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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
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,
8. RESULTS:
9.
10. Table 6.1: Standardisation of KMnO4 solution.
11.
12. Trial
13. I
14. II
16. 0.2100
17. 0.2097
19. 13.70
20. 26.90
22. 0.00
23. 13.70
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
43. 0.00
44. 15.80
46. 7.40
47. 8.40
54. 0
.2015
57. 7
.80
60. 0
.00
63. 7
.80
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.
107.
91.
0.2100g Na2C2O4 x
mol Na2C2O4
108.
0.2054g Na2C2O4 x
mol Na2C2O4
92.
94.
-3
111.
113.
-3
-3
5 mol
Na2C2O4
115.
98.
5 mol
Na2C2O4
99.
-4
101.
Concentration of KMnO4
102.
-3
112.
Number of moles of
KMnO4 solution
100.
134 g Na2C2O4
110.
95.
97.
109.
134.0 g Na2C2O4
93.
123.
Trial 2
-4
116.
117.
Concentration of KMnO4
118.
-4
-4
6.268 x 10 mol KMnO4 119.
124.
0.04588 M + 0.04645 M
125.
126.
132.
0.04617 M x 0.0078 L =
-4
3.6013 x 10 mol
-
133.
134.
-4
154.
Trial 2
155.
0.04617 M x 0.01050 L
-4
= 4.848 x 10 mol
-
156.
157.
-4
135.
158.
136.
1 mol
KMnO4
-4
159.
-
137.
138.
139.
2-
-4
-4
160.
161.
162.
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
167.
145.
Mass of oxalate
168.
-4
177.
25.98
2-
= 0.0660 g C2O4
179. 2
Theoretical
180.
= 54.17 %
-1
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
193.
0.075 M x 0.0078 L =
-4
5.85 x 10 mol
214.
Trial 2
215.
0.075 M x 0.0105 L =
-4
7.875 10 mol
194.
195.
-4
216.
217.
-4
196.
218.
197.
1 mol
KMnO4
-4
219.
198.
199.
200.
2-
-4
-4
221.
222.
2-
-4
224.
2- -3
225.
226.
Mass of oxalate
207.
C2O4
208.
2 mol
MnO4
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
227.
-3 2-
2 mol
MnO4
228.
-3 2-
2-
= 0.1733 g C2O4
236.
237.
73.35 %
239. 2
Theoretical
240.
-1
= 49.75 %
-1
-1
1.9688 x 10 mol
x 88.0 g mol
63.87 + 83.00
269.
249.
0.0750 M x 0.0076 L =
-4
5.700 x 10 mol
Number of moles of MnO4
251.
270.
0.0750 M x 0.0064 L =
-4
4.800 x 10 mol
250.
Trial 2
-4
271.
272.
-4
252.
273.
253.
1 mol
KMnO4
-4
274.
254.
255.
256.
2-
-4
-4
276.
277.
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
294. 2
Theoretical percentage of oxalate
295.
-1
296.
3 x 88.0 g mol
297.
298.
-1
491.21 g mol
299.
Percentage
282.
Mass of oxalate
262.
C2O4
263.
2 mol
MnO4
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
The unbalanced
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.
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.
KMnO 4
and
320.
321. The
results
we
collected
show
the
concentration
of
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
contaminants,
side-products,
and/or
unreacted
reagent
during
322.
323.
324.
325.
326. Precaution
327.
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
occurred
throughout
the
experiment.
During
335.
Future recommendations
336.
of
can
be
reduced
by
taking
more
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.
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.
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.
364.