AIM:

1. To prepare and analyze potassium cis-diaquadioxalatochromate(iii) dihydrate

2. To calculate the percentage of oxalate and chromium ions in the salt

INTRODUCTION:

Potassium cis-diaquadioxalatochromate(iii) dehydrate, K[Cr(H2O2C2O4].2H2O ia a

bidentate ligands. They have Lewis bases that donate two pairs (bi) of electrons to a
metal atom. K[Cr(H2O2C2O4].2H2O contains a chelating ligands. (chelate – Greek word
for claw.)

K[Cr(H2O2C2O4].2H2O is prepared from oxalic acid dehydrate, potassium

dichromate, carbon dioxide and water. The reaction equation is:

K2Cr2O7 + 7H2C2O4.2H2O  2 K[Cr(C2O4)2(H2O)2].2H2O + 6CO2 + 13H2O

Cis-K[Cr(H2O2C2O4].2H2O have two water molecules adjacent to each other;

giving it the cis properties. They have different chemical and physical properties. Both
of each respective properties will be determined via this experiment.
METHODOLOGY:

1. Synthesis of K[Cr(H2O)2(C2O4)2]2H2O

 The procedures are as follow in Inorganic Year 2 Lab Manual

i. Weigh the oxalic acid and potassium dichromate and place them in their
respective mortars.

ii. Grind both separately and mix the two materials.

iii. Continue to grind until a frothing of CO2 is released. The reaction is started.

iv. Immediately pour ethanol in the mixture and heat until the syrup solidifies into
dry powder.

v. Grind the newly formed dry powder (K[Cr(H2O)2(C2O4)2]2H2O).

Apparatus Pestle & mortar, Spatula, Distilled Water, Dropper,

Evaporating dish, 50 ml beakers, hot plate

Material/Chemical (12g, 0.095 mol) oxalic acid, (4g,0.013mol) potassium

dichromate, 20ml ethanol

2. Analysis of the oxalate content in K[Cr(H2O)2(C2O4)2]2H2O

 The procedures are as follow in Inorganic Year 2 Lab Manual and done in
duplicate.

i. Weigh K[Cr(H2O)2(C2O4)2]2H2O powder and add water and KOH in a beaker.

ii. Heat the mixture until a green precipitate is formed.

iii. Filter off the precipitate. Only use hot distilled water for washing.

iv. Wash the precipitate until a clear filtrate is formed. Keep the washing and heat it
up to about 70◦C.
 v. Titrate it with standard KMnO4.

Apparatus 50 ml beakers, weighing balance, 250ml conical flask,

filter, filter paper, hot plate, burette, distilled water

Material/Chemical 0.3g K[Cr(H2O)2(C2O4)2]2H2O, 10ml KOH (10%),

H2SO4, 2ml H3PO4, 0.02M KMnO4

3. Analysis of the chromium content in K[Cr(H2O)2(C2O4)2]2H2O

 The procedures are as follow in Inorganic Year 2 Lab Manual and done in
duplicate.

 Weigh 0.2g K[Cr(H2O)2(C2O4)2]2H2O and dissolve in 50ml distilled water and add
silver nitrate solution and potassium persulfate solution. Heat the solution for 20
minutes and let it cool.

 Add sulphuric acid and phosphoric acid. Let it cool again.

 Add potassium iodide and concentrated hydrochloric acid. Titrate the liberated
iodine with standardized thiosulfate solution.

Apparatus 50 ml beakers, weighing balance, 250ml conical flask,

filter, filter paper, hot plate, burette, distilled water

Material/Chemical 0.2g K[Cr(H2O)2(C2O4)2]2H2O, 2ml silver nitrate, 10ml

potassium persulfate solution, 10ml H2SO4 (10%),
2ml H3PO4, 10ml concentrated HCl, 1g KI, 0.05M
standardized thiosulfate solution
RESULTS/ DATA:

1. Synthesis of K[Cr(H2O)2(C2O4)2]2H2O

Mass of oxalic acid dihydrate = 12.20 g

Masses (g)

Plastic beg + K[Cr(H2O)2(C2O4)2]2H2O 9.38

Plastic beg 0.56

K[Cr(H2O)2(C2O4)2]2H2O 8.82

K2Cr2O7 + 7H2C2O4.2H2O  2 K[Cr(C2O4)2(H2O)2].2H2O + 6CO2 + 13H2O

12 g
1
 0.09519mol
 The limiting reactant is H2C2O4.2H2O which is 126.06 gmol

From the equation above:

7 mol of H2C2O4.2H2O produce 2 mol of K[Cr(C2O4)2(H2O)2].2H2O

0.09519  2
 0.09519 mol of H2C2O4.2H2O produce 7 mol of K[Cr(C2O4)2(H2O)2].2H2O

= 0.0272 mol of K[Cr(C2O4)2(H2O)2].2H2O

= 0.0272 mol × 339.20 gmol-1

= 9.23 g K[Cr(C2O4)2(H2O)2].2H2O

8.82
 100%
Percentage yield = 9.23

= 95.56%
2. Analysis of the oxalate content in K[Cr(H2O)2(C2O4)2]2H2O

Titration with standard KMnO4 (0.02M)

Burette reading 1 2

Final reading (cm3) 33.80 32.10

Initial reading (cm3) 4.50 2.10

Volume of KMnO4 used (cm3) 29.30 30.00

After adding a drop of potassium permanganate to the last washing of the precipitate,
the solution become pale pink then change to colourless after shaking.

