CHM 475: INORGANIC

CHEMISTRY
NO. OF EXPERIMENT
TITLE
NAME
STUDENT NUMBER
PARTNERS NAME
GROUP
LECTURERS NAME
LAB. INSTRUCTOR
DATE OF EXPERIMENT
DATE OF SUBMITION

6
Determination of the
Percentage of Ligands in
Coordination Compounds.
Nurul Iman Amani Bt Che Awang
2014179961
Muhamad Nurasyraf Bin Mohd
Razip
2014532595
ED247/4A
Dr Amalina Mohd Tajuddin
1st November 2016
8th November 20116

INTRODUCTION:
There are two sections of this experiment. Part A involves standardization of potassium
permanganate solution which will be used in part B of the experiment. Part B involves
determining the amount of oxalate content in coordination compound of Potassium
Tris(oxalato)chromium(III)

Trihydrate,

Copper(II)

Oxalate

and

Potassium

Tris(oxalato)ferrate(III) Trihydrate that we have prepared previously. The determination of

oxalate content in coordination compound is further calculated based on stoichiometry
principle.

OBJECTIVE:
The aim of this experiment is to determine the oxalate content in coordination compounds that
we have prepared in experiment 3, 4 and 5.
Apparatus
Conical flask
Weighing balance
Hot plate
Thermometer
Buret

Materials
50 mL of 1M Sulfuric acid
0.20 g of Na2C2O4
0.20 g of Potassium Tris(oxalato)chromium(III)
Trihydrate
0.20 g of Copper(II) Oxalate
0.20 g of Potassium Tris(oxalato)ferrate(III)
Trihydrate
Potassium permanganate solution

PROCEDURE:
A. Standardisation of potassium permanganate solution.
1. 0.20 g of dried Na2C2O4 was weighed and it was transferred into conical flask.
2. It was dissolved in 50 ml of 1 M H2SO4.
o
3. The solution was heated to 60 C.
4. The solution was titrated with KMnO 4 solution until the first persistent pink
colour appeared.
5. The volume of KMnO4 solution used or titrated was recorded in the table 6.1.
6. This process was repeated at least one more time utill a consistent values is
obtained.
B. Determination of the oxalate content in coordination compounds.
1. 0.20 g of the crystal Potassium Tris(oxalato)chromium(III) Trihydrate,
K3[Cr(C2O4)3].3H2O prepared previously was weighed and it was
placed in conical flask.
2. It was dissolved in 50 ml of 1 M H2SO4.
o
3. The solution was heated to 60 C.
4. It was titrated slowly with KMnO4 solution until slightly pink color appeared.
5. The volume of KMnO4 solution used was recorded in the table 6.2.
6. This process was repeated for one more time.
7. The

whole

steps

was

repeated

with

Copper(II)

Oxalate,

K2[Cu(C2O4)2(H2O)2] and Potassium Tris(oxalato)ferrate(III) Trihydrate,

K3[Fe(C2O4)3].3H2O.

8. RESULTS:
9.
10. Table 6.1: Standardisation of KMnO4 solution.
11.
12. Trial

13. I

14. II

15. Mass of Na2C2O4. (g)

16. 0.2100

17. 0.2097

18. Final volume in burette. (mL)

19. 13.70

20. 26.90

21. Initial volume in burette. (mL)

22. 0.00

23. 13.70

24. Volume of KMnO4 used. (mL)

25. 13.70

26. 13.20

27.
28.
29.
30.
31. Table 6.2a: determination of oxalate content in K3[Cr(C2O4)3].3H2O
32.
33. Trial
34. I

35. II

36. Mass of
K3[Cr(C2O4)3].3H2O. (g)
39. Final volume in burette. (mL)

37. 0.2048

38. 0.2054

40. 7.40

41. 7.40

42. Initial volume in burette. (mL)

43. 0.00

44. 15.80

45. Volume of KMnO4 used. (mL)

46. 7.40

47. 8.40

48. Table 6.2b: determination of oxalate content in K2[Cu(C2O4)2(H2O)2]

49.
50. Trial
51.
I
53. Mass of
K2[Cu(C2O4)2(H2O)2]. (g)
56. Final volume in burette. (mL)
59. Initial volume in burette. (mL)
62. Volume of KMnO4 used. (mL)
65.
66.

