample bottle/sample vial wrapped with foil and
kept for the next experiment.

DATA AND RESULTS :

Result for experiment 3 :Theoretical yield of K3[Cr(C2O3]3] . 3H2O
Mass of K3[Cr(C2O4)3] . 3H2O obtained
Percent Yield of K3[Cr(C2O4)3] . 3H2O

5.9954g
5.7217g
95.43%

Result for experiment 4 :Theoretical yield of K2[Cu(C2O4)2(H2O2)2]

Mass of K2[Cu(C2O4)2(H2O2)2] obtained
Percent Yield of K2[Cu(C2O4)2(H2O2)2]

2.8826g
2.7238g
94.49%

Result for experiment 5 :Theoretical yield of K3[Fe(C2O4)3]. 3H2O

Mass of K3[Fe(C2O4)3]. 3H2O obtained
Percent Yield of K3[Fe(C2O4)3]. 3H2O

6.2883g
2.4639g
39.18%

CALCULATIONS :
Experiment 3 :
2 K2C2O4 . H2O + 7H2C2O4 + K2Cr2O4 2K2[Cr(C2O4)2] . 3H2O + 6CO2 + 3H2O
a) To find the limiting reactant :Experimental mass of H2C2O4 = 5.0595g

5.0595 g H2C2O4 x

1 mol H 2 C 2 O4
90.04 g H 2 C 2 O4

MM = 90.04g

Cr ( C 2 O 4 2 ] .3 H 2 O

x
2mol K 2

Cr ( C 2 O 4 2 ] .3 H 2 O
= 0.0161 mol
K2
Experimental mass K2Cr2O7 = 1.8089g

MM = 294.22g

1.8089 g K2Cr2O7 x

1mol K 2 C r 2 O7
294.22 g K 2 C r 2 O7

Cr ( C 2 O 4 2 ] .3 H 2 O

x
2mol K 2

Cr ( C 2 O 4 2 ] .3 H 2 O
= 0.0123 mol
K2
The limiting reactant is K2Cr2O7
b) To find the theoretical yield

Cr ( C 2 O 4 2 ] .3 H 2 O
0.0123 mol
K2

= 5.9954g

Cr ( C 2 O 4 2 ] .3 H 2 O

Cr ( C 2 O 4 2 ] .3 H 2 O
x
1m ol K 2
487.43 g K 2

Cr ( C 2 O 4 2 ] .3 H 2 O
K2

c) To find the percentage yield

Actual : 5.7217g
Cr ( C 2 O 4 2 ] .3 H 2 O

Cr ( C 2 O 4 2 ] .3 H 2 O
Percentage yield =
5.9954 g K 2
5.7217 g K 2

x 100% = 95.43%

Experiment 4 :
CuSO4 . 5H2O + 2K2C2O4 . H2O K2[Cu(C2O4)2(H2O2)2] + K2SO4 + 5H2O
a) To find limiting reactant
Experimental mass CuSO4 . 5H2O = 2.0344g

1 mole CuS O4 .5 H 2 O
249.72 g CuSO 4 .5 H 2 O

2.0344 g CuSO4 . 5H2O x

C2 O4 2

Cu

x
1 mole K 2

C2 O4 2
Cu
= 0.008147mol
K 2

Experimental mass K2C2O4 . H2O = 6.2032g

6.2032 g K2C2O4 . H2O x

1mol K 2 C 2 O4 . H 2 O
184.218 g K 2 C 2 O 4 . H 2 O

C2 O4 2
Cu
= 0.0168 mol
mole K 2

The limiting reactant is CuSO4 . 5H2O

b) to find theoretical yield
C 2 O 4 2

C 2 O 4 2
C2 O4 2
Cu
Cu
0.008147 mol
x
1 mol K 2
K 2
Cu
353.82 g K 2

= 2.8826g
c) to find percentage yield
Actual yield : 2.7238g

C2 O4 2

Cu

x
1 mole K 2

C 2 O4 2

C 2 O4 2

Cu
% yield =
94.49%
2.8826 g K 2
Cu
2.7238 g K 2

Experiment 5 :
Fe(NH4) (SO4)2 . 6H2O + H2C2O4 FeC2O4 + H2SO4 + (NH4)2SO4 + 6H2O
Fe3+ + 3OH- Fe(OH)3
Overall chemical equation :
3K2C2O4 + 2Fe(OH)3 + 3H2C2O4 2K2[Fe(C2O4)3] . 3H2O + 3H2O
a) to find the limiting reactant of Fe(OH)3
iExperimental mass of Fe(NH4) (SO4)2 = 5.0109g
H
S O 4 2 .6 H 2 O
O

