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NO. OF EXPERIMENT
TITLE
NAME
STUDENT NUMBER
PARTNERS NAME
STUDENT NUMBER
GROUP
LECTURERS NAME
LAB. INSTRUCTOR
DATE OF EXPERIMENT
DATE OF SUBMITION
3, 4 & 5
Synthesis of potassium
tris(oxalate)chromium(III) trihydrate,
copper(II) oxalate complex and
potassium tris(oxalate)ferrate(III)
trihydrate.
Nurul Iman Amani Bt Che Awang
2014179961
Muhamad Nurasyraf Bin Mohd Razip
2014532595
ED247/4A
Dr Amalina Mohd Tajuddin
Nurul Izza Taib
11th &18th October 2016
1st November 2015
CHEMISTRY
INTRODUCTION:
Synthesis is process in which substances combine to form completely
new substances .In this experiment we are synthesizing coordination
compound. Coordination compound is the product of a Lewis acid-base
reaction in which neutral molecules or anions bond to central metal by
coordinate covalent bonds. A coordinate covalent bond is a covalent bond
in which one atom supplies both electrons.
Transition metals have many special properties. One of them is
varieties in their color. This is due to the concept of crystal field theory
between the ligands that will result in separation of energy called as crystal
field splitting.
The amount of product that can be calculated based on the
stoichiometric reaction of product to the limiting reagent is called the
theoretical yield .While the actual yield of the compound can be calculated
by weighing the last product of each experiment. The ratio of these
theoretical yield and actual yield can be used to determine the percent yield
of the reaction. Thus, by determining the percent yield, we can determine
the rate of effiency of each reaction.
OBJECTIVE:
tris(oxalate)chromium(III)
trihydrate,
and
potassium
tris(oxalate)ferrate(III)
K3[Fe(C2O4)3].3H2O.
2. To determine the percentage yield of each compound.
trihydrate,
Materials
5 g of oxalic acid
10 mL of distilled water
1.8 g of potassium dichromate
2.10
g
potassium
oxalate
monohydrate
95% ethanol
Experiment 4
Apparatus and equipment
Conical flask
Funnel
Beaker
Ice water bath
Buchner funnel
Oven
Weighing balance
Measuring cylinder
Hot plate
Glass plate
Materials
2 g copper(II) sulphate pentahydrate
Distilled water
6.20
g
potassium
oxalate
monohydrate
3 mL cold water
Experiment 5
Apparatus and equipment
Conical flask
Funnel
Beaker
Ice water bath
Buchner funnel
Oven
Weighing balance
Measuring cylinder
Hot plate
Glass plate
Glass rod
Test tube
Filter paper
Thermometer
Dropper
Materials
5 g ferrous ammonium sulfate
Distilled water
Dilute sulfuric acid
2.50 g oxalic acid dehydrate
3.50 g solid potassium oxalate
monohydrate
10 mL of 6% H2O2
2 g oxalic acid dihydrate
95% ethanol
METHOD:
Experiment 3
Experiment 4
1. 2.00 g copper(II) sulphate pentahydrate, (CuSO4 .5H2O) was weighed
and it was added into conical flask containing 30 ml of distilled
water. The flask was heated slowly on a hot plate until the solid
dissolved.
2. 6.20 g of potassium oxalate monohydrate, K 2 C2 O4. H2O was
dissolved in another flask containing 30 ml of distilled water at
room temperature.
3. The heated CuSO4 solution was added using a funnel, into the
flask containing potassium oxalate monohydrate slowly. The
flask was swirled slowly to allow mixing of the compound.
4. The mixture was cooled in an ice bath for 40 minutes. Blue crystals
formation were observed.
5. The complex was collected by suction filtration and the crystal were
washed with 3mL portions of cold water.
6. The crystals were placed on the watch glass and it was allowed to
dry in the oven.
7. The mass of the synthesis crystals and percentage yield were
determined.
8. The crystals were transferred into a labelled plastic packet. It was
kept for next experiment.
Experiment 5
Procedure A
1. 5.00 g of ferrous ammonium sulphate was dissolved in
20 ml distilled water containing 1 ml of diluted sulphuric
acid in the beaker.
2. 2.50 g of oxalate acid dihydrate was dissolved in 25 ml of
distilled water in another beaker. Then it was added into the
first beaker containing ferrous ammonium sulphate.
3. The mixture was heated slowly until boiling and the yellow
precipitateis
allowed
to
settle.
The
supernatant
was
Procedure B
1. The crystals were collected by suction filtration. The beaker
was rinsed with 10 ml of 1:1 ethanol/distilled water crystals
and with cooled acetone.