54. 0
.2015
57. 7
.80
60. 0
.00
63. 7
.80

67. Table 6.2c: determination of oxalate content in K3[Fe(C2O4)3].3H2O.

68.
69. Trial
70.
I
72. Mass of
K3[Fe(C2O4)3].3H2O. (g)
75. Final volume in burette. (mL)
78. Initial volume in burette. (mL)
81. Volume of KMnO4 used. (mL)

73. 0
.2053
76. 7
.60
79. 0
.00
82. 7
.60

52.
I
55.
.2088
58.
.80
61.
8.30
64.
0.50

71.
I
74.
.2066
77.
.60
80.
4.00
83.
.40

I
0
7
1
1

I
0
7
1
6

84. CALCULATION:
85.
86. Standardisation of KMnO4 solution.
87.
88. Trial 1

89.

90.

Number of moles of Na2C2O4

107.

Number of moles of Na2C2O4

91.

0.2100g Na2C2O4 x
mol Na2C2O4

108.

0.2054g Na2C2O4 x
mol Na2C2O4

92.

94.

-3

1.567 x10 mol Na2C2O4

111.

113.

-3

1.567 x10 mol Na2C2O4 x 2

mol KMnO4

-3

1.5328 x10 mol Na2C2O4 x 2

mol KMnO4
114.

5 mol
Na2C2O4
115.

98.

5 mol
Na2C2O4
99.

-4

101.

Concentration of KMnO4

102.

-3

1.5328 x10 mol Na2C2O4

112.
Number of moles of
KMnO4 solution

96. Number of moles of KMnO4

solution

100.

134 g Na2C2O4

110.

95.

97.

109.

134.0 g Na2C2O4

93.

123.

Trial 2

6.268 x 10 mol KMnO4

-4

116.

6.1312 x 10 mol KMnO4

117.

Concentration of KMnO4

118.

-4

6.1312 x 10 mol KMnO4

-4
6.268 x 10 mol KMnO4 119.

124.
0.04588 M + 0.04645 M

Average concentrate KMnO4 =

= 0.04617 M

125.

126.

127. Determination of oxalate content in K3[Cr(C2O4)3].3H2O

128.
129.
Trial 1
130.
131.

Number of moles of KMnO4

132.
0.04617 M x 0.0078 L =
-4
3.6013 x 10 mol
-

133.

Number of moles of MnO4

134.

3.6013 x 10 mol KMnO4 x 1

mol MnO4

-4

154.

Trial 2

Number of moles of KMnO4

155.
0.04617 M x 0.01050 L
-4
= 4.848 x 10 mol
-

156.

Number of moles of MnO4

157.

3.00 x 10 mol KMnO4 x 1

mol MnO4

-4

135.

158.

136.

1 mol
KMnO4

-4

159.
-

137.

= 3.6013 x 10 mol MnO4

138.

Number of moles of C2O4

139.

3.6013 x 10 mol MnO4

25 mol C2O4

2-

-4

-4

160.

= 3.00 x 10 mol MnO4

161.

Number of moles of C2O4

162.

3.00 x 10 mol MnO4

25 mol C2O4

2-

-4

140.

164.

MnO4
142.
143.

165.

166.

2-

Mass of oxalate
146.

147.
C2O4

-4 2-

-1

9.0033 x 10 mol
x 88.0 g mol

169.
C2O4
170.

2 mol
MnO4

2- -4

= 7.500 x 10 mol C2O4

167.

= 9.0033 x 10-4 mol C2O4

145.

Mass of oxalate
168.

-4

177.
25.98

2-

= 0.0660 g C2O4

Average percent of Oxalate = 38.69 +

= 32.34 %
178.

179. 2
Theoretical

180.

percentage oxalate in complex 3 x 88.0

-1

= 54.17 %
-1

181. 487.36 g molPercentage

182.

purity of complex.
183.
X 100 = 59.70 %

32.34

2-

7.500 x 10 mol
x 88.0 g mol

176.

g mol

163.

2 mol

141.

144.

1 mol
KMnO4

-1

188. Determination of oxalate content in K2[Cu(C2O4)2(H2O)2]

189.
190.
Trial 1
191.
192.

Number of moles of KMnO4

193.
0.075 M x 0.0078 L =
-4
5.85 x 10 mol

214.