S O 4 2 .6 H 2 O
S O4 2 .6 H 2 O
3
5.0109g
X 392.21 g Fe ( N H 4 ) x

Fe ( N H 4 )
S O4 2 .6 H 2 O
1 mol Fe ( N H 4 )
1 mol Fe

= 0.0128 mol

H
O

Fe

Experimental mass of H2C2O4 = 2.5059g

2.5059 g H2C2O4 x

1 mol H 2 C 2 O4
90.04 g H 2 C 2 O4

H
O

x
3
1 mol Fe

= 0.02783 mol

H
O

Fe

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

ii- to find the limiting reactant of K2[Fe(C2O4)3] . 3H2O
mole of Fe(OH)3 = 0.0128 mol

0.0128 mol Fe(OH)3 x

OH 3
2 mol Fe
2 mol K 2 [ Fe ( C 2 O 4 ) 3 ] .3 H 2 O = 0.0128 mol

K 2 [ Fe ( C 2 O 4 )3 ] .3 H 2 O
Experimental mass of H2C2O4 = 2.0062g

2.0062g H2C2O4 x

1 mol H 2 C 2 O4
90.04 g H 2 C 2 O4

Fe ( C 2 O 4 2 ] .3 H 2 O

= 0.01485 mol
2 mol K 3

Fe ( C2 O 4 2 ] .3 H 2 O
K3
Experimental mass of K2C2O4 = 3.5018g

3.5018 g

K2C2O4 x

1mol K 2 C 2 O4
166.22 g K 2 C 2 O 4

Fe ( C2 O4 2 ] .3 H 2 O

= 0.0140 mol
2 mol K 3

Fe ( C2 O4 2 ] .3 H 2 O
K3
The limiting reactant is Fe(OH)3
c) To find theoretical yield
0.0128 mol

K 2 [ Fe ( C 2 O 4 )3 ] .3 H 2 O

K 2 [ Fe ( C 2 O 4 )3 ] .3 H 2 O

491.27 g K 2 [ Fe ( C 2 O 4 )3 ] .3 H 2 O
x

1 mol K 2 [ Fe ( C 2 O 4 )3 ] .3 H 2 O

= 6.2883g

d) To find percentage yield

Actual yield : 2.4639g
2.4639 g K 2 [ Fe ( C2 O4 )3 ] .3 H 2 O
Percentage yield =

6.2883 g K 2 [ Fe ( C2 O4 )3 ] .3 H 2 O

x 100 =39.18

DISCUSSION :
In experiment 3, the coordination compound that was formed when the lewis acid, Cr2+ was
react with the lewis base. Regarding to the reagent used, the lewis base are the H2O and C2O4.
Firstly , the solution of oxalic acid was mixed with the potassium dichromate causing the
potassium reacted in acidic solution and an orange colour of solution was formed. The orange
solution was filtered then. However, when the potassium oxalate monohydrate were added,
the dark green with precipitate solution formed and it used to be filtered. The dark green
crystal that was formed and collected was washed by cooled water along with acetone to
clean out the crystal and was dried before it was weighed. Based on result, the mass obtained
for the last product is 5.7217g. the theoretical yield of the product calculated is 5.9954 that is
near to the actual mass obtained. After both value of theoretical and actual yield obtained, the
percentage yield calculate for this product of potassium tris(oxalato) chromium(III)
Trihydrate obtained is about 95.43% that is almost accurate to near of 100% yield.
For experiment 4 synthesising of copper(II) oxalate complex, a transition metal like copper
tend to have more tendency to form a complex ion. Firstly, when the copper (II) sulphate
pentahydrate reacted with the potassium oxalate monohydrate, a coordination compound that
is copper(II) oxalate complex was formed. The heated copper(II) sulphate was mixed with the
potassium oxalate was cooled for a period of time resulting that a dark blue colour with
amount of precipitate was formed in the flask. After cooled, the solution was filtered by
suction filtration where the blue crystal was collected and was washed with cooled water.
After that, the crystal was dried and was weighed to obtain its mass. The mass of copper(II)
oxalate obtained during experiment is 2.7238g and the theoretical yield calculated is 2.8826g.
the percentage yield for the product formed is 94.49%.
Next, experiment of synthesising the potassium tri(oxalato) ferrate (III) trihydrate, the iron,
Fe act as a lewis acid that react with the lewis base, which is C2O4 and H2O that also known
as a ligands. As for lewis acid the Fe act as electron pair that will accept the electron while
the lewis base as electron pair donor. Firstly, ferrous ammonium sulphate was dissolved in
acidic solution that consist of dilute sulphuric acid added with solution of oxalic acid. Then

