CHM 477

No of experiment: 3
Title of experiment:
Synthesis of Potassium Tris(oxalate) chromium
(III) Trihydrate: 𝐾3 [𝐶𝑟(𝐶2𝑂4 )3]. 3𝐻2 𝑂

Name of lecturer: Mohd Sufri bin Mastuli

Name: Nur Sarah Hannis bt Kamarulzaman
2019291342
Lab partners: 1. Khaliesah Nur Asyiqah binti Abu Bakar
2019406776
2. Amirah Najiha binti Mohd Affandi
2019685864
3. Aida Nabilah Binti Haily
2019291496
Introduction
Synthesis process is one of the most important aspects of any chemical research is the
preparation of new compounds. In this experiment, a special kind of coordination compound
called coordination compound will be synthesized. A coordination compound consists of a
central metal ion chemically bonded to one or more atoms or groups of atoms(ligands) by
coordinate covalent bonds. Transition metals readily form these coordination compounds, often
resulting in bright colours.
Chromium(III) is the most stable oxidation state of chromium. It forms a number of complexes,
in which six monodentate ligands surround the cation octahedrally. In the above compound,
two oxalate anions (bidentate ligands) and two water molecules coordinate the chromium
cation to provide oxygen atoms at the corners of the octahedron. Two geometrical isomers exist
for the complex ion, [𝐶𝑟(𝐶2 𝑂4 )2 (𝐻2 𝑂)2 ],two (𝐶2 𝑂4 )2− ions [or two H2O molecules] can be on
the same side of octahedron structure of the complex ion giving the cis-isomer or on the
opposite sides giving you trans-isomer.
The amount of coordination compound expected from a given mass of reactants can be
calculated and is called the theoretical yield.
𝐴𝑐𝑡𝑢𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
% 𝑦𝑖𝑒𝑙𝑑 = × 100%
𝑇ℎ𝑒𝑜𝑟𝑖𝑡𝑖𝑐𝑎𝑙 𝑦𝑖𝑒𝑙𝑑
Objective

i.
To synthesize 𝐾3 [𝐶𝑟(𝐶2 𝑂4 )3 ]. 3𝐻2 𝑂
Materials & Apparatus

Materials Apparatus
Oxalic acid Conical flask
Distilled water Filter funnel
Potassium dichromate, 𝐾2 𝐶𝑟2 𝑂2 Glass rod
Potassium oxalate monohydrate, Beaker
𝐾2 𝐶𝑟2 𝑂2 . 𝐻2 𝑂 Glass plate
95% ethanol

Procedure

1. Weigh 5.00g of oxalic acid using analytical balance and dissolve it into a conical flask
containing 10 mL of water.
2. Add 1.8g of potassium dichromate slowly to the mixture and place a filter funnel on the
flask.
3. After the reaction has subsided in about 15 minutes, dissolve 2.0g of 𝐾2 𝐶𝑟2 𝑂2 . 𝐻2 𝑂 in the
hot green-black liquid and heat to boiling for 5 minutes. Cool the vicious reaction to room
temperature and add 10 mL of 95% ethanol and cool the beaker further in ice with frequent
stirring.
4. After cooling in ice until precipitation appear completely, collect the complex through
suction filtration. Wash the crystals with two 5 mL portions of 1:1 ethanol/water followed
by 13 mL of 95% ethanol.
5. Place the solid in a beaker or glass plate and allow it to dry in the oven with temperature
about 80℃.
6. Determine the mass of product and hence, the percentage yield. Then, transfer the product
to a labelled vial. Keep for the next experiment.

