CHM 475
INORGANIC CHEMISTRY
(EXPERIMENT 3)
Course Name : Bachelor in Education Science (Hons.) Chemistry
Course Code : ED 260
Title of experiment : Synthesis of Potassium Tris(oxalato) chromium(III)
Trihydrate: K3[Cr(C2O4)3].3H2O
Name : Nur Fatma Hanis binti Abdullah Sani
Matrix no : 2014665254
Group Partner : Salmee Safina binti Mohd Yusuf
Group : ED2602A
Lecturer’s name : Dr Amalina binti Mohd Tajuddin
Date of Submission : 10/04/2015
EXPERIMENT 3
OBJECTIVE
The objective of this experiment is to synthesize potassium tris(oxalato) chromium(III)
trihydrate.
INTRODUCTION
Synthesis is process in which substances combine to form completely new substances.
Chromium(III) is the most stable oxidation state of chromium. It forms a number of complexes,
in which six monodentate ligands surround the cation octahedrally. The balance chemical
equation for this experiment is 8H+ + 3H2C2O4 + 6K2C2O4.H2O + K2Cr2O7 6CO2 + 9H2O +
8K+ + 2K3[Cr(C2O4)3].3H2O. From the balance chemical quation, we can calculate theoretical
yield by determining the limiting reagent. The percentage yield can be calculate by following
formula : % yield = actual yield x 100%
theoretical yield
CHEMICAL AND APPARATUS
Conical flask Boiling water bath
Oxalic acid 95% ethanol
Weighing balance Ice cube
Distilled water Beaker
K2Cr2O7 Oven
Potassium oxalate
PROCEDURE.
1. 5.00 g of oxalic acid was dissolved in 10 ml of distilled water in a conical flask.
2. 1.80 g of potassium dichromate, K2Cr2O7 was added to the mixture using a funnel.
3. After 15 minutes, 2.10 g of potassium oxalate monohydrate was added in the hot
green-black liquid and was boiled for 5 minutes.
4. 10 ml of 95% ethanol was added and the beaker was cooled in ice with continuously
stirred.
5. The complex was collected by a suction filtration.
6. The crystal was washed with two 5 ml portions of 1:1 ethanol/water followed by 13
ml of 95% ethanol.
7. The solid was placed on a glass plate and was allowed to dry in the oven.
DATASHEET EXPERIMENT 3
Name : Nur Fatma Hanis binti Abdullah Sani Date : 31/03/2015
Student ID : 2014665254 Group : ED2602A
Determination of limiting reactant.
Balance chemical equation
8H+ + 3H2C2O4 + 6K2C2O4.H2O + K2Cr2O7 6CO2 + 9H2O + 8K+ +
2K3[Cr(C2O4)3].3H2O.
The number of moles H2C2O4
5.04 g / 90 gmol-1 = 0.0560 moles
The number of moles K2Cr2O7
1.77 g / 294 gmol-1 = 0.0060 moles
The limiting reactant is K2Cr2O7.
1. Theoretical yield of K3[Cr(C2O4)3].3H2O
1 mole of K2Cr2O7 = 2 moles of K3[Cr(C2O4)3].3H2O
0.0060 moles of K2Cr2O7 x 2 moles of K3[Cr(C2O4)3].3H2O
1 moles of K2Cr2O7
0.0120 moles of K3[Cr(C2O4)3].3H2O
0.0120 moles of K3[Cr(C2O4)3].3H2O x 487 gmol-1 = 5.84 g
Theoretical yield of K3[Cr(C2O4)3].3H2O is 5.84 g
2. Mass of K3[Cr(C2O4)3].3H2O obtained
Mass of K3[Cr(C2O4)3].3H2O obtained is 4.62 g
3. Percent yield of K3[Cr(C2O4)3].3H2O
4.62 g x 100% = 79.11 %
5.84 g
The percentage yield of K3[Cr(C2O4)3].3H2O is 79.11 %.
QUESTIONS.
1. What is the oxidation state of chromium in K2Cr2O7, and in the product?
Oxidation state of chromium in K2Cr2O7 is +6.
