Experiment 4: Preparation of Potassium Tri(oxalate)aluminate(III)trihydrate

Objective
1. Synthesis potassium tri(oxalate)aluminate(III) trihydrate

Reagents

Apparatus

Potassium Hydroxide (KOH)

Beaker (250 Ml)

Oxalic Acid Dehydrate (H2C2O4. 2H2O)

Graduated Cylinder

Ethanol

Hot Plate

Acetone

Glass Rod

Distilled Water

Buchner Funnel
Filter Paper
Watch Glass
Aluminium Foil

Introduction
Aluminium, like many of the transition metals, forms octahedral complex ions. In this lab
we will synthesize potassium tris(oxalato)aluminate(III), K3[Al(C2O4)3]3H2O.
First, lets cover some background on aluminium. Like several other metals, aluminium
is reactive enough to displace hydrogen from water. However, this does not take place because
aluminium develops a layer of aluminium oxide that protects the metal surface. This oxide
coating can be dissolved by acid, according to the equation shown below.
Al2O3 + 3HCl 6Cl- + 2Al3+ + 3H2O
But, in this experiment the oxide coating is dissolved by excess hydroxide, forming the
[Al(OH)4]- ion. The chemical equation for this particular reaction is as follows:
Al2O3 + 2OH- + 3H2O 2[Al(OH)4]-

Procedure

1. Aluminium foil was cut into roughly one-centimetre squares and measure approximately
0.50 grams (this should require 12-14 squares of foil). The exact mass used was recorded.

2. The foil was transferred to a 250-mL beaker.

3. Using a graduated cylinder, 30 mL of water and 15 mL of 4.0 M KOH was added. A

stirring rod was used to ensure that the aluminium foil is submerged.

4. When the reaction has subsided, the solution was heated to boiling on a hotplate to
dissolve any unreacted aluminium.

5. Next, 8.0 grams of oxalic acid dihydrate was added, in small portions, to the hot solution.

6. The hot solution was filtered through a Buchner funnel and the filtrate was transferred
back to the 250-ml beaker.

7. The beaker was placed in an ice bath and was cooled to 10C.

8. 20 mL of ethanol was added approximately and the beaker was leave in the ice bath until
crystallization appears complete.

9. The product was recovered by suction filtration, rinsed with 10mL of acetone, and was
allowed to dry.

10. The sample was weighted and recorded.

Result

Discussion
In this experiment, K3[Al(C2O4)3]3H2O was synthesized. First, aluminium metal is
reacted with potassium hydroxide to produce the [Al(OH)4]- ion. Next, oxalic acid (H2C2O4) is
added, which neutralizes the excess hydroxide and provides a source of the oxalate ion. Lastly,
the [Al(C2O4)]3- ion that is produced is precipitated as the potassium salt by the addition of
ethanol. Ethanol is added to reduce the polarity of the solution. The overall reaction is
represented by the equation shown below.
Al + 3KOH + 3H2C2O42H2O K3[Al(C2O4)3]3H2O + 6H2O + 3/2 H2
From the calculation the limiting reagent are both aluminium and potassium hydroxide. The
theoritical

value

that

calculated

should

yield

about

7.4

gram

of

potassium

tri(oxalate)aluminate(III) trihydrate. From the experiment we managed to synthesized 5.389

gram of potassium tri(oxalate)aluminate(III) trihydrate. From the formula :

Conclusion
We have successfully synthesized our desired product Potassium
Tri(oxalate)aluminate(III)trihydrate with a yield of 73%.

References
House, J. E. (2013). Inorganic Chemistry 2nd Edition. Oxford: Elsevier.
McClure, M. (2009). Retrieved December 2, 2014, from University of North Carolina at
Pembroke web site:
http://www2.uncp.edu/home/mcclurem/courses/chm226/introduction_Coordination
Silberberg, M. S. (2013). Chemistry: The Molecular Nature of Matter and Change 6th edition.
New York: McGraw-Hill.