Title: Preparation and Studies of Potassium Tris(Oxalato) 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

Apparatus and Materials: Aluminium Sulphite, distilled water, potassium oxalate

monohydrate, oxalic acid dihydrate, sodium hydroxide, hydrochloric acid, sulphuric acid,
potassium manganate, ethanol, beaker, Buchner funnel, vacuum filter, glass rod, filter paper,
conical flask, filter funnel.

Procedure:

1. 0.005 mole of Al2(SO4)3.18H2O was dissolved in 50ml of distilled water. About 3-

5ml of 5M NaOH was added to the mixture dropwise with stirring.

2. The freshly precipitated Al(OH)3 was filtered using vacuum filtration technique and
the precipitate was washed a few times using 10ml of distilled water each time.

3. 0.008 mole of oxalic acid dihydrate and 0.008 mole of potassium oxalate
monohydrate were weighed and dissolved in 125ml of distilled water in a 250ml
beaker. Al(OH)3 was added to the solution and the mixture was heated on a steam
bath with stirring using a glass rod to dissolve the Al(OH)3.

4. The solution was evaporated to about 15ml using a hot plate. The concentrated
solution was gravity filtered into a beaker.

5. 18ml of ethanol was added to the solution dropwise over 10 minutes and cooled in ice
to precipitate completely colourless crystals of the product.

6. The product was vacuum filtered as in step 2 and washed four times with 5ml of
ethanol and dried completely by vacuum suction.

7. The dry product was kept for the next experiment.

8. The product was weighed. About 0.5g was transferred into a small beaker to carry out
the following tests for the presence of potassium, aluminium and oxalate in the
product.
Qualitative Analysis

1. Test for potassium

The flame test was performed for potassium in a fume cupboard using a platinum
wire. The colour was noted.

2. Test for aluminium

About 0.2g of the product was dissolved in 5ml water 1ml of dilute sodium hydroxide
was added to the solution. Any precipitate in the solution was noted. Now a fresh
solution of 0.2g of the product was prepared in 10ml dilute HCl, the solution was
warmed and added with sodium hydroxide solution dropwise until a precipitate was
formed and redissolved in excess sodium hydroxide. The solution was shook after
each addition.

3. Test for oxalate

0.5g of the product was dissolved in 20ml of distilled water. The solution was divided
into two almost equal portions.5ml of dilute sulphuric acid was added in one of the
solutions. Both solutions were heated and added with 3-4 drops of dilute solution of
potassium manganate

Results:

Weight Al2SO4 in Oxalic acid Potassium Product

(g) distilled dihydrate oxalate
water monohydrate

3.0707 1.0084 1.4789 1.6840

Observations

Test 1 Purple coloured flame was formed

Test 2 After addition of NaOH, some precipitate was formed

Test 3 The solution decolourised with the addition of H2SO4

and heating.
Questions:

1. Write an ionic equation for the formation of Al(OH)3 using Al2(SO4)3.18H2O and
NaOH.
Al3+ + OH- Al(OH)3

2. The formation of tris(oxalate) aluminate(III) complex anion is carried out by reacting

Al(OH)3 with the exact number of moles of the oxalate ion and oxalic acid. The
number of moles of each reactant is given in step (3) of the procedure. Using this
information, balance the equation for the reaction:
2Al(OH)3 + 3(C2O42-) + 3H2C2O4 2[Al(C2O4)3]3- + 6H2O

3. Aluminium is present as a free cation when Al2(SO4)3.18H2O is dissolved in water.

Which ions are present when K3[Al(C2O4)3].3H2O is dissolved in water? The function
of acid used in carrying out test (ii) is to release Al3+ from the complex ion,
[Al(C2O4)3]3-. The [Al3+(H2O)6] ion written in simple form as Al3+ is then identified as
described in test (ii). Write equations for the reaction of acid with the product and for
the reaction which indicates the presence of aluminium (III) in the product.
[Al(C2O4)3]3-(aq) + HCl(aq) AlCl3(aq) + 3H+(aq) + 6CO2(g)

4. Aluminium (III) hydroxide is an amphoteric substance i.e., it reacts both with acids
and alkalis to form the aluminium salt of the acid and AlO2- anion respectively. Write
equations for the reactions of Al(OH)3 with HCl and NaOH to indicate the amphoteric
nature of Al(OH)3
Al(OH)3 + 3HCl AlCl3 + 3H2O
Al(OH)3 + NaOH NaAlO2 + 2H2O

5. The oxalate ion is oxidised by the permanganate ion in the acid solution. Follow the
following steps to derive the two half ionic equations for this reaction:

Oxidation of oxalate ion to carbon dioxide

(i) Write C2O42- on the left and Mn2+ on the right of the
(ii) Balance the carbon and oxygen atoms.
(iii) Balance the charge by writing electrons (e-) on the right hand side.

Why is it called oxidation reaction?

Reduction of MnO4- to Mn2+ in acid solution
 (i) Write MnO4- on the left and Mn2+ on the right of
(ii) Balance oxygen by writing H2O on the right hand side
(iii) Balance hydrogen by writing H+ on the left hand side
(iv) Balance the charge by writing electrons (e-) on the left hand side

Multiply with the appropriate factor to obtain the same number of electrons in each
half-equations. Add the two half-equations to obtain the overall equation for the
oxidation-reduction reaction. Why is it called reduction reaction?

What evidence did you see for this redox reaction in test (iii) to indicate the presence
of oxalate in your product?

[O]: C2O42- 2CO2 + 2e-

Oxidation reaction because C2O42- loses electrons

[H]: MnO4- + 8H+ + 5e- Mn2+ + 4H2O

Reduction reaction because MnO4- gains electrons

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

Purple colour of potassium permanganate solution decolourised.

6. Calculate the percentage (%) yield of the product.

Percentage (%) yield = (actual yield / theoretical yield) x 100%
= (1.6840 / 23.119) x 100%
= 7.284%
7. Draw the structure of the oxalatoaluminate anion, taking oxalate as a bidentate ligand.

3-

[ ]
Conclusion:

Potassium tris(Oxalato) aluminate(III) trihydrate {K3[Al(C2O4)3].3H2O} was successfully

formed, and the presence of potassium, aluminium and oxalate were successfully tested.