Oxidation state of chromium in K3[Cr(C2O4)3].3H2O is +3.
2. Write two half-equations for each reaction involved in the preparation of the complex
using oxalic acid dihydrate and potassium dichromate, and a balanced equation for the
overall reaction.
14H+ + Cr2O72- + 6C2O42- + 6e 2Cr(C2O4)33- + 7H2O
DISCUSSION
A. Interpretation.
The potassium dichromate dissolved slightly in acid solution.
When potassium dichromate solution was added to oxalic acid solution, orange colored
mixture spontaneously warm up almost to boiling.
When potassium oxalate monohydrate was added to the solution, the following chemical
reaction take place, 8H+ + 3H2C2O4 + 6K2C2O4.H2O + K2Cr2O7 6CO2 + 9H2O + 8K+ +
2K3[Cr(C2O4)3].3H2O.
The theoretical yield obtained is 5.84 gram and the mass of 2K 3[Cr(C2O4)3].3H2O
obtained was 4.62 gram.
The percentage yield obtained is not 100% due to some errors occur during the
experiment. The error occurred were stated below.
B. Error
Using contaminated apparatus - we need to make sure our conical flask is cleaned before
we are using it, this is important because the other substance may left in the conical flask
and cause our product to contaminate.
Period of heating – when there is heating process, limited working experiment may force
the students shorten the heating period so the mixture cannot react completely or maybe
the mixture was over heated.
C. Safety Precaution
We must wear gloves as a protection as we do not want to have direct contact with toxic
chemicals.
We also need to be careful when heating oxalic acid, potassium chromate and potassium
oxalate as it will bump when we heat too long.
D. Suggestion Mark
For an accurate result, we can carry out this experiment in the unlimited working time.
We also must weigh accurately according to the actual weight that required in the lab
manual.
CONCLUSION
The balance chemical equation is 8H+ + 3H2C2O4 + 6K2C2O4.H2O + K2Cr2O7 6CO2 +
9H2O + 8K+ + 2K3[Cr(C2O4)3].3H2O.
The theoretical yield of K3[Cr(C2O4)3].3H2O is 5.84 gram.
The mass of K3[Cr(C2O4)3].3H2O obtained is 4.62 gram.
The percentage yield is 79.11%.
The percentage error is 20.89%.
REFERENCES
hang, R. (2013). In R. Chang, Chemistry (pp. 103,104). Mc Graw Hill Copyright.
Rayyan, U. (n.d.).
https://www.academia.edu/7725871/To_synthesize_potassium_tris_oxalato_chromium_III_trih
ydrate_K3_Cr_C2O4_3_.3H2O_. Retrieved April 2015, from https://www.academia.edu:
https://www.academia.edu/7725871/To_synthesize_potassium_tris_oxalato_chromium_III_trih
ydrate_K3_Cr_C2O4_3_.3H2O_
CHM 475
INORGANIC CHEMISTRY
(EXPERIMENT 4)
Course Name : Bachelor in Education Science (Hons.) Chemistry
Course Code : ED 260
Title of experiment : Synthesis of Copper(II) Oxalate Complexes
Name : Nur Fatma Hanis binti Abdullah Sani
Matrix no : 2014665254
Group Partner : Salmee Safina binti Mohd Yusuf
Group : ED2602A
Lecturer’s name : Dr Amalina binti Mohd Tajuddin
Date of Submission : 10/04/2015
EXPERIMENT 4
OBJECTIVE
The objective of this experiment is to prepare a copper(II) oxalate complex.
INTRODUCTION
Synthesis is process in which substances combine to form completely new substances.
Coordination compound (oxalic acid) is the production by reacting oxalic acid with transition
metal. Transition metal acts as a Lewis acid and oxalate ion and water act as Lewis bases. The
balance chemical equation for this experiment is CuSO4.5H2O + 2K2C2O4.H2O
K2[Cu(C2O4)2(H2O)2] + K2SO4 + 5H2O. From the balance chemical equation, we can calculate
theoretical yield by determining the limiting reagent. The percentage yield can be calculate by
following formula : % yield = actual yield x 100%
theoretical yield
CHEMICAL AND APPARATUS
Copper(II) sulphate pentahydrate Ice bath
Distilled water Suction filtration
Conical flask Cold distilled water
Hot plate Oven
Potassium oxalate monohydrate Funnel
PROCEDURE.
