NAME : TLOTITSO

SURNAME : MPHOMELA

STUDENT NO : 202101291

COURSE CODE : PAC 211

EXPERIMENT 10

TITTLE : PREPARATION OF POTASSIM

TRIS (OXALATO) FERRATE

(III) TRIHYDRATE

DUE DATE : 23 MAY 2023

INTRODUCTION

Potassium tris(oxalato)ferrate (III) is an iron metal complex that is linked to the central metal
atom by three oxalate ligands (C 2 O42-). The ligand is bidentate, meaning that it binds to the
metal atom at 2 different places. The metal complex has the chemical formula
K3[Fe(C2O4)3].3H2O.

This compound is utilized in photographic printing with platinum and palladium because it is a
photosensitive substance that changes when exposed to light. It is also frequently employed as an
acidometer to measure monochromatic radiant fluxes from the ultraviolet to visible wavelengths.

The resulting geometry is an octahedral structure, which can be considered as distorted

octahedral due to strict effect due to the bending of the ligand, the different ways the ligands
attach causes the appearance of a stereoisomers. In this experiment, the complex was created by
adding oxalic acid to ferrous ammonium sulfate hexahydrate (Fe (NH 4)2 (SO4)2 .6H2O) in an
acidic environment.

This forms iron (II) oxalate (FeC2O4), a yellow precipitate. This is then added to potassium
oxalate (K2C2O4) and hydrogen peroxide is used to oxidize the iron from a (II+) to (III+) state,
resulting in the creation of the desired green product. Adding potassium oxalate directly to Iron
(III) chloride hexahydrate is an alternative procedure that yields the desired product; the method
we used requires more steps, intermediates, and reactants, in addition to the fact that some of the
reactants are also rather hazardous and dangerous, such as hydrogen peroxide. As a result, it is
the less preferred option of the two. In the second part after the complex has been prepared it, as
subjected to analysis to determine the percentage of oxalate in the sample. This was
accomplished by introducing hot acid to the complex to break it down to its constituent ions, and
then titrating the oxalate ions with MnO4- (Ox-Red reaction). The obtained data were compared
to the predicted proportion of oxalate ions after that. It must be further noted that extra
precautions must be held during analysis of the complex sample due to its photosensitivity.

ABSTRACT

In this experiment, The Fe complex K3 [Fe (C2O4)3].3H2O was prepared. This has been achieved
by first making a Fe2+ complex (ferrous oxalate – FeC2O4) and then adding potassium ion.
Followed by oxidation of Fe2+ to Fe3+ using hydrogen peroxide. The crystals obtained are green in
color.

RESULTS

• Weighed ion (II) ammonium sulphate = 5.0968g

• Weighed oxalic acid dehydrate = 2.5367g

• Weighed potassium oxalate monohydrate = 3.5061g

• Mass of product = 2.3708g

CALCULATIONS

Mr (NH4Fe (SO4)2 = 14.01 + 4(1.008) + 55.84 + 2(32.06) + 8(16.00)

= 266.002 g/mol

m
n(NH4Fe (SO4)2) =
M

5.0968 g
= 266.002 g/mol

= 0.01916075819 mol

Mr ((COOH)2. 2H2O) = 2(12.01) + 2(16.00) + 2(16.00) + 2(1.008) + 4(1.008) + 2(16.00)

= 126.068g/mol

n
n((COOH)2. 2H2O) = M

2.5367 g
= 126.068 g /mol

= 0.02012168036 mol

Mr (C2H2K2O5) = 2(12.01) + 2(1.008) + 2(39.10) + 5(16.00)

= 184.24g/mol
 n
n(C2H2K2O5) =
M

3.5061 g
= 184.2 4 g/mol

= 0.01903006947 mol

⸫Potassium oxalate monohydrate is the limiting reagent since it has small number of moles.
3K2 C2O4 + 2Fe(OH)3 + 3H2C2O4 2K3[Fe(C2O4)3]•3H2O + 3H2O

Mr (2K3[Fe(C2O4)3]•3H2O) = 3(39.10) + 55.84 +6(12.01) + 12(16.00) +6(1.008) + 3(16.00)/2

= 245.624g/mol

2K3[Fe(C2O4)3]•3H2O

3:2

2(0.01903006947) : 3x

0.3806013894/3 : 3x/3

⸫ x = 0.01268671298

m=n×M

m = 0.01268671298 mol × 245.624g/mol

m = 3.116161189g

⸫ Theoretical yield = 3.116161189g

Actual yield
%yield = ×100 %
Theoretical yield

2.3708 g
= × 100 %
3.116161189 g

= 76.08%

DISCUSSION
The hue changes to yellow when oxalic acid is added because of the precipitate Fe 2C2O4. Upon
the addition of Potassium oxalate a brown color is observed. Fe(OH)2 precipitate. When
hydrogen peroxide H2O2 is added, a black color is seen. Hydrogen peroxide with its oxidative
role causes the transformation of Fe (II) to Fe (III) and during this process a black color is
observed. Finally, the green color upon the addition of H2C2O4 that leads to the dissolving of all
brown colored Fe(OH)3 precipitate, where it continues with the formation of
K3[Fe(C2O4)3•3H2O. Clearly the green color is the color of our component.

REFERENCES

1. Hadariah Bahron, Kamariah Muda, S. Rohaiza S. Omar, Karimah Kassim (2011).

2. Inorganic Chemistry. Experiments for undergraduates, UPENA UiTM 2008.

3.http//chem. science oregonstate

edu/courses/ch221-3s/ch223s/2010_U_session_1/report_Guideline_Green_Crystal_Sp_2010.pdf

4. Roscoe, Henry E. (1869–1870). "Research on Vanadium. Part II". Proceedings of the Royal
Society of London. 18 (114–122): 37–42. doi:10.1098/rspl.1869.0012

5. Weast, Robert (1984). CRC, Handbook of Chemistry and Physics. Boca Raton, Florida:
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