CH204

EXPERIMENT 4

PREPARATION AND ANALYSIS

OF CHROMIUM OXALATE
COMPLEXES

NAME: PRISHILA DEWAR

ID: S11144724

LAB PARTNERS: SONIKA CHANDRA

ID: S11144458

LAB SESSIONS: FRIDAY (8-12AM)

DATE OF EXPERIMENT: 17/08/18

DATE OF REPORT SUBMISSION: 30/08/18

INTRODUCTION:

Chromium is aBtransition element and ions of theseNelements in aqueous solution for complexNions. The chro
mium salt is surroundedNby two bidenate oxalateNligands and two-monodenate waterNligands. The methods
that arM used in
thisNexperimentare grinding, evaporation, decanting, centrifuging, boiling (steam bath), filtration andNlastly sp
ectroscopy. The purpose of thisNexperiment is to prepare many complexesNthat are forms between oxalate
andMchromium (III), and examiningBsome of the properties and determiningNthe purity of the sample
prepared.

EXPERIMENTAL:

Apparatus used:

Beaker stirring rod

Filter paper watch glass

Clamp/ring stand measuring cylinder

Conical flask pipette

Burette dropper

Suction flask wash bottle

Spatula

1. PREPARATION OF POTASSIUM TRIOXACHROMATE

Reagents required:
4.5g Oxalic acid dichromate 2cm3 ethanol
1.5g potassium dichromate 5cm3 1:1 mixture of ethanol
1.8g potassium oxalate 5cm3 pure ethanol

PROCEDURE:

To a solution of 4.5g of oxalic acid dehydrate in 10ml of warm distilled water, portion of 1.5g of potassium
dichromate was added. The resulting solution was heated to boiling with addition of 1.8g of potassium oxalate
with constant stirring when the vigorous solution was subsided. The solution was cooled to room temperature,
added 2ml of ethanol, and continued cooling (using ice-bath) until the blue-green crystals was separated from
the black solution. The product was collected into a filter paper (using suction), washed with 5ml of 1:1 mixture
of ethanol and water and finally with 5ml of pure ethanol. The product was dried on a filter paper and the
percentage yield was calculated.
RESULTS:

PART 1:

Mass of oxalic acid = 4.5 g Potassium dichromate = 1.5 g

Mass of beaker + reactant = 36.0445 g Beaker + potassium dichromate = 32.8511 g

Empty beaker = 31.6875 g Empty beaker = 31.3641 g

Potassium oxalate = 1.8 g Vile + lid = 11.0987

Potassium oxalate + beaker = 33.5667 g Product + vile+ lid = 11.6189 g

Empty beaker = 31.6875 g Final product = 11.6189 – 11.0987

= 0.5202 g

Preparation of Potassium trioxalatochromate (III)

N ( K2C2O3) = m/M r

= 1.5 g

294.10 g/mol

= 0.0051 mol

N ( H2C2O4.2H2O) = m/Mr

= 4.5 g

126 g/mol

= 0.0357 g/mol

N ( K2C2O4.H2O) = m/Mr

= 1.8 g

184 g/mol

= 0.0098 g/mol

Equation 1:

K2C2O3 + H2C2O4.2H2O + 2 K2C2O4.H2O--------- > 2K3C2O4.H2O

Mole ratio

K2Cr2O7 : H2C2O4.2H2O : 2 K2C2O4.H2O

1 : 1 : 2
0.0051 : 0.0357 : 0.0098

Limiting reagent : 2 K2C2O4.H2O Mass of vile + lid + product = 11.6189 g

K2C2O7 : 2 K2C2O4.H2O Mass of product = 0.5202 g

1 : 2 Theoretical yield of 2K3[Cr(C2O4)3.3H2O]

0.0051 mol : x

X (2 K2C2O4.H2O) = 0.01 mol

M = n x Mr

= 0.01mol x 677 g/mol

= 6.91 g

Percentage yield = Experimental yield x 100

Theoretical yield

= 0.5202 g x 100

6.91 g

= 7.54 %

DISCUSSION:
The percentage yield of the product is low which was 7.54% because the experiment may have contained some
impurities, may have been evaporated during the process when kept outside and also some of the chemicals
might have been wasted while transferring from one place to another. The experiment contained some errors
such as weighing errors and measuring instruments.

ANALYSIS:

A. DETERMINATION OF PERCENTAGE OXALATE

Reagents required:
10% KOH solution
Dilute H2 SO4
KMnO4
 PROCEDURE:
0.3g of the sample was weighed accurately into a beaker. 10ml of distilled water and 10ml of 10% solution
of KOH was added. The mixture was boiled until no more green precipitate was visible, was filtered and
washed well with hot distilled water. The filtrate was titrated and washed at 70˚C with standard KMnO 4 to
the first pink color after acidification with dilute sulphuric acid.