1. 2.00 g of copper(II) sulphate pentahydrate was weighed using a weighing balance.
2. 30 ml of distilled water was added in the conical flask together with the copper(II)
sulphate pentahydrate.
3. The solution was heated until the solid dissolved.
4. 6.20 g of potassium oxalate monohydrate was weighed and added to a conical flask.
5. The potassium oxalate monohydrate was dissolved with 40 ml distilled water at
room temperature.
6. The heated copper(II) sulphate solution was added slowly to the potassium oxalate
solution and the flask swirled slowly.
7. The solution was chill in ice bath for 30 minutes.
8. The crystal produced after the cooling process was collected by suction filtration.
9. The crystal was washed twice with 3 ml portions of cold water.
10. The crystal was dried in the oven.
DATASHEET EXPERIMENT 4
Name : Nur Fatma Hanis binti Abdullah Sani Date : 31/03/2015
Student ID : 2014665254 Group : ED2602A
Determination of limiting reactant.
Balance chemical equation
CuSO4.5H2O + 2K2C2O4.H2O K2[Cu(C2O4)2(H2O)2] + K2SO4 + 5H2O.
The number of moles CuSO4.5H2O
2.04 g / 159.61 gmol-1 = 0.0128 moles
The number of moles 2K2C2O4.H2O
6.27 g / 184.22 gmol-1 = 0.0340 moles
The limiting reactant is CuSO4.5H2O.
1. Theoretical yield of K2[Cu(C2O4)2(H2O)2]
1 mole of CuSO4.5H2O = 1 moles of K2[Cu(C2O4)2(H2O)2]
0.0128 moles of CuSO4.5H2O x 1 moles of K2[Cu(C2O4)2(H2O)2]
1 moles of CuSO4.5H2O
0.0128 moles of K2[Cu(C2O4)2(H2O)2]
0.0128 moles of K2[Cu(C2O4)2(H2O)2] x 353.80 gmol-1 = 4.53 g
Theoretical yield of K2[Cu(C2O4)2(H2O)2] is 4.53 g
2. Mass of K2[Cu(C2O4)2(H2O)2] obtained
Mass of K2[Cu(C2O4)2(H2O)2] obtained is 3.90 g
3. Percent yield of K2[Cu(C2O4)2(H2O)2]
3.90 g x 100% = 86.09 %
4.53 g
The percentage yield of K2[Cu(C2O4)2(H2O)2] is 86.09 %.
DISCUSSION
A. Interpretation.
Copper(II) oxalate complexes was formed when copper(II) sulphate pentahydrate
solution react with potassium oxalate monohydrate solution.
After heating and cooling, the copper(II) oxalate complexes formed in the form of blue
precipitate.
The precipitate was suck using suction filtration and the blue crystal was dried in an
oven.
The overall reaction takes place is CuSO4.5H2O + 2K2C2O4.H2O K2[Cu(C2O4)2(H2O)2]
+ K2SO4 + 5H2O.
The theoretical yield obtained is 4.53 gram and the mass of K 2[Cu(C2O4)2(H2O)2]
obtained was 3.90 gram.
The percentage yield obtained is not 100% due to some errors occur during the
experiment. The errors occurred were stated below.
B. Error
Using contaminated apparatus - we need to make sure our conical flask is cleaned before
we are using it, this is important because the other substance may left in the conical flask
and cause our product to contaminate.
Period of heating – when there is heating process, limited working experiment may force
the students shorten the heating period so the mixture cannot react completely or maybe
the mixture was over heated.
Period of cooling - when there is heating process, limited working experiment may force
the students shorten the heating period so the mixture cannot react completely.
C. Safety Precaution
We must wear gloves as a protection as we do not want to have direct contact with toxic
chemicals.
D. Suggestion Mark
For an accurate result, we can carry out this experiment in the unlimited working time.
We also must weigh accurately according to the actual weight that required in the lab
manual.
