PRACTICAL 1: COMPREHENSIVE

REPORT

Manyoni N
Student no.: 22026724
Group: B
Lecturer: Dr. Mokhothu & Dr. Ntola
Due date: 30 April 2021
Tittle: PREPARATION OF POTASSIUM TRIOXALATOCHROMATE (III)

Aim: Prepare potassium trioxalatochromate (III)

Introduction
Chromate is a group 6 element (VIb) characteristic to the d-block with a wide
range of possible oxidation states (existing in the oxidation states of -2 to +6),
where the +3 state is the most stable energetically. Cr(III) ion has a high
polarization strength thus like any other transition metal forms octahedral
complex ions.
A complex chemical species with central metals atom surrounded by plenty
ligands. Chromium (III) compounds has an amphoteric character which allows
it to form chromoxalate when it reacts with oxalic acid. It is water insoluble but
can dissolve in acids. Consider the example below:
7C7H2O4.2H2O + K2H2Cr2O7 → K2H2Cr2(C2O4)4(OH)2 + 6CO2 + 19H2O
K2Cr2O7 + C2H2O4 + K2C2O4 → K3[Cr(C2O4)3].3H2O + CO2 + H2O

Experimental (methodology)
Potassium oxalate (3.0715g) and oxalic acid (7.0257g) were weighed and
dissolved in warm water and to this solution added the solution of potassium
dichromate (1.01g) slowly with continuous stirring. The precipitate of potassium
dichromate was boiled with aqueous solution of oxalic acid dehydrate and
potassium oxalate formed by dissolving them in 100mL of distilled water.

The unreacted potassium dichromate was filtered off and filtrate evaporated
to saturation to effect crystallisation. The product was filtered off, washed with
small quantity of acetone and dried in the oven. The product (Potassium
trioxalatochromate (III), 6.0418g) was weighed after cooling and weight will be
used to calculate percentage yield.

Why we wash off the product with acetone and not water?
Acetone is a ketone and is not easily oxidized by acidified potassium
dichromate and it the product of potassium trioxalatochromate (III)is insoluble
in water.

Results and discussion

Table of results
Potassium Oxalic acid Potassium
oxalate dichromate
Weight of sample (g) 3.0715 7.0257 1.01

Yield of product formed

Weight of container + sample (g) 34.1416 g
Weight of container (g) 28.0998 g
Weight of the sample(g) 6.0418g

Calculations
Theoretical yield
K2Cr2O7 + 7C2H2O4 + 2K2C2O4 → 2K3[Cr(C2O4)3].3H2O + 6CO2 + H2O
Molecular mass of K3[Cr(C2O4)3].3H2O = (3 x 39.10) + 52 + [3(2 x 12.01)+
(4 x 16.00)] + [3 (2 x 1.01)+(16)]
= 487.42 g/mol
Mass of K3[Cr(C2O4)3].3H2O = 6.0418g

Actual yield
Molecular mass of C2H2O4 = (2 x 12.01) + (2 x 1.01) + ( 4 x 16)
= 90.04g/mol
𝑚 7.0257
𝑛= = = 0.08 𝑚𝑜𝑙𝑠
𝑀 90.04

Ratio = 0.08/7
= 0.01

Molecular mass of K2Cr2O7 = (2 x 39.10) + (2 x 52) + (7 x 16)

 = 294.2g
𝑚 1.01
𝑛= = = 3.43 × 10−3 𝑚𝑜𝑙𝑠
𝑀 294.2

Ratio = 3.43 × 10−3 ÷ 1 = 3.43 × 10−3

1.01 > 3.43 𝑥 10−3

Therefore K2Cr2O7 is a limiting reagent

1K2Cr2O7 : 2K3[Cr(C2O4)3].3H2O
3.43 × 10−3 ∶ 𝑥
𝑥 = 6.86 × 10−3

𝑚 = 𝑛𝑀
= 6.86 × 10−3 × 487.42
= 3.34g

𝑎𝑐𝑡𝑢𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
𝑝𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 𝑦𝑖𝑒𝑙𝑑 = (𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 ) × 100
𝑦𝑖𝑒𝑙𝑑

3.34
𝑝𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 𝑦𝑖𝑒𝑙𝑑 = (6.0418) × 100

= 55.28%

Discussion
From the experimental results the crystals are monoclinic holohedral and black
in colour. They are not always a mere modest croft’s salt however a complex
because they undergo through a redox reaction. Potassium oxalate and
oxalic acid dehydrate were dissolved in warm water and mixed. The sample
was left for some time to allow the formation of crystals. In a dry environment,
the crystals lose water and decompose into a crystalline powder, while in a
humid environment, they absorb water, and become liquid. As a result, the
precise number of water molecules associated with water formula unit is
unknown. Potassium oxalate and oxalic acid are insoluble in water. The
percentage yield (55.28%) of product formed, was lower than expected due
to random and systematic errors encountered while weighing. The product
was well evaporated and dried well to eliminate errors due to water. The
complex is:

EXOTHERMIC GRAPH
CONCLUSION
The percentage yield of a product formed is less than anticipated. This might
be due to random and systematic errors encountered at some point weighing.
These errors may be minimised by performing the experiment in pressure-
controlled environment. The product must be systematically evaporated to
saturation to impact crystallisation and dried well to eliminate errors due to
water.

References
Jaeger, 1991; Wyrouboff, 1900; Rammelsberg, 1854; Schabus, 1854
Practical manual
Dit ambrose (Makerere University Of Natural Science), April 2017