SEM OCTOBER 2020 - FEBRUARY 2021

LABORATORY REPORT
CHM361

ANALYSIS OF COORDINATION COMPOUND

K3[Fe(C2O4)3].3H2O

NAME : SITI MAIZATUL AKMA BINTI USLEY

STUDENT ID : 2018422676

GROUP : AS120 5J

CRITERIA FULL OBTAINED

Procedure 2%

Results / Data / Observation (Datasheet) 2%

Data Analysis / Justification / Validation 4%

Question 2%

Discussion 2%

Conclusion 1%

Format 2%

Data Sheet EXP 1 5%

Total 20%
ANALYSIS OF COORDINATION COMPOUND K 3 [Fe(C 2 O 4 ) 3 ].3H 2 O

OBJECTIVE

1. To synthesis a coordination compound, potassium tris (oxalato)ferrate(III) trihydrate under

carefully controlled conditions.
2. To standardize the potassium permanganate solution.
3. To determine the percentage of ligands in K3[Fe(C2O4)3].3H2O.

INTRODUCTION
Synthesis is a useful technique in all areas of chemistry. This technique is important because it is the
basis for developing new compounds, which may be useful for animals and vegetation. Most
developments in the pharmaceutical industry as well as the introduction of new and less harmful
pesticides are made possible because the chemicals involved are synthesised and tested in the
laboratory. In addition, many chemical compounds used in everyday life are synthesised from simpler
materials. This experiment involves preparing a substance by reacting known quantities of chemicals.
The expected product is potassium tris(oxalato)ferrate(III) trihydrate, K3[Fe(C2O4)3]·3H2O.

Standardization of potassium permanganate (KMnO4) solution is carried out by titration against a

standard solution of oxalic acid. Oxalic acid is a good primary standard because the compound is
available in solid form, as H2C2O4.2H2O, which can be prepared to a very high degree of purity and
is not hygroscopic nor efflorescent.

PROCEDURES

PART A: SYNTHESIS OF COMPOUND

1. 5 g ferrous ammonium sulphate salt weighed. The actual weight used recorded. It was
put into a 125 ml Erlenmeyer flask. This compound dissolved with 15 ml of distilled water
and 5 drops of 3M sulphuric acid added.
2. 50 ml of 0.5 M oxalic acid added to that solution and it heated to boiling, stirring
constantly to prevent bumping.
3. The Erlenmeyer flask removed from the heat and the yellow precipitate of FeC 2O4 allowed
to settle. The supernatant liquid decant and the precipitate washed by using 20 ml of hot
distilled water. The mixture swirled and the precipitate allowed to settle; decant and
repeat the washing once more.
4. 20 ml of 1M K2C2O4 added to the precipitate, stirred and heated to 40◦C. When the
temperature at 40◦C, 10 ml of 6% H2O2 dropwise added and stirred continuously.
5. The resulting solution heat to boiling. 20 ml of 0.5 M HCO4 added all at once while
maintaining the temperature near boiling.
6. Then swirled constantly, 15 ml of ethanol added slowly to the solution. Allowed to cool in
an ice bath prepared in a 400 ml beaker. The bottom portion of the flask immersed in the
ice bath and the solution stirred slowly until crystal begin to form.
7. The vacuum filtration apparatus prepared.
8. The supernatant liquid decanted away from the green crystals. The crystal transferred to
the Bucher funnel with the aid of clean glass rod and suction applied for about 20
minutes.
9. The suction stopped and 10 ml of the 1: 1 ethanol/water solution added. Then suction
applied for 2 minutes after waited for 30 seconds.
10. The crystals transferred to a preweighed labelled dry 50 ml beaker. The wash solution
discarded.

PART B: DETERMINE PERCENTAGE OF LIGAND

SECTION I: STANDARDIZATION OF KMnO4

1. A burette filled with the KMnO4 solution to be standardized.

2. 20 ml of the standard oxalic acid solution pipetted into a 250 ml conical flask and 20
ml of 2 M H2SO4.
3. The conical flask warmed about 80◦C and the permanganate solution titrated against
the oxalic acid solution. The KMnO4 solution added slowly or manganese (IV) reached
when the addition of one drop permanganate solution produced a permanent pink
colour. The results recorded in a table.
4. The titration repeated until consistent results are obtained.