Trial 2

Number of moles of KMnO4

215.
0.075 M x 0.0105 L =
-4
7.875 10 mol

194.

Number of moles of MnO4

195.

5.85 x 10 mol KMnO4 x 1

mol MnO4

-4

216.

Number of moles of MnO4

217.

7.875 x 10 mol KMnO4 x 1

mol MnO4

-4

196.

218.

197.

1 mol
KMnO4

-4

219.

198.

= 5.85 x 10 mol MnO4

199.

Number of moles of C2O4

200.

5.85 x 10 mol MnO4

25 mol C2O4

2-

-4

-4

= 7.875 x 10 mol MnO4

221.

Number of moles of C2O4

222.

7.875 x 10 mol MnO4

25 mol C2O4

2-

-4

224.

2- -3

225.

226.

Mass of oxalate

207.
C2O4
208.

2 mol
MnO4

= 1.4625 x 10 mol C2O4

205.

206.

223.

202.
203.

220.

201.

204.

1 mol
KMnO4

1.4625x 10 mol
x 88.0 g mol

-1

2-

= 0.1287 g C2O4

Mass of oxalate

229.
C2O4
230.

2- -3

= 1.9688 x 10 mol C2O4

227.
-3 2-

2 mol
MnO4

228.

-3 2-

2-

= 0.1733 g C2O4

236.
237.
73.35 %

Average amount of Oxalate =

238.

239. 2
Theoretical

240.

percentage oxalate in complex 2 x 88.0

g mol

-1

= 49.75 %
-1

241. 353.79 g molPercentage

242.

purity of complex. 73.35 %=

147.44 %

-1

1.9688 x 10 mol
x 88.0 g mol

63.87 + 83.00

244. Determination of oxalate content in K3[Fe(C2O4)3].3H2O.

245.
246.
Trial 1
247.
248.

Number of moles of KMnO4

269.

249.
0.0750 M x 0.0076 L =
-4
5.700 x 10 mol
Number of moles of MnO4

251.

5.700 x 10 mol KMnO4 x 1

mol MnO4

Number of moles of KMnO4

270.
0.0750 M x 0.0064 L =
-4
4.800 x 10 mol

250.

Trial 2

-4

271.

Number of moles of MnO4

272.

4.800 x 10 mol KMnO4 x 1

mol MnO4

-4

252.

273.

253.

1 mol
KMnO4

-4

274.

254.

= 5.700 x 10 mol MnO4

255.

Number of moles of C2O4

256.

5.700 x 10 mol MnO4

25 mol C2O4

2-

-4

-4

= 4.800 x 10 mol MnO4

276.

Number of moles of C2O4

277.

4.800 x 10 mol MnO4

25 mol C2O4

2-

-4

-3

279.
280.

2-

281.

2- -1

-3

284.
C2O4

1.425 x 10 mol
x 88.0 g mol
2-

= 0.1254 g C2O4

285.

2 mol
MnO4

2- -3

Mass of oxalate
283.

-3

2-

1.200 x 10 mol
x 88.0 g mol
2-

= 0.1056 g C2O4

291.
292.
51.11

Average amount of Oxalate = 61.08 +

= 56.10 %
293.

294. 2
Theoretical percentage of oxalate

295.

-1

296.

3 x 88.0 g mol

297.

298.

-1

491.21 g mol

299.

Percentage

purity of complex 56.10 %=

104.39 %

= 1.200 x 10 mol C2O4

282.

Mass of oxalate

262.
C2O4
263.

2 mol
MnO4

= 1.425 x 10 mol C2O4

261.

278.

258.

260.

275.

257.

259.

1 mol
KMnO4

= 53.74 %

-1

301. DISCUSSION:
302.
303. The experiment is conducted based on the principle of
standardization and redox titration method. The experiment is divided into
parts, part A and B; where each part discussed each principle.
304.

Standardization

process

is

defined

as

the

process

of

determining the exact concentration (molarity) of a solution. Titration is

one type of analytical procedure often used in standardization. In a
titration, an exact volume of one substance is reacted with a known
amount of another substance. The titration process is performed using
burette. The reactants called as titrant is hold by burette. It will be titrated
into a reaction vessel containing another reactant. The titrant is KMnO 4,
while Na2C2O4 solution will be in the reaction vessel.

The unbalanced

equation of the reaction is as follow:

305.
306.