the solution was boiled until a yellow colour of precipitate formed. In this reaction involved
based on the chemical equation :Fe(NH4) (SO4)2 . 6H2O + H2C2O4 FeC2O4 + H2SO4 + (NH4)2SO4 + 6H2O
The solution was decanted and added with the potassium oxalate and heate until there was
brown precipitate formed. The observation showed indicated that the oxidation of ferrous ion
to ferric ion has occurred due to this chemical equation.
Fe3+ + 3OH- Fe(OH)3
The product then was addd with excess of oxalic acid until solution turned to pale green lime
solution. the same process was conducted where the solution undergo a suction filtration in
order to obtain the green crystal. The green crystal was washed and dried in the oven. The
result obtained where the mass of green crystal formed is 2.4639g, the theoretical yield is
6.2883g and the percentage yield obtained only 39.18% where the percent have the huge
different from 100%. Regarding to these experiments, there are some errors that contribute to
the inaccurate result obtained. There are some steps of precaution needs to be taken in order
to obtain accurate value and minimizing errors. Firstly all apparatus should be washed and
rinsed with distilled water in order to remove any foreign substance that might cause the
product to be contaminated. Next, during heating the solution the heating solution should be
heated in a constant heat level and in a short period to avoid bumping as bumping of solution
can cause a loss of the solution where the solution tend to splashed out of the container and
affect the results at the end of experiment. Next, during suction filtration process, the filter
paper are appropriately used by two pieces to avoid any leakage when filter the crystal of
product formed that can also causing to a loss of product.

CONCLUSION :
In conclusion , the coordination compound of the potassium(tris)oxalato chromium(III)
Trihydrate, copper (II) oxalate complex and the potassium tris (oxalato) ferrate (III) trihydrate
were synthesised. For the experiment 3, the actual yield obtained of oxalato chromium(III)
Trihydrate is 5.7217g and its theoretical yield value is 5.9954g compute to a percent yield of
95.43%. while experiment 4 of copper(II) oxalate complex, the theoretical yield obtained is
2.8826g and its actual is 2.7238g and the percentage yield is 94.49%. next, for experiment 5
synthesising the potassium tris (oxalato) ferrate (III) trihydrate give the value of theoretical
6.2838g and actual yield obtained is 2.4639g give the percentage yield of 39.18%.

REFERENCES :
1. Hadariah, B. Kamariah, M. Sharifah Rohaiza, S. (2015) Inorganic Chemistry
Experiments for Undergraduates Laboratory Manual, Experiment 1 and 2
Qualititative Analysis for Metal Cations, Penerbit Press Universiti Teknologi Mara.
2. Robert, J.L. (2002, November) Oxalates Complex of Chromium and Copper
retrieved from : http://wwwchem.uwimona.edu.jm/lab_manuals/c10expt15.html
3. Jespersen. N (2015). General Chemistry 7th Edition, Chapter 21 : Metal Complexes.
Wiley Publishing.
QUESTION :
1. K2Cr2O4 =
Cr in K2Cr2O4 =
2(1) + 2x + 7(-2) = 0
2x = 12
x = +6 , Cr = +6
Cr ( C 2 O 4 2 ] . 3 H 2 O
Cr in
K 2
3(1) + x +6(3) + 12(-2) +6(1) +3(-2) = 0
-3 + x = 0
x = +3

2. oxidation:

3C2O4 2- 6CO2 + 6e-

reduction: 14H+ + Cr2O7 2- + 6C2O4 2- + 6e- 2 Cr(C2O4 )3 3- + 7H2O

overall :
2K3[Cr(C2O4)3]3H2O + 6CO2 + H2O K2Cr2O7 + 7H2C2O4 + 2K2C2O4

JOTTER :