Results

1. Theoretical mass of 𝐾3 [𝐶𝑟(𝐶2 𝑂4 )3 ]. 3𝐻2 𝑂 = 5.5803 g

2. Mass of 𝐾3 [𝐶𝑟(𝐶2 𝑂4 )3 ]. 3𝐻2 𝑂 obtained = 4.6887 g
3. Percent yield of 𝐾3 [𝐶𝑟(𝐶2 𝑂4 )3 ]. 3𝐻2 𝑂 = 84.02 %

Calculation

7𝐻2 𝐶2 𝑂4 + 𝐾2 𝐶𝑟2 𝑂7 + 2𝐾2 𝐶𝑟2 𝑂7 + 2𝐻2 𝐶2 𝑂4 ∙ 3𝐻2 𝑂 → 2𝐾3 [𝐶𝑟(𝐶2 𝑂4 )3 ] ∙ 3𝐻2 𝑂 + 4𝐶𝑂2 + 3𝐻2 𝑂

Determination of limiting reactant

𝑚𝑎𝑠𝑠
𝑀𝑜𝑙 𝑜𝑓 𝐻2 𝐶2 𝑂4 =
𝑚𝑜𝑙𝑎𝑟 𝑚𝑎𝑠𝑠

5.0272𝑔
𝑚𝑜𝑙 =
90𝑔
𝑚𝑜𝑙

= 0.05586 𝑚𝑜𝑙

7 𝑚𝑜𝑙 𝑜𝑓 𝐻2 𝐶2 𝑂4 ≈ 2𝐾3 [𝐶𝑟(𝐶2 𝑂4 )3 ] ∙ 3𝐻2 𝑂

2
0.05586 𝑚𝑜𝑙 𝑜𝑓 𝐻2 𝐶2 𝑂4 ≈ 𝐾 [𝐶𝑟(𝐶2 𝑂4 )3 ] ∙ 3𝐻2 𝑂 × (0.05586𝑚𝑜𝑙)
7 3

≈ 0.0160 𝑚𝑜𝑙
 1.8740𝑔
𝑀𝑜𝑙 𝑜𝑓 𝐾2 𝐶𝑟2 𝑂7 =
294.2𝑔/𝑚𝑜𝑙

= 6.3698 × 10−3 𝑚𝑜𝑙

1𝑚𝑜𝑙 𝐾2 𝐶𝑟2 𝑂7 ≈ 2𝐾3 [𝐶𝑟(𝐶2 𝑂4 )3 ] ∙ 3𝐻2 𝑂

6.3698 × 10−3 𝑚𝑜𝑙 𝐾2 𝐶𝑟2 𝑂7 ≈ 2𝐾3 [𝐶𝑟(𝐶2 𝑂4 )3 ] ∙ 3𝐻2 𝑂 × (6.3698 × 10−3 )

≈ 0.01274 𝑚𝑜𝑙

2.1085𝑔
𝑀𝑜𝑙 𝐾2 𝐶𝑟2 𝑂7 ∙ 𝐻2 𝑂 =
184.22𝑔/𝑚𝑜𝑙

= 0.01145 𝑚𝑜𝑙

1𝑚𝑜𝑙 𝐾2 𝐶𝑟2 𝑂7 ∙ 𝐻2 𝑂 ≈ 1𝑚𝑜𝑙 𝐾3 [𝐶𝑟(𝐶2 𝑂4 )3 ] ∙ 3𝐻2 𝑂

∴ 𝐾2 𝐶𝑟2 𝑂7 ∙ 𝐻2 𝑂 𝑖𝑠 𝑡ℎ𝑒 𝑙𝑖𝑚𝑖𝑡𝑖𝑛𝑔 𝑟𝑒𝑎𝑐𝑡𝑎𝑛𝑡

𝑚𝑎𝑠𝑠
0.01145𝑚𝑜𝑙 =
487.36𝑔/𝑚𝑜𝑙

𝑇ℎ𝑒𝑜𝑟𝑖𝑡𝑖𝑐𝑎𝑙 𝑚𝑎𝑠𝑠 𝑜𝑓 𝐾3 [𝐶𝑟(𝐶2 𝑂4 )3 ] ∙ 3𝐻2 𝑂 = 5.5803𝑔

𝐴𝑐𝑡𝑢𝑎𝑙
% 𝑦𝑖𝑒𝑙𝑑 = × 100%
𝑇ℎ𝑒𝑜𝑟𝑖𝑡𝑖𝑐𝑎𝑙

4.6887𝑔
= × 100%
5.5803𝑔

= 84.02%

Discussion

In this experiment, we are required to synthesize potassium tris(oxalate) chromium (III)

trihydrate through a process called crystallization. It is the process of formation of a solid
crystals from solution, melt or by deposition directly from a gas phase. 5.0272g of oxalic acid
was dissolved in 10mL of water then followed by 1.8740g of K2Cr2O7 and dissolved 2.1085g
K2C2O4∙H2O. This reaction formed 2K3[Cr(C2O4)3]∙3H2O + 4CO2 + 3H2O. The limiting
reactant was calculated from this balanced equation to determine theoretical mass of
2K3[Cr(C2O4)3]∙3H2O . Based on the calculation, K2C2O4∙H2O is the limiting reactant and the
theoretical mass of 2K3[Cr(C2O4)3]∙3H2O obtained is 5.5803g with 84.02% of yield. One of
the possible reason that caused this error was probably due to less product been taken from
the Buchner funnel. To overcome this problem, ensure all of the product has left the flask and
walls of the funnel by washing the flask and the wall with 1:1 ethanol:water multiple times to
obtain as many product as we can get.

Conclusion

The synthesize of 2K3[Cr(C2O4)3]∙3H2O yield 84.02% of product and the theoretical mass
obtained was 5.0272g.