SECTION II: DETERMINE PERCENTAGE OF LIGAND

1. Weighed 0.20 g of the coordination compound that was previously prepared.

2. The sample boiled with 50 ml of 1M sulphuric acid in a conical flask.
3. The solution allowed to cool to 60◦C and titrated lowly with the KMnO4 solution provided.
4. The end point reached when the addition of one drop of permanganate solution produced a
permanent pink colour. The results recorded in a table.
5. The titration repeated until consistent results obtained.

RESULTS

Synthesis of Potassium tris(oxalato)ferrate(III) trihydrate

1. Mass of Fe(NH4)2(SO4)2.6H2O used = 5.0264 g
2. Moles of Fe(NH4)2(SO4)2.6H2O used = 0.0128 mol
3. Mass of K3[Fe(C2O4)3].3H2O obtained = 5.2208 g
4. Theoretical yield of K3[Fe(C2O4)3].3H2O (moles) = 0.0128 g

5. Theoretical yield of K3[Fe(C2O4)3].3H2O (mass) = 6.288 g

6. Percent yield of K 3[Fe(C2O4)3].3H2O = 83.03%

Standardization of Potassium Permanganate Solution

Rough Accurate titrations
estimation 1 2
Final burette reading (mL) 19.00 18.55 38.45
Initial burette reading (mL) 0.00 0.00 20.00
Vol. of KMnO4 used (mL) 19.00 18.55 18.45
Mean vol. of KMnO4 used (mL) 18.5

Determination of the Percentage of Ligands in K 3[Fe(C2O4)3].3H2O

Rough Accurate titrations
estimation 1 2
Mass of K3[Fe(C2O4)3].3H2O (g) 0.2012 0.2004 0.2002
Final burette reading (mL) 23.20 22.50 32.20
Initial burette reading (mL) 0.00 0.00 10.00
Vol. of KMnO4 used (mL) 23.20 22.50 22.20
Mean vol. of KMnO4 used (mL) 22.35

DATA ANALYSIS/CALCULATIONS

Synthesis of Potassium tris(oxalato)ferrate(III) trihydrate

Moles of Fe(NH4)2(SO4)2.6H2O used = 0.0128 mol
Number of moles = mass of substance/atomic mass
= 5.0264/392.13
= 0.0128 g
Theoretical yield of K3[Fe(C2O4)3].3H2O (moles) = 0.0128 g
Theoretical yield of K3[Fe(C2O4)3].3H2O (mass) = 6.288 g
0.0128 = mass of substance/molecular mass
= mass of substance/491.24
Mass of substance = 0.0128 x 491.25
= 6.288 g
Percent yield of K 3[Fe(C2O4)3].3H2O = 83.03%
% of yield = (actual mass/theoretical mass) x 100
= 5.2208/6.288 x 100
= 83.03 %

DISCUSSION

Synthesis of Potassium Tris(oxalato)ferrate(III) Trihydrate (K3[Fe(C2O4)3].3H2O)

The colourless solution was turn to pale green solution. The product was obtained by suction
filtration process which is the solution was washed with 15 ml ethanol slowly and leave the solution
to recrystallize. After that the green crystal is filtered and washed with 1:1 ethanol, and cooled in an
ice bath prepared in 400 ml. The mass of green crystal obtained is 5.2208 g, the theoretical yield is
6.2888 g and the percentage yield is 83.03 %.

There is some precaution that we should practices while doing an experiment is we need to clean all
the apparatus that we used for example conical flask. This is important because there may have
other substances left in the flask and this can cause our product is contaminated so we do not get
the result. Next, while we are heat the solution of ferrous ammonium sulphate and solution of oxalic
acid dehydrate we need to slow the hot plate to avoid the bumping of the solution. While we are
doing an experiment there occur bumping of the solution, some of the solution was bumped to
outside of the conical flask. The mass loss due to the bumping, so there is large different between
15.55% to100%.

