Title: Preparation and Studies of Potassium Diaquabis(Oxalato) Chromate (III) Dihydrate

{K[Cr(C2O4)2(H2O)2] . 2H2O}

Objective: To prepare potassium diaquabis(oxalate) chromate (III) dihydrate complexes and

study its reactions.

Results:

Mass of oxalic acid dihydrate used 7.0265g

Mass of potassium dichromate used 2.0041g
Mass of sintered glass crucible: 77.0227g
Mass of sintered glass crucible + product 80.9159g
Mass of product 3.8932g
Colour of flame observed Purple colour flame
Observation for isomers Deep-green solution rapidly forms upon the addition of
ammonia and no solid remains indicating a cis-isomer.
Addition with HCl restores the original colour of the
isomeric form.
1. What is the oxidation state of chromium in K2Cr2O7 and in the product? Write two
halfequations for each reaction involved in the preparation of the complex using
oxalic acid dihydrate (H2C2O4.2H2O) and potassium dichromate (K2Cr2O7) and a
balanced equation for the overall reaction.

Oxidation state of chromium in K2Cr2O7: +1(2) + 2x – 2 = 0

x = +6

Oxidation state of chromium in product: x + 0(2) +0(2) = -1

x = -1

Two half equations:

Oxalic acid dihydrate: H2C2O4 2CO2 + 2H+ + 2e- (Oxidation reaction)
Potassium dichromate: Cr2O72- + 14H+ + 6e- 2Cr3+ + 7H2O (Reduction reaction)

Balanced overall equation:

K2[Cr2O7] + 7H2C2O4 . 2H2O 2{K[Cr(C2O4)2(H2O)2] . 2H2O} + 6CO2 +13H2O
2. Calculate the % yield of the product.
K2[Cr2O7] + 7H2C2O4 . 2H2O 2{K[Cr(C2O4)2(H2O)2] . 2H2O} + 6CO2 +13H2O
From equation: 1 mole of K2Cr2O7 produces 2 moles of {K[Cr(C2O4)2(H2O)2] .
2H2O}
Molar mass of K2Cr2O7 = 294.19g/mol
Molar mass of {K[Cr(C2O4)2(H2O)2] . 2H2O}= 339.19g/mol

No. of moles of K2Cr2O7 = mass / molar mass

= 2.0041g / 294.1g/mol
= 6.81 x 10-3 mol

No. of moles of {K[Cr(C2O4)2(H2O)2] . 2H2O} = 2(6.81 x 10-3 mol)

= 0.01362 mol

Theoretical mass of {K[Cr(C2O4)2(H2O)2] . 2H2O} = no. of moles x molar mass

= 0.01362 x 339.19
= 4.6198g

Actual mass of {K[Cr(C2O4)2(H2O)2] . 2H2O} = 3.8932g

Percentage yield (%) = (Actual mass / Theoretical mass) x 100%
= (3.8932 / 4.6198) x 100%
= 84.27%

3. Write the chemical equations for the reactions involved in the tests for the detection of
chromium (III) and oxalate ions. Indicate in each case whether it is an acid-base or
oxidation-reduction reaction.

The test for chromium (III) is an acid-base reaction. Product was dissolved in water
form hexaaquachromium (III) ions [Cr(H2O)6]3+. When abase was added into the
solution, neutral complex and precipitate were formed. For example, reactions with
ammonia solution. The ammonia acts as a base and a ligand. By adding small amount
of ammonia solution, hydroxide ions (OH-) are pulled off the hexaaqua ion to give the
neutral complex.
Equation: [Cr(H2O)6]3+ + 3NH3 [Cr(H2O)3(OH)3] + 3NH4+
 By adding excess ammonia solution, ammonia will replace water as a ligand to give
hexaamminechromium(III) ions.
Equation: [Cr(H2O)6]3+ + 3NH3 [Cr(NH3)6]3+ + 6H2O

Next, the test for oxalate ion is oxidation-reduction reaction reaction. Purple colour of
potassium permanganate will decolourise immediately if react with acid like dilute
sulphuric acid with purple colour of potassium permanganate decolourise slowly with
dilute sulphuric acid. In this case, acid acts as a catalyst in this redox reaction. The
oxalate ion is oxidised by the permanganate ion in the acid solution. Potassium
permanganate acts as an oxidising agent. In this oxidation-reduction reaction, the
C2O42- is oxidised to CO2 and the permanganate ion MnO4+ will be reduced to Mn2+
Equations: C2O42- 2CO2 + 2e-
MnO4+ + 5e- Mn2+

4. Draw the structures of the two possible geometrical isomers of the complex. What is
your conclusion regarding the nature of the isomer in the test (iv)? When dilute
ammonia is added to the solid complex, one molecule of the ligand H2O is replaced
by OH- ion. Write equations for both the isomers to represent this reaction as well as
for the reaction of the hydroxo product and HCl to restore the original complex.

The geometrical isomer that exists in {K[Cr(C2O4)2(H2O)2] . 2H2O} is isomer because

it formed a deep green solution and spreads over the filter paper and there was no
solid remains. The ammonia acts as both a base and ligand. When dilute ammonia is
added to the solid complex, one molecule of the ligand H2O is replaced by OH- ion.
 Equation for both isomers:

K[Cr(C2O4)2(H2O)2] . 2H2O + NH3 K[Cr(C2O4)2(H2O)(OH)] . 2H2O + NH4+

K[Cr(C2O4)2(H2O)(OH)] . 2H2O + HCl K[Cr(C2O4)2(H2O)2] . 2H2O + Cl-

Conclusion:
The potassium diaaquabis(oxalate) chromate (III) dihydrate complexes were successfully
formed and studied. The percentage yield of the product was 84.27%. A deep-green
solution with no solid remains was observed when the product was reacted with ammonia
indicating that it is a cis-isomer.