CONCLUSION
The balance chemical equation is CuSO4.5H2O + 2K2C2O4.H2O K2[Cu(C2O4)2(H2O)2]
+ K2SO4 + 5H2O.
The theoretical yield of K2[Cu(C2O4)2(H2O)2] is 4.53 gram.
The mass of K2[Cu(C2O4)2(H2O)2] obtained is 3.90 gram.
The percentage yield is 86.09 %.
The percentage error is 13.91 %.
REFERENCES
Chang, R. (2013). In R. Chang, Chemistry (p. 758 and 1002). Mc Graw Hill copyright.
Rayyan, U. (n.d.). https://www.academia.edu. Retrieved April 2015, from
https://www.academia.edu:
https://www.academia.edu/7725865/preparation_of_copper_II_oxalate_complexes
CHM 475
INORGANIC CHEMISTRY
(EXPERIMENT 5)
Course Name : Bachelor in Education Science (Hons.) Chemistry
Course Code : ED 260
Title of experiment : Synthesis of Potassium Tris(oxalato)
Ferrate(III) Trihydrate
Name : Nur Fatma Hanis binti Abdullah Sani
Matrix no : 2014665254
Group Partner : Salmee Safina binti Mohd Yusuf
Group : ED2602A
Lecturer’s name : Dr Amalina binti Mohd Tajuddin
Date of Submission : 10/04/2015
EXPERIMENT 5
OBJECTIVE
The objective of this experiment is to synthesize potassium tris(oxalato) ferrate(III) trihydrate.
INTRODUCTION
Synthesis is process in which substances combine to form completely new substances. Ferrous
ammonium sulphate was dissolved in a slightly acid solution, excess oxalic acid, H2C2O4 is
added, and the balance chemical reaction that take place is Fe(NH 4)2(SO4)2.6H2O + H2C2O4
FeC2O4 + H2SO4 + (NH4)2SO4 + 6H2O. FeC2O4 precipitate was added with potassium oxalate
which produces slightly basic solution for the oxidation of the ferrous ion to the ferric ion.
Ferrous ion react with hydroxide ion to form ferric hydroxide that formed as brown precipitate.
With the addition of excessive H2C2O4, the ferric hydroxide dissolve and the soluble complex
formed. The balance chemical equation is : 3K 2C2O4 + 2Fe(OH)3 + 3H2C2O4
2K3[Fe(C2O4)3].3H2O + 3H2O.
CHEMICAL AND APPARATUS
Ferrous ammonium sulfate Dilute sulfuric acid
Distilled water Beaker
Weighing balance Oxalic acid dehydrate
Boiling water bath 6% H2O2
Solid potassium oxalate monohydrate 95% Ethanol
Buchner funnel Suction filtration
Cooled acetone Funnel
PROCEDURE.
Procedure A.
1. 5.00 g of ferrous ammonium sulfate was well-stirred in 20 ml of water containing 1 ml of
dilute sulfuric acid in the beaker.
2. 2.50 g of oxalic acid dihydrate was added in 25 ml of water.
3. The oxalic acid solution was added to the ferrous ammonium sulfate solution.
4. The mixture was heated slowly and yellow precipitate was formed. Supernatant was
decant.
5. 15 ml of hot water was added to the yellow precipitate and the supernatant was decant.
Then 15 ml of hot water was added again to the mixture.
6. 3.50 g solid potassium oxalate monohydrate was added to the mixture and it was heated
approximately 40 ˚C.
7. At 40 ˚C, 10 ml of 6% H2O2 was added to the mixture and was heated until boiling.
8. A solution of 2.00 g of oxalic acid dihydrate in 30 ml of water in portions was added to
the mixture.
9. The clear solution was boiled and was filtered through a Buchner funnel.
10. 30 ml of 95% ethanol was added slowly to the solution.
11. The crystals was dissolved by heating.
Procedure B.
1. The crystals was obtained using suction filtration.
2. The crystal was washed twice with a cooled 1:1 ethanol/water mixture and with cooled
acetone.