2. The crystals were placed on the watch glass and it was allowed
to dry in oven.
3. The mass of the synthesis crystals and percentage yield were
determined.
4. The crystals were transferred into a plastic packet. It was kept
for the next experiment
5. RESULTS:
6.
7. Experiment 3: mass of K2[Cr(C2O4)3].3H2O
8.
9. Mass of watch glass and filter paper
11.
Mass of watch glass and filter
paper + crystals
13.
Mass of crystals
21.
15.
Theoretical yield
17.
Percent yield
10.
35.
6137 g
12.
40.
0201 g
14.
4.4064g
16.
6.
1017 g
18.
79.2
%
19.
20.
Experiment 4: mass of K2[Cu(C2O4)2.(H2O)2
22.
23.
Mass of watch glass and filter
paper
25.
Mass of watch glass and filter
paper + crystals
27.
Mass of crystals
29.
Theoretical yield
31.
Percent yield
24.
38.
1022 g
26.
40.
0800 g
28.
1.9
778 g
30.
2.8
666 g
32.
68.99%
33.
34.
35.
Experiment 5: mass of K3[Fe(C2O4)3].3H2O
36.
37.
Mass of watch glass and filter
paper
39.
Mass of watch glass and filter
paper + crystals
41.
Mass of crystals
38.
37.9500 g
40.
32.7600 g
42.
5.1900 g
43.
Theoretical yield
44.
6.2851 g
45.
Percent yield
46.
82.5 %
47. CALCULATION:
48.
49. Experiment 3:
50.
51.
3H2O
52.
53.
90.036
54.
55. Theoretical mass of H2C2O4
56.
57.
5.0841 g H2C2O4
mol K3[Cr(C2O4)3. 3H2O
1 mol H2C2O4
58.
90.036 g H2C2O4
59.
mol H2C2O4
60.
61. =
0.01613 mol K3 [Cr (C2O4)3. H2O
62.
63.
Molar mass of K2Cr2O7
64.
65. 294.22
66.
1.8419 g K2Cr2O7
mol K3[Cr(C2O4)3. 3H2O
1 mol K2Cr2O7
294.2 g K2Cr2O7
1 mol 2K2C2O4.H2O
67.
68.
mol K2Cr2O7
69.
70.
71.
184.04
72.
2.1012 g K2C2O4.H2O
x
2 mol K3 [Cr (C2O4)3. 3H2O
73.
2K2C2O4.H2O
74.
75.
184.04
g
2 mol 2K2C2O4.H2O
76.
77.
78.
79.
80.
81.
487.36
K3[Cr(C2O4)3].3 H2O
82. 1 mol K3 [Cr (C2O4)3. 3H2O
83.
84.
85.
86. Percent yield of K3[Cr(C2O4)3. 3H2O
87.
88.
4.
4064 g
93.
X 100
89.
90.
6.
1017 g
91.
92. =
72.2 %
94. Experiment 4:
95.
96.
CuSO4.5H2O +2K2C2O4.H2O
(C2O4)2(H2O)2] +
K2SO4 + 5H2O
K2
[Cu
97.
98.
99.
249.61 g
100.
101.
102.
103.
104.
105.
mol CuSO4.5H2O
106.
107. =
249.61 g CuSO4.5H2O
108.
109. Molar mass K2C2O4.H2O
110. 184.22 g
111.
112.
6.2566 g K2C2O4.H2O x
1 mol K2C2O4.H2O x
1mol K2[Cu(C2O4)2(H2O)2]
113.
114.
K2C2O4.H2O
184.22 K2C2O4.H2O 2
mol
115.
116.
(C2O4)2(H2O)2]
117.
118.
0.01698
mol
K2
[Cu
353.6
119.
128. Percent
yield
of
(C2O4)2(H2O)2]
129. 1.9778 g
130.
131. 2.8666 g
132.
68.99 %
x 100
K2
[Cu
133.
Experiment 5:
134.
135.
3H2C2O4
3K2C2O4
+
2Fe (OH) 3
2K3 [Fe (C2O4)3].3H2O +
3H2O
136.
137. Theoretical mass of K3 [Fe (C2O4)3].3H2O
138.
139. Molar mass Fe(NH4)2(SO4). 6H2O
140.
141. 392.07 g
142.
143.
144.
5.0330
Fe
(NH4)2(SO4).
6H2O
149.
No of mol of Fe(OH)3
= 0.0128
mol
150.
151.
152.
166.04 g
153.
3.5004 g K 2 C 2 O 4
1 mol K 2 C 2O 4
166.04 g K 2C 2 O 4
154.
