Experiment 8: PREPARATION AND STUDIES OF POTASSIUM

TRIS(OXALATO)ALUMINATE(III) TRIHYDRATE {K3[Al(C2O4)3].3H2O}

Title

Preparation and studies of potassium tris(oxalate)aluminate(III) trihydrate

{K3[Al(C2O4)3].3H2O}.

Objective
To prepare Potassium tris(oxalato)aluminate(III)trihydrate {K3[Al(C2O4)3].3H2O} and
study its reactions.

Introduction

Aluminum is a chemical element symbolized by Al with atomic number 13, the element
is a hard, strong and white metal. Element aluminum itself is clearly metallic and ionic in
their character.It is the group 13 element in periodic table. The electronic configuration
is [Ne]3s23p1 as a result the trivalent state is its most important state. It is the commonest
metallic element in the earth’s crust and occurs widely in nature in silicates such a micas
and feldspares.Oxalate ion is a versatile ligand since it can act as a mono - , bi - ,
tri - and tetradentate ligand and capabl of forming bridged polynuclear complexes.
Oxalate is the dianion with the formula C2O42-. Either name is often used for derivatives,
such as salts of oxalic acid, for example sodium oxalate Na2C2O4, or dimethyl oxalate
((CH3)2C2O4). Oxalate also form coordination compounds where it is sometimes
abbreviated as ox.
Aluminum occurs widely in nature as aluminosilicate minerals and as bauxite,
Al2O3.xH2O from which the metal can be produced by electrolysis after dissolving in
molten cryolite, Na3AlF6. The metal is mainly used in aluminum alloys. The
organoaluminum compounds are used in the catalysts involved in the polymerisation of
ethane. Group 13 of the Periodic Table includes the elements boron (B), aluminum (Al),
gallium (Ga), indium (In) and thallium (Tl). The electronic configuration is ns2np1 and
the group valency is three. Aluminum is present in the third period and contains empty 3d
orbitals and favours the formation of complexes with six coordination number. It forms
stable octahedral complexes with ligands such as 8-hydroxyquinoline which also known
as “oxine” (C9H7NO) and with the oxalate anion. In this experiments you are to
prepare an oxalate-aluminum (III) complex and study its reactions.
Materials and apparatus
0.005 mole of Al2(SO4)3.18H2O, distilled water, 5M NaOH, oxalic acid, potassium
oxalate monohydrate, beaker, vacuum filter, hot plate, measuring cylinder, and Bunsen
burner.

Procedure
1. Dissolve 0.005 mole of Al2(SO4)3.18H2O in 50 ml of distilled water. Prepare the
solution of 5M NaOH in 10 ml of distilled water. Add the solution dropwise with
stirring.
2. Filter the precipitate using a suction filtration and wash with distilled water few
times using 10 ml of distilled water each time
3. Weigh 0.0159 mole of oxalic acid and 0.0163 mole of potassium oxalate
monohydrate and dissolve in 125ml of distilled water in a 250ml beaker. Add
Al(OH)3 to the solution and heat the mixture on a steam bath with stirring using a
glass rod to dissolve Al(OH)3.
4. Evaporate the solution to about 15ml of ethanol to the solution dropwise over 10
min and cool in ice to precipitate completely colorless crystals of the product.
5. Filter the solution by using suction filtration and wash four times with 5ml of
ethanol each time, dry completely by vacuum suction.
6. Weigh the product.
7. Using the product to do qualitative test.

Qualitative test
1) Test for potassium
Perform the flame test in a fume cupboard using a platinum wire. Record down the
color of flame.

2) Test for aluminum

Dissolve about 0.2g of the product in 5ml water and add 2ml of dilute sodium
hydroxide solution. Record down the observation. Prepare a solution using another
0.2 g of the product in 10ml of dilute HCI, warm the solution and add NaOH
solution dropwise until a precipitate formed and redissolved in excess NaOH.
Shake the solution after each addition.

3) Test for oxalate

Dissolve 0.5g of product in 20ml of distilled water. Divide the solution into two
almost equal portions. Add 5ml dilute H2SO4, in one of the solution. Heat both the
solution and add in each solution 3-4 drop of dilute KMnO4. Note the color of the
solution.
Results
Weight of Al2(SO4)3.18H2O: 3.1518g
Weight of oxalic acid dihydrata: 1.0090g
Weight of potassium oxalate: 1.5030g
Weight of product: 1.4088g

Test Potassium Aluminum Oxalate

Observation Violet flame White precipitate 1. Test tube with
produce when the formed when react product + H2SO4
product burn of with sodium remain the same
Bunsen burner hydroxide. 2. Test tube with
only product
decolorize the
KMnO4

Report

1) Al2(SO4)2 + 6NaOH  2Al(OH)3 + 3Na2SO4

2) 2Al(OH)3 + 3(C2O42-) + 3H2C2O4  2[Al(C2O4)3]3- + 6H2O

3) When K3[Al(C2O4)3].3H2O dissolve in water, it forms K+ cation and [Al(C2O4)3]3-

anion. Equation: [Al(C2O4)33- + HCl  AlCl3 + 3H + 6CO2

4) with NaOH: Al(OH)3 + NaOH  NaAlO2 + 2H2O

With HCl: Al(OH)3 + HCl  AlCl3 + 2H2O

5) Ionic equation 1: C2O42-  2CO2 + 2e-

Ionic equation 2: MnO4- + 8H+ + 5e-  Mn2+ + 4H2O

Overall equation: 2MnO4- + 5C2O42- + 16H+  2Mn2+ + 10CO2 + 8H2O

Called reduction is because the oxidation number of Mn reduce from (+7) to (+2)
Evidence: the purple color of KMnO4 been decolorize by the oxalate ion. MnO4- will
been in purple color while the Mn2+ ion is colorless
 𝑎𝑐𝑡𝑢𝑎𝑙 𝑚𝑎𝑠𝑠
7) percentage of yield = × 100%
𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑚𝑎𝑠𝑠

Number of mole of Al2(SO4)2 = mass/molar mass

= 3.1518/342.15
= 0.00921mol

1 mol of Al2(SO4)2 produce 2 mol of Al(OH)3

Mol of Al(OH)3 = 2 x 0.00921mol

= 0.0184mol

1 mol of Al(OH)3 produce 1 mol of K3[Al(C2O4)3].3H2O

Mol of K3[Al(C2O4)3].3H2O = 0.0184mol

Theoretical mass = mole x molar mass

= 0.0184 x 408.33
= 7.52g
1.7650
Percentage yield = × 100%
7.52
= 23.46%