3. The crystal was dried in air and weighed.
DATASHEET EXPERIMENT 5
Name : Nur Fatma Hanis binti Abdullah Sani Date : 24/03/2015
Student ID : 2014665254 Group : ED2602A
Determination of limiting reactant.
Chemical equation involved.
1) Fe(NH4)2(SO4)2.6H2O + H2C2O4 FeC2O4 + H2SO4 + (NH4)2SO4 + 6H2O
2) Fe3+ + 3OH- Fe(OH)3
Note that the number of mole of Fe(OH)3 is equal to the number of mole of
Fe(NH4)2(SO4)2.6H2O.
Balanced chemical equation
3K2C2O4 + 2Fe(OH)3 + 3H2C2O4 2K3[Fe(C2O4)3].3H2O + 3H2O.
The number of moles K2C2O4
3.31 g / 166.22 gmol-1 = 0.0199 moles
The number of moles H2C2O4
2.67 g / 90.02 gmol-1 = 0.0297 moles
The number of moles Fe(NH4)2(SO4)2.6H2O
5.04 g / 392.01 gmol-1 = 0.0129 moles
Since the number of mole of Fe(OH)3 is equal to the number of mole of Fe(NH4)2(SO4)2.6H2O, so
the number of mole of Fe(OH)3 is 0.0129 moles.
The limiting reactant is Fe(OH)3.
4. Theoretical yield of K3[Fe(C2O4)3].3H2O
2 mole of Fe(OH)3 = 2 moles of K3[Fe(C2O4)3].3H2O
0.0129 moles of Fe(OH)3 x 2 moles of K3[Fe(C2O4)3].3H2O
2 moles of Fe(OH)3
0.0129 moles of K3[Fe(C2O4)3].3H2O
0.0129 moles of K3[Fe(C2O4)3].3H2O x 491.21 gmol-1 = 6.34 g
Theoretical yield of K3[Fe(C2O4)3].3H2O is 6.34 g
5. Mass of K3[Fe(C2O4)3].3H2O obtained
Mass of K3[Fe(C2O4)3].3H2O obtained is 4.82 g
6. Percent yield of K3[Fe(C2O4)3].3H2O
4.82 g x 100% = 76.03 %
6.34 g
The percentage yield of K3[Cr(C2O4)3].3H2O is 76.03 %.
DISCUSSION
A. Interpretation.
Ferrous ammonium sulphate was dissolved in a slightly acid solution, excess oxalic acid,
H2C2O4 is added, and the balance chemical reaction that take place is
Fe(NH4)2(SO4)2.6H2O + H2C2O4 FeC2O4 + H2SO4 + (NH4)2SO4 + 6H2O.
The brown precipitate formed due to the presence of ferric hydroxide that produce from
reaction between hydroxide ion and ferrous ion.
The balance chemical equation is : 3K2C2O4 + 2Fe(OH)3 + 3H2C2O4
2K3[Fe(C2O4)3].3H2O + 3H2O.
The theoretical yield obtained is 6.34 gram and the mass of 2K 3[Fe(C2O4)3].3H2O
obtained was 4.82 gram.
The percentage yield obtained is not 100% due to some errors occur during the
experiment. The error occurred were stated below.
B. Error
Using contaminated apparatus - we need to make sure our conical flask is cleaned before
we are using it, this is important because the other substance may left in the conical flask
and cause our product to contaminate.
Period of heating – when there is heating process, limited working experiment may force
the students shorten the heating period so the mixture cannot react completely or maybe
the mixture was over heated.
C. Safety Precaution
We must wear gloves as a protection as we do not want to have direct contact with toxic
chemicals.
D. Suggestion Mark
For an accurate result, we can carry out this experiment in the unlimited working time.
We also must weigh accurately according to the actual weight that required in the lab
manual.
CONCLUSION
The balance chemical equation is 3K2C2O4 + 2Fe(OH)3 + 3H2C2O4
2K3[Fe(C2O4)3].3H2O + 3H2O.
The theoretical yield of K3[Fe(C2O4)3].3H2O is 6.34 gram.
The mass of K3[Fe(C2O4)3].3H2O obtained is 4.82 gram.
The percentage yield is 76.03%.
The percentage error is 23.97%.