MnO4- (aq) + C2O42- aq)

Mn2+ aq) + CO2 (g)

307.
308. Aqueous solution of permanganate ion is not stable over a long
period of time. Thus, the exact concentration of KMnO 4 must be
determined by titration with a known amount of odium oxalate, Na2C2O4.
309. In order to determine the oxalate content in the coordination
compound, first we have to determine the mass percent of oxalate ion in
the salt by titration with a standard KMnO 4.

The process is called

oxidation-reduction titration. The KMnO4 will oxidize all the oxalate to

carbon dioxide which escapes.

The oxalate is oxidized and the

permanganate is reduced.
310.
311. The reaction takes place in acidic medium (H 2SO4) as the
reaction required the dissociation of the reacting ion. Sulfuric acid is
added to sodium oxalate to produce H2C2O4, or oxalic acid plus sodium
chloride. The H2C2O4 oxalate in an acidic environment dissociates into C 2O4
plus two H+ ions. Potassium permanganate in an acidic environment
dissociates into the potassium or K + ions and permanganate or MnO4- ions.
The process is quite slow; therefore the salt compound is heated at 60-70
degree centigrade to speed up the reaction.
312.

313. The ion C2O42- and Mn2+ are colorless while the MnO4- has a deep
purple color. Until all the oxalate salt is consumed in the reaction, the
titrated solution will remain colorless. When the reaction is complete, the
solution will be a light pink color.
314.

315. Before reaching the endpoint, we will momentarily see a spot

of pink color, but it will disappear as you swirl. As more and more
persistent color occurs, we slowed down the addition of the titrant. This is
important to ensure we obtained a preliminary final volume reading and
did not overshoot with one more drop. The presence of excess unreacted
permanganate ion can be detected by the appearance of the first
consistent pink color (for about 30 seconds). This is considered as the
endpoint of titration. Endpoint or also called as equivalence point is the
point at which there will be equal number of moles of

KMnO 4

and

Na2C2O4 in the solution.

316.
317. At the completing of the reaction, the moles of KMnO4 which
are added from the burette can be determined from the grams of
Na2C2O4 by using the calculated moles of Na2C2O4, using the concept of
stoichiometry. The calculation will be shown in the result and analysis. The
balance equation of the reaction is as follow:
318.
319. 2 MnO4- + 5 H2C2O4 + 6 H

10 CO2 + 2 Mn2+ + 8 H2O

320.
321. The

results

we

collected

show

the

concentration

of

standardized KMnO4 solution was 0.04617 M. Then, we had determined

amount of oxalate ions in coordination compounds by titrating with
standardized KMnO4 solution. After calculation using stoichiometry
method from balanced half chemical equation, we know that the ratio of
the reaction in this experiment was 2 mol of MnO 4 reacted with 5 mol
C2O4

produce Mn2+,CO2 and water. The percentage of oxalate in

coordination compounds were 54.17 %% in K3[Cr(C2O4)3].3H2O, 49.75 %

in

K2[Cu(C2O4)2(H2O)2]

percentage

purity

of

and

53.74

complex

%in
for

K3[Fe(C2O4)3].3H2O.
K2[Cu(C2O4)2(H2O)2]

The
and

K3[Fe(C2O4)3].3H2O exceeded 100%. This may be due to uncomplete

drying of the complex. This will cause the increase of samples weigh due
to the presence of additional water. Another reason could be the presence
of

contaminants,

side-products,

conducting the experiment.

and/or

unreacted

reagent

during

322.
323.
324.
325.

326. Precaution
327.

There are some precautionary steps need to be

considered during the experiment. Safety goggles, aprons, and

gloves must be worn in lab at all times. This is because the
materials that are used need to be handled properly. Oxalate is
very toxic via oral and inhalation routes and severe kidney
damage is possible if oxalate salts are taken internally. Oxalate
compounds can be absorbed through the skin; gloves and
washing affected areas with cold water are required. 1 M
sulfuric acid is slightly corrosive. Wear gloves when handling
these compounds and wash any affected areas thoroughly
with cold water. KMnO4 is a very strong oxidizing agent and
must not be poured into the organic collection bottles.
328.