155.
156. =
2.496 g H2C2O4
1 mol H 2 C 2 O 4
90.036 g H 2C 2O 4
161.
162. =
163.
164.
491.21 g
182.
100
183.
DISCUSSION
184.
185.
186.
187.
process
often
involves
number
of
chemical
1) Dissolving
with
each
other.
190.
191.
temperature and it
using
suction filtration.
192.
193.
194.
3) Suction filtration
remaining
4) Drying
separation process by
is dried in an oven to eliminate the
solvent.
197.
198.
201.
Percentage yield=
Actual yield
100%
Theoretical yield
205.
Experiment 3
206.
207.
potassium
tris(oxalate)chromium(III)
trihydrate,
to
3+
Cr
208.
++Cr 2 O7
14 H
2-
6 C2 O4
2-
6e
2Cr
3-
7 H2O
(reduction process)
209.
210.
3 C2 O 4
2-
6 CO2
6e
(oxidation process)
The
mixture
is
added
with
potassium
oxalate
212.
As
result,
the
dark-green
crystal
of
potassium
213.
214.
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 O 7 6 CO 2 +9 H 2 O+8 K
8H
Percentage yield=
Actual yield
100%
Theoretical yield
217.
QUESTION
K 2 Cr 2 O7
and
in the product?
218.
219.
In
K 2 Cr 2 O7
220.
2 (+1 ) +2 x+ 7 (2 ) =0
221.
2+2 x 14=0
222.
2 x =12
223.
x=+6
224.
K 2 Cr 2 O7
is +6 .
225.
226.
In the product:
227.
3 (+ 1 )+ x +3 (2 )+ 3 ( 0 )=0
228.
+3+ x6=0
229.
x3=0
230.
x=+3
231.
+3 .
232.
2. Write two half-equations for each reaction involved in the
preparation of the complex using oxalic acid dehydrate,
K2C2O4. H2 O
K 2 Cr 2 O7
and a
234.
235.
++Cr 2 O7
14 H
2-
6 C2 O4
2-
6e
2Cr
3-
7 H2O
236.
237.
3 C2 O 4
2-
6 CO2
6e
239.
240.
Overall equation:
241.
242.
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 O 7 6 CO 2 +9 H 2 O+8 K
8H
243. Experiment 4
244.
245.
copper
(II)
sulphate
pentahydrate
solution
resulting
the
247.
CuSO 4 .5 H 2 O
O
+ K 2 SO 4 +5 H 2 O
Cu
2 K 2 C 2 O4 . H 2 O K 2
CuSO 4 .5 H 2 O
value is quite low which also showed that there must be some errors
while conducting this experiment.
250.
251.
252.
253.
254.
255.
256.
257.
258.
259.
Experiment 5
260.
The
potassium
K3[Fe(C2O4)3].3H2O
tris(oxalate)ferrate(III)
is
synthesized
by
two
trihydrate,
consecutive
FeC 2 O 4
in the form of
SO
. 6 H2O
Fe
261.
NH
262.
H2C2O4
FeC 2 O 4 (s )
H 2 SO 4
6 H 2 O(l)
solution and isolation all of the iron as ferrous oxalate. After all
the yellow precipitates allowed settling, decantation of the
supernatant is performed. This step is essential to remove more
oxalic acid and improves purity of precipitate.
263.
Upon
addition
of
peroxide, oxidation of
potassium
2+
Fe
to
oxalate
3+
Fe
and
hydrogen
266.
267.
H 2 O+ HO 2
2+
2 Fe
3++3 OH
2 Fe
OH
ions
Fe(OH )3
268.
269.
Fe(OH )3 (s)
3++3 OH
Fe
After that, more oxalic acid was added which caused the
270.
C
Fe .3 H 2 O+ 3 H 2 O
271.
all the three experiment. This can be seen as the actual yield of
each product obtained is less than the theoretical yield. The
errors that might affect the theoretical yield were as follow:
274.
275.
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.
284.
CONCLUSION
287.
that
the
reactions
have
occurred.
Meanwhile,
291.
292.
293.
294.
295.
Reference:
296.
297.
1.
Hadariah Bahron, Kamariah Muda, Sharifah Rohaiza,
Karimah Kassim. (2008).
Inorganic Chemistry:
Experiments for Undergraduates.
298.
Kuala Lumpur: UiTM Press.
299.
300.
301.
2.
Raymond Chang and Kenneth A.Goldsby , Chemistry,
302.
303.
copyright 2013 ,
304.
305.
306.
29 Oct 2015