Determination of the Percentage of Ligands in K3[Fe(C2O4)3].3H2O

This experiment is a redox titration where potassium permanganate (KMnO4) is the titrant
and oxalic acid is the analyte. Also, KMnO4 is the oxidizing agent and oxalic acid is the reducing
agent. The reaction between KMnO4 and oxalic acid is carried out in an acidic medium because
permanganate ion in the acidic medium is a very strong oxidizing agent. Acidity is introduced by
adding dil. H2SO4. No indicators are used to determine the endpoint, because KMnO4 is a self-
indicator. Permanganate (MnO4-) ion has a dark purple colour. In an acidic medium, MnO4- is
reduced to colorless manganese (Mn2+) ions. On reaching the end point, the addition of the last
single drop of permanganate imparts a light pink colour to the solution.
Questions

SECTION I: STANDARDIZATION OF KMnO4

1. From the average volume of KMnO4 solution used, calculate the concentration of
the solution.

a1M1V1 = a2M2V2
KMnO4 = oxalic acid
5(M)(18.5) = 2(0.02)(300)
M = 0.13 M

2. Why is it necessary to heat the oxalic acid solution?

All reactions during the titration needs activation energy. The preheating up during the titration
will provide the enough kinetic energy. The heated mixture can have the higher frequency of collision
among the particles. The heating about 80°C keeps oxalic acid in decomposed state to facilitate better
interaction between oxalate and potassium permanganate because the reaction between oxalic acid
and potassium permanganate in acidic medium is extremely slow at normal temperature.

3. In this experiment oxalic acid is used as a reducing agent. Could oxalic acid be
used as a primary standard to standardise a solution of a base, such as sodium
hydroxide? Explain your answer.

Yes. Oxalic acid can be as a primary because have the advantage that they can
be weighed (the analytical balance is normally the most accurate instrument in the laboratory)
and they are stable under laboratory conditions.

SECTION II: DETERMINE PERCENTAGE OF LIGAND

1. Given that MnO4− ion is being reduced to Mn2+ ion, and C2O4 2− ion is being oxidised to CO2,
write a balanced redox equation for the above titration. Use the equation to calculate the
concentration of the oxalate ions in the coordination compound.
Oxidation numbers:

MnO4- Mn + 4(-2) = -1  Mn = +7

H2C2O4 O=C – C=O  C = +3

I I
OH OH

CO2 C + 2(-2) = 0  C = +4

Balancing redox equations – Half Equations

+7 +2
MnO4-  Mn2+ REDUCTION

+3 +4
H2C2O4  2CO2 OXIDATION

Balance the charges by adding electrons

+7 +2
REDUCTION: MnO4- + 5e-  Mn2+

2(+3) 2(+4)
OXIDATION: H2C2O4  2CO2 + 2e-

Balance the hydrogens by adding H+

+7 +2
REDUCTION: MnO4- + 5e- + 8H+  Mn2+

2(+3) (+4)
OXIDATION: H2C2O4  2CO2 + 2e- + 2H+

Balance H by adding H2O

REDUCTION: MnO4- + 5e- + 8H+  Mn2+ + 4H2O } X2

OXIDATION: H2C2O4  2CO2 + 2e- + 2H+ } X5

REDUCTION: 2MnO4- + 10e- + 16H+  2Mn2+ + 8H2O

OXIDATION: 5H2C2O4  10CO2 + 10e- + 10H+

REDOX: 2MnO4- + 5H2C2O4 + 6H+  2Mn2+ + 10CO2 + 8H2O

CONCENTRATION OF KMnO4

Number of moles of KMnO4

0.02 M x 0.022 L = 4.4 x 10-4 mol

Number of moles of MnO4-

4.4 x 10-4 mol KMnO4 x 2 mol MnO4-

-------------------
1 mol KMnO4

= 8.8 X 10-4 mol MnO4-

Number of moles of C2O4

8.8 X 10-4 mol MnO4- x 5 mol H2C2O4

-------------------
2 mol MnO4-

= 2.2 x 10-3 mol C2O4

Concentration of C2O4

= 2.2 x 10-3 mol C2O4

-----------------------------------
0.02 L

= 0.11 M
2. Calculate the percentage by weight of oxalate ions in the complex. Compare this with the
theoretical value and thus obtain the percentage purity of the complex.