B. DETERMINATION OF PERCENTAGE OF CHROMIUM

Reagents required:
Conc. H2 SO4 1.5g solid KBrO3
5.0g ammonium sulphate 10ml conc. HCL
1.0g solid KI standard thiosulphate solution

PROCEDURE:
2.0g of the sample was weighed accurately into a 250ml conical flask. 50ml of water was added followed
by 3ml of Conc. H2 SO4. 1.5g of solid KBrO3 was added and boiled for 10 minutes. 5.0g of ammonium
sulphate was dissolved in the minimum volume of hot water and added to the hot reaction solution. The
whole solution was boiled for 30-40 minutes until all the excess of Br2 was been volatilized. Now 10ml of
1M HCI solution was added and boiled again until starch-iodine paper was not stained when held in the
stream. The liquid was cooled, 10ml of conc. HCI was added and 1.0g of solid KI. Titrated the liberated
iodine with the standard thiosulphate solution providing to the first light green color.

RESULTS:

a. Results for percentage oxalate

Initial Final Titre

1 8.00ml 10.50ml 2.50ml
2 10.50ml 12.6ml 2.10ml
Average volume=2.30ml

Empty beaker = 31.4931 g N (MnO4) = C x V

Initial reading of the burette = 0.00 mL = 0.0160M x 18.5L

Final reading =18.50 mL =0.296mol/L

Titre = 18.50 mL
Equation 2:
2MnO4-(aq) + 5C2O42-(aq) 26H+ → 2Mn2+ + 8H2O (aq) + 10CO2 (aq)
Moles of Oxalate (C2O42-)
Mole Ratio Mass of Oxalate
2MnO4-(aq) : 5C2O42-(aq) M = n/Mr
2 : 5 =0.74mol/88.02g.mol
0.296 : X =0.0084g
1.48 : 2x
2x 2x
X = 0.74

Percentage of oxalate 2K3(Cr(C2O4)3).3H2O : 5C2O42-

%C2O42- = mass of C2O42- / Mass of sample taken X 100 2 : 5
= 0.0084/0.20 x 100 0.01 : x
= 4.2%
X (C2O42) = 0.025mol
M = n/Mr Theoretical %= 2.2005/6.773 x 100
= 0.025mol/ 88.02g.mol = 32.49%
= 2.2005g Percentage purity
44.74% - 32.49% = 12.25%

b. Results for percentage of chromium

Initial Final Titre
1 0.00ml 8.20ml 8.20ml
2 8.20ml 16.15ml 7.95ml
Average volume=8.075ml

Determination of percentage of chromium

Equation 3
6BrO32-(aq) + 10Cr3-(aq) + 36H-(aq) → 3Br2 (aq) + 10Cr6+(aq) + 18H2O(l)
Equation 4
6H-(aq) + 2Cr6-(aq) → 2Cr3-(aq) + 3I-(aq)
Equation 5
2S2O32-(aq) + I2(aq) → 2I-(aq)
Mole Ratio
2S2O32- : I2 : 2Cr3+
2 : 1 : 2
3 : 2
6 : 3 : 2

% chromium Moles of Cr3+

N= c x v N= C x V
= 0.0801M x 9x10-3L = 1/3 x 7.21x10-4
= 7.21x10-4 mol = 2.40x10-4 mol

Mass of Cr3+ Percentage Chromium = 0.012g/o.20 x 100

M = n x Mr = 6%
= 2.40x10-4 x 51.996
= 0.012g

DISCUSSION:

The results obtained from the two results had few difference in the average volume for both oxalate and
chromium ions. They did not have much difference in the titre values. There were some of the errors made
while the experiment was carried out which might have affected the product as well. Such as misreading
volumes which might affect the final result. However the percentage of the final product was very low.

POST LAB ANSWERS:

1. Oxalic acidNsolution is heated before titrationNwith KMnO4 solution because this reactionNhappens
only in certain temperature. If not heated the Light pinkNtitrated solution turns brown soon
andNreaction takes longer time. All reactionsBrequire activation energy and the correctBorientation. If
you do not heat the mixture, the reactants won't haveBenough activation energy (in a short time) to start
theNreaction even they are in the correctBorientation. However, if you heat, the heat energyNgained by
particles convert it to kineticNenergy, so they move withNhigher speed. This results in
higherNfrequency of collision among theNparticles, so, increased frequency ofNeffective collision.
Thus, rate of reaction increasesNand you will be able to obtain yourMresults in a shorterNtime.
2. The green precipitate that formed was oxalate.
CONCLUSION:

It can be concluded, that after doing the experiment it can be said that the percentage yield differs hence the
percentage purity always differs because there might have been some of the impurities held during the
experiment and also errors were being made thus, the purity percentage might be very low in a sense it had lot
of impurities in the oxalate percentage of purity.

REFERENCE:

Experiment 4 lab handout, preparation and analysis of chromium oxalate complexes

(Prof. Robert J. Lancashire, 2015) http://wwwchem.uwimona.edu.jm/lab_manuals/c10expt15.html

(Jim Clark, 2003) chromium, https://www.chemguide.co.uk/inorganic/transition/chromium.html