Exp 4 CHM361

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Objective

To synthesise a coordination compound, potassium tris(oxalato)ferrate(III) trihydrate


under carefully controlled conditions.

Introduction
Synthesis is a useful technique in all areas of chemistry. This technique is
important because it is the basis for developing new compounds, which maybe useful
for animals and vegetation. Most developments in the pharmaceutical industry as
well as the introduction of new and less harmful pesticides are made possible
because the chemicals involved are synthesised and tested in the laboratory. In
addition, many chemical compounds used in everyday life are synthesised from
simpler materials.

Ferrous ammonium sulphate was dissolved in a slightly acid solution, excess


oxalic acid, H 2 C 2 O4 is added, and the balance chemical reaction below show the
reaction take place in the experiment:
Fe( NH 4 ¿2( SO 4 ¿2.6 H 2 O + H 2 C 2 O4 FeC 2 O4 (s)+ H 2 SO 4 +( NH 4 ¿2 +6 H 2 O(l)

FeC 2 O 4 (s) is finely divided precipitate and tends to collodial. When the solution
was heated it may causes the solution to coagulate and the facilities separating the
precipitate from the solution.

FeC 2 O 4 (s) precipitate was added with potassium oxalate which produces a
slightly basic solutionfor the oxidation of the ferrous ion to the ferric ion to the by
hydrogen peroxide, H 2 O 2. The following reaction takes place:
2+¿¿
H 2 O+ H O 2 +2 Fe 2 Fe3 +¿¿ + 3OH −

The OH − ion concentration of the solution is high enough so that some Fe3 +¿¿
reacts with the OH −to form ferric hydroxide that is brown precipitate as follows:
3 +¿¿
Fe + 3OH

Fe(OH¿3 . H 2 C 2 O4 was added in excess the Fe(OH¿3 dissolves
and the soluble complex K 3 ¿ . Ethanol is added to the solution to cause the complex
ion salt to precipitate.
Results
1. Mass of Fe( NH 4 ¿2( SO 4 ¿2.6 H 2 O used = 5 g
2. Moles of Fe( NH 4 ¿2( SO 4 ¿2.6 H 2 O used = 0.0165 mol
3. Mass of K 3 ¿ obtained = 3.6 g
4. Moles of K 3 ¿ obtained =0.01 mol
5. Theoretical yield of K 3 ¿ (moles) = 0.01 mol
6. Theoretical yield of K 3 ¿ (mass) = 4.9 g
7. Percent yield of K 3 ¿ = 73.47%

Calculations
2) Mass of Fe( NH 4 ¿2( SO 4 ¿2.6 H 2 O used = 5g
Molar mass of Fe( NH 4 ¿2( SO 4 ¿2.6 H 2 O = 302.1 g/mol

Mole = Mass/Molar Mass


= 5 g/ 302.13g/mol
= 0.0165 mol

3) Mass of filter paper and flask = 10.46g


Mass of filter paper + flask + K 3 ¿ = 14.06g

Mass of K 3 ¿ obtained = 14.06g - 10.46g


= 3.6g

4) Mass of K 3 ¿ = 3.6g
Molar Mass of K 3 ¿ = 491.1 g/mol

Mole = Mass/Molar Mass


= 3.6g/ 491.1 g/mol
= 0.0073 mol

5) Theoretical yield of K 3 ¿ (moles) = 0.01 mol

6) Theoretical yield of K 3 ¿ (mass)

= 0.01 mol × 491.1 g/mol


= 4.9 g

7) Percent yield of K 3 ¿

3.6 g
= × 100%
4.9 g

= 73.43%

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