Trial 1 Trial 2
Number of moles of KMnO4 Number of moles of KMnO4

0.02 M x 0.0225 L = 4.5 x 10-4 mol 0.02 M x 0.0222 L = 4.44 x 10-4 mol

Number of moles of MnO4- Number of moles of MnO4-

4.5 x 10-4 mol KMnO4 x 2 mol MnO4- 4.44 x 10-4 mol KMnO4 x 2 mol MnO4-
------------------- -------------------
1 mol KMnO4 1 mol KMnO4

= 9.0 x 10-4 mol MnO4- = 8.88 x 10-4 mol MnO4-

Number of moles of C2O4 Number of moles of C2O4

5.85 x 10-3 mol MnO4- x 5 mol H2C2O4 8.88 x 10-3 mol MnO4- x 5 mol H2C2O4
------------------- -------------------
2 mol MnO4- 2 mol MnO4-

= 2.25 x 10 -3 mol C2O4 = 2.22 x 10 -3 mol C2O4

Mass of oxalate Mass of oxalate

2.25 x 10 -3 mol C2O4 x 88.0 g/mol 2.22 x 10 -3 mol C2O4 x 88.0 g/mol
= 0.198 g C2O4 = 0.195 g C2O4

Percent of oxalate Percent of oxalate

0.198 g C2O4 x 100 0.195 g C2O4 x 100
------------------ ------------------
0.2004 g 0.2002 g

= 98.8% = 97.4 %

Average amount of Oxalate = 98.8 + 97.4 = 98.1 %

---------------
2

Theoretical percentage of oxalate

3 x 88.0 g mol-1
---------------------- = 53.74 %
491.21 g mol-1

Percentage purity of complex

98.1 % = 1.83%
------------
53.74 %
CONCLUSION

Synthesis of Potassium Tris(oxalato)ferrate(III) Trihydrate (K3[Fe(C2O4)3].3H2O)

Potassium tris(oxalato)Ferrate(III)Trihydrate , (K3[Fe(C2O4)3].3H2O) was synthesize. The actual

mass obtained 5.2208 g was while the theoretical yield obtained was. So 6.288 g the theoretical yield
is 83.03 %.

Determination of the Percentage of Ligands in K3[Fe(C2O4)3].3H2O

From the above experiment it is evident that potassium permanganate can be effectively
standardized by using oxalic acid. The concentration of oxalate solution was 0.11 M. The oxalate
content in coordination compound is determined by calculating theoretical percentage of oxalate and
the percentage purity of complex. The percentage of oxalate in coordination compounds 53.74 % in
K3[Fe(C2O4)3].3H2O.

REFERENCES

1. amrita.olabs.edu.in,. (2013). Determination of concentration of KMnO₄ solution. Retrieved 20

December 2020, from http://amrita.olabs.edu.in/?brch=8&cnt=1&sim=115&sub=73
2. R. W. Coltman. The Determination of Manganese. Industrial & Engineering Chemistry 1924,
16 (6) , 606-609. https://doi.org/10.1021/ie50174a028
3. Kasture AV, Wadodkar SG, Gokhale SB, Practical Pahrmaceutical Chemistry-I. Nirali
Prakashan; 1993;53.
DATA SHEET

EXPERIMENT 1

Predicting Molecular Shape and Polarity Using VSEPR Theory

Name : SITI MAIZATUL AKMA BINTI USLEY

Student ID : 2018422676
Date of Experiment :

RESULTS

Table 1: Molecular shape and polarity prediction using VSEPR theory

Formula Sketch Lewis Number of Number of Electronic Sketch Molecular geometry and bond Molecular
structure bonding pair lone pair geometry angles polarity
CS2 2 0 linear nonpolar

PF3 3 1 tetrahedral polar

Formula Sketch Lewis structure Number of Number of Electronic Sketch Molecular geometry and Molecular
bonding pair lone pair geometry bond angles polarity

3 0 Trigonal planar nonpolar

SO3

4 0 Tetrahedral
SiCl4 nonpolar
4 2 octahedral
ICl4-

polar

AsF5 5 0 Trigonal nonpolar

Bipyramidal

Formula Sketch Lewis structure Number of Number of Electronic Sketch Molecular geometry and Molecular
bonding pair lone pair geometry bond angles polarity
5 1 octahedral
TeF5-
polar

SCl2 2 2 tetrahedral polar

IOF5 6 0 octahedral nonpolar

IF4+ 4 1 Trigonal polar

Bipyramidal