5C2O42- + 2MnO4- + 16H+ → 10CO2+ 2Mn2+ + 8H2O

For sample 1,

Mass of dried K[Cr(H2O)2(C2O4)2]2H2O = 0.31 g

5 MV

No. of mol of C2O42- = 2 1000

5 0.02  29.30

= 2 1000

= 1.465 × 10-3 mol

Mass of C2O42- = 1.465 ×10-3mol × 88.02gmol-1

= 0.1289 g

0.1289
 100%
 Percentage of oxalate in sample 1 = 0.31

= 41.58%
For sample 2,

Mass of dried K[Cr(H2O)2(C2O4)2]2H2O = 0.31 g

5 0.02  30.00

No. of mol of C2O42- = 2 1000

= 1.50 × 10-3 mol

Mass of C2O42- = 1.50 ×10-3mol × 88.02 gmol-1

= 0.1320 g

0.1320
 100%
 Percentage of oxalate in sample 2 = 0.31

= 42.58%

41.58  42.58
 Average of percentage of oxalate in the product = 2

= 42.08%

Theoretically,

Molecular relative mass of K[Cr(H2O)2(C2O4)2]2H2O = 339.20 gmol-1

Molecular relative mass of (C2O4)2 = 176.04 gmol-1

176.04
 100%
Percentage of oxalate in K[Cr(H2O)2(C2O4)2]2H2O = 339.20

= 51.90%

42.08
 100%
 Percentage of the purity of K[Cr(H2O)2(C2O4)2]2H2O = 51.90

= 81.08%
3. Analysis of the chromium content in K[Cr(H2O)2(C2O4)2]2H2O

a. Oxidation to dichromate using potassium persulfate

Titration with thiosulfate solution (0.05M)

Burette reading 1 2

Final reading (cm3) 30.60 32.50

Initial reading (cm3) 1.20 1.10

Volume of KMnO4 used (cm3) 29.40 31.40

Cr2O72- + 6I- + 14H+  3I2 + 2Cr3+ +7H2O ------------------- (1)

I2 + 2S2O32-  2I- + S2O63- -------------------- (2)

Balancing equation (1) and (2)

3I2 + 6S2O32-  6I- + 3S2O63- --------------------- (3)

From equation (1), 6 mol I- Ξ 2 mol Cr3+

From equation (3), 6 mol I- Ξ 6 mol S2O32-

 2 mol Cr3+ Ξ 6 mol S2O32-

For sample 1,

Mass of dried K[Cr(H2O)2(C2O4)2]2H2O = 0.20 g

MV
no. of mol of S2O32- = 1000

0.05  29.40
= 1000
 = 1.47 × 10-3 mol

Since 2 mol Cr3+ Ξ 6 mol S2O32-,

2

 1.47  10 3 mol 
 no. of mol of Cr3+ = 6

= 4.9 × 10-4 mol

Mass of Cr3+ = 4.9 × 10-4 mol × 52 gmol-1

= 0.0255 g

0.0255
 100%
Percentage of Cr3+ in sample 1 = 0.20

= 12.75%

For sample 2,

Mass of dried K[Cr(H2O)2(C2O4)2]2H2O = 0.22 g

MV
no. of mol of S2O32- = 1000

0.05  31.40
= 1000

= 1.57 × 10-3 mol

Since 2 mol Cr3+ Ξ 6 mol S2O32-,

2

 1.57  10 3 mol 
 no. of mol of Cr = 6
3+

= 5.23 × 10-4 mol

Mass of Cr3+ = 5.23 × 10-4 mol × 52 gmol-1

= 0.0272 g
 0.0272
 100%
Percentage of Cr3+ in sample 2 = 0.22

= 12.36%

12.75  12.36
 Average of percentage of Cr3+ in K[Cr(H2O)2(C2O4)2]2H2O = 2

= 12.56%

Theoretically,

Molecular relative mass of K[Cr(H2O)2(C2O4)2]2H2O = 339.20 gmol-1

Molecular relative mass of Cr3+ = 52.00 gmol-1

52.00
 100%
Percentage of Cr3+ in K[Cr(H2O)2(C2O4)2]2H2O = 339.20

= 15.33%

12.56
 100%
 Percentage of the purity of K[Cr(H2O)2(C2O4)2]2H2O = 15.33

= 81.93%

DISCUSSION:

For the preparation of K[Cr(H2O)2(C2O4)2]2H2O, oxalic acid dehydrate and

potassium dichromate are grinded together. After the mixture is left for a while, a reaction
occurred where gas carbon dioxide and water are released to form a thick and black
syrup, K[Cr(H2O)2(C2O4)2]2H2O.

K2Cr2O7 + 7H2C2O4.2H2O  2 K[Cr(C2O4)2(H2O)2].2H2O + 6CO2 + 13H2O

Some precautions can be carried out during the experiment:

i. Ethanol is added until it covered all the thick syrup to make sure that ethanol is
enough to replace water inside the complex. This replacement could make the
syrup to become more stable.
 ii. After the chromium (III) hydroxide is completely precipitated, the precipitate is filter
off to eliminate Cr3+ ion. This is because Cr3+ ion would affect the titration of C2O42-
with standard potassium permanganate.

Conclusion:

i. Percentage yield of K[Cr(H2O)2(C2O4)2]2H2O = 95.56%

ii. Percentage of oxalate in K[Cr(H2O)2(C2O4)2]2H2O:

Experimentally = 42.08%

Theoretically = 51.90%

iii. Percentage of Cr3+ in K[Cr(H2O)2(C2O4)2]2H2O:

Experimentally = 12.56%

Theoretically = 15.33%