During the titration, KMnO4 must not be added or swirled

rapidly as it may result in brown coloration in your solution. This is due to the
formation of manganese (IV) oxide (MnO2). If you have not added any more
KMnO4 than needed to reach the endpoint, the excess oxalate should reduce
the MnO2 momentarily. However, if you fail to swirl the sample and overshoot
the endpoint while MnO2 is formed, the titration is ruined and must be
performed again. The apparatus especially burette must be rinsed
properly to ensure there is no contaminants present that will
affect our data. When you remove the thermometer to perform the
titration, be sure to rinse the thermometer into the flask since you do not want
to lose any of the sodium oxalate.
329.
330.

Errors

331.
error

There are some random, systematic and human

may

occurred

throughout

the

experiment.

During

transferring compounds from, some of it left in the weighing

boat, leading to inaccuracy of the compounds mass. In this
experiment, the limited time and little amount of apparatus
limit us to collect two readings of very consistent values.
332.

The compound may not completely dissolve in the

solvent before mixing with other solution because of improper

stirring condition. During the titration, the titrant or reactant in
the conical flask may contain some impurities that may cause

inaccuracy of the data.

333.

The apparatus such as conical flask and burette might be

contaminated with other chemicals as it was not cleaned and

dried enough before being used.
334.

335.

Future recommendations

336.
of

The random errors that are resulted from inaccuracy

measurements

can

be

reduced

by

taking

more

measurements with high consistent values and take the

average of the data. During transferring the compound from
the weighing boat, rinsing can be done to ensure the entire
compound is successfully transferred. 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.
337.

Lastly, It is useful to run what is called a blank for this titration since

the sulphuric acid solution may contain some impurities that would react with
the potassium permanganate and bring error to your data.
338.

To correct for this a blank containing only the

solvent must be titrated. The "corrected volume" is equal to

the volume of KMnO4 required to titrate oxalate ion in solvent
minus the volume required to titrate the solvent alone.
339.
340. CONCLUSION:
341.
342.

The conclusions were we had standardized the KMnO4 solution

by titrating against Na2C2O4. The concentration of KMnO4 solution was

0.04617 M. The oxalate content in each coordination compound is determined
by calculating theoretical percentage of oxalate and the percentage purity of
complex. the percentage of oxalate in coordination compounds were 54.17 %%
in K3[Cr(C2O4)3].3H2O, 49.75 % in K2[Cu(C2O4)2(H2O)2] and 53.74 %in
K3[Fe(C2O4)3].3H2O.

343.
344. ANSWERS FOR QUESTIONS:
345.
346.

1. 16 H

2MnO4 + 10e

2Mn

2+

8H2O

347.
5C2O4

348.

10CO2 +

10e

349.
+

16 H
+ 10CO2
351.

350.

2MnO4

5C2O4

2Mn

352.
2.

Based on the calculation:

353. Experimental Percentage oxalate in K3[Cr(C2O4)3].3H2O is
32.34 %% Experimental Percentage oxalate in K2[Cu(C2O4)2(H2O)2]
is , 73.35 % Experimental Percentage oxalate in K3[Fe(C2O4)3].3H2O
is 56.10 % Theoretical percentage in oxalate in K3[Cr(C2O4)3].3H2O
is 54.17 % Theoretical percentage in oxalate in K2[Cu(C2O4)2(H2O)2]
is 49.75 % Theoretical percentage in oxalate in K3[Fe(C2O4)3].3H2O
is 53.74 % Percentage purity of K3[Cr(C2O4)3].3H2O is 59.70 %
354. Percentage purity of K2[Cu(C2O4)2(H2O)2 is
147.44 % Percentage purity of K3[Fe(C2O4)3].3H2O is
104.39 %

2+

8H2O

355.
356.
357. REFERENCES:
358.
1. Hadariah Bahron, Kamariah Muda, Sharifah Rohaiza Syed Omar, Karimah
Kassim/2015/Inorgani Chemistry: Experiment for
Undergraduates/UiTM PRESS.
2.

Silberberg, Amateis/2015/Chemistry: The Molecular Nature of Matter and

th
Change 7 edition/Mc Graw Hill Education.
359.

3. Wasserman, R.,(2015). Does Sodium Oxalate

React With Potassium

Permanganate? Retrieved from
http://www.livestrong.com/article/286203-does- sodiumoxalate-react-with-potassium-permanganate/
360.
361.
362.
363.

364.