MATERIALS

Distilled water

Potassium iodide

Sulphuric acid

Sodium thiosulphate

Potassium iodate

Starch indicator solution

METHOD

Generation of I2

A 1.2349g of KIO3 was weighed and quantitatively transferred to 500ml volumetric flask to
top up the mark. A 50ml aliquote of the iodate solution was transferred into 250ml conical
flask and then 2.030g of KI were also added. The solution was acidified with 2 drops of
H2SO4.

Preparation of thiosulphate

An 8.7195g of NaS2O3.5H2O was transferred to 500ml volumetric flask to top up to the

mark. A 45.5ml of above solution was added to another 500ml volumetric flask and top up to
the mark.

By means of a measuring cylinder 50, 40, 25, and 10ml of a saturated solution was placed in
I2 and H2O and 500ml (1 to 4) volumetric flasks were properly labelled. Approximately 0,
10, 25 and 40ml chloroform was added to the bottles respectively. About 150ml of distilled
water was added to each of the bottles. The flask was stoppered tightly and shaken for 6 times
thoroughly. A 20ml of the aqueous layer was withdrawn carefully and titrated against 0.01 M
Na2S2O3 using starch solution as indicator .to analyse the chloroform layer, 5ml of the layer
was withdrawn and titrated against 0.1 M thiosulphate solution. While titrating the non-
aqueous layer (chloroform), the titration flask was constantly shaken to avoid the
disappearance of purple colour of non-aqueous layer. Similarly, the aqueous and chloroform
layer was titrated from bottle nos. 2, 3 and 4.

OBJECTIVES

To prepare standard solution of potassium iodate

To determine the ratio of concentrations

To determine the partition coefficient from four bottles

INTRODUCTION

Iodometry is the quantitative analysis of solution of an oxidizing agent by adding an iodide

which reacts to form iodine, which is then titrated. Iodometric titrations, is a method of
volumetric analysis, a redox titration where the appearance or disappearance of elementary
iodine indicates the end point. Iodometry involves indirect titration of iodine liberated by
reaction with analyte, whereas iodometry involves direct titration using iodine as titrant. The
use of iodine as a titrant suffers from two major disadvantages. First, iodine is not particularly
soluble in water, and second, iodine is somewhat volatile. Dilute triiodide solutions are
yellow, more concentrated solutions are brown, and even more concentrated solutions are
violet. Iodide solutions are colourless. If all of other solution components are colourless, it is
possible to detect the endpoint if titrations involving triiodide without the use of an indicator.
Endpoint detection is considerably easier, however, with an indicator.

The indicator that is usually chosen for titrations involving iodide is starch. Starch forms a
dark blue complex with iodine. The end point in iodometry corresponds to a sudden colour
change to blue. Likewise the end point in iodometry corresponds to a sudden loss of blue
colour due to the complex. Sodium thiosulphate is a chemical and medication. As medication
it is used to treat cyanide poisoning and pityriasis versicolor. It is an inorganic compound that
is typically available as the pentahydrate, Na2S2O.5H2O. The solid is an efflorescent (loses
water readily) crystalline substance that dissolves well in water. It is also called sodium
hyposulfite. Solvent extraction is a very common laboratory separation procedure used when
isolating or purifying a product. It is extremely useful for rapid and clean separation of both
organic and inorganic substances. It involves the distribution of a solute between two
immiscible liquid phases. A separation funnel is used for this process (Weber et al, 1986).

RESULTS

Volume of Volume of Volume of thiosulphate

thiosulphate(Vts) in thiosulphate (0,01M) (0,1M) in ml
ml in ml
10 7,5 15,0
25 22,9 15,4
40 28,5 19,6
50 34,7 ////////////////////////////////

CALCULATIONS

3I2 + 6S2O3-3S4O6^-2 + 6I2

TRIAL 1

1. C=n/v

= (0.01) (7, 5/1000) (3/6)

=0.0000375 mol

C=n/v

=0.0000375/ (20/1000)

=0.001875M

2. C=n/v

n =CV
 = (0.010) (22.9/1000) (3/6)

=0.0001145 MOL

C=n/v

=0.0001145/(20/1000)

=0.005725 M

3. C=n/v

n =CV

= (0.01) (28.5/1000) (3/6)

=0.0001125 mol

C=0.0001125(20/1000)

=0.007125 M

4. C=n/v

n =CV

= (0.01) (34.7/1000) (3/6)

=0.0001735 mol

C=n/v

=0.0001735/ (20/1000)

=0.008675 M

TRIAL 2

1. C=n/v
 n = CV

= (0.1) (15.0/1000) (3/6)

=0.00075 mol

C=n/v

=0.00075/ (5/1000)

=0.15 M

2. C=n/v

n =CV

= (0.1) (15.4/1000) (3/6)

=0.00077 mol

C=n/v

=0.00077/ (5/1000)

=0.154 M

3. C=n/v

n =CV

= (0.1) (19.6/1000) (3/6)

=0.00098 mol

C=n/v

=0.00098/ (5/1000)

=0.196 M

CALCULATIONS OF KD
1. KD= [ORGANIC]/ [AQUA]

=[0.001875]/[0.15]

=0.0125

2. KD= [ORGANIC]/ [AQUA]

=[0.005725]/[0.154]

=0.0372

3. KD= [ORGANIC]/ [AQUA]

=[0.007125]/[0.196]

=0.0364
Discussion

From the experiment performed above, the reaction of measured gram of potassium iodide,
the purple colour was decolourised by iodide ion. 2 drops of sulphuric acid was added to the
iodide solution to prevent the decomposition of the ions in the solution and also to create
medium for the solution to proceed. The solution was then titrated against 0.01 M standard
sodium thiosulphate, the titration proceeds with colour changes till pale yellow colour was
observed, showing the presence of iodine in solution. The solution was allowed for two
minutes, this was done to see whether the pale yellow colour will stand, starch solution was
added to the pale yellow solution and the colour changes to blue black, confirming the
presence of the iodine. A few drops of the thiosulphate turn the solution colourless. The
volume of titration was recorded and addition of another titration with 0.1 M thiosulphate
was conducted, provided recording its volume also. The partition coefficient was observed to
be 0.0125 and 0.0372, which clearly shows that the I2 molecules clearly tend to quantitative
distribution in the chloroform, this implies that a large amount of the solid iodine was
extracted into the organic phase, chloroform. The chloroform layer that was drawn from the
beaker was found to contain just some small amount of the iodine.

Precautions

In the second test, the titration was done in drop wise in order to avoid exceeding the
endpoint since just a small amount of the iodine was left in the chloroform phase.

A little of the aqueous layer was left at the tip of the funnel in order to prevent some of the
organic phase from entering the aqueous phase that was collected.

Conclusion
From the experiment and the calculation above, I can conclude that the value of partition
coefficient of iodine in system water-chloroform is 0.0125 and 0.0372 and the ratio of
concentration is 0.1 M.

References

1. Weber W.Jr.Chin Y.P. and Rice C.P. (1986) Determination of Partition coefficients
and aqueous solubilities by reverse phase chromatography-1.Theory and background.
Wat. Res.20, 1433-1442.
2. Modern inorganic chemistry, 2nd edition by William L, jolly, 2010, page 46 to 49
3. Journal of solid state chemistry, 2012, page 4-7, retrieved from
http://www.sciencedirect.com/scince
4. Concise inorganic chemistry, 5th edition by J.D Lee, 2007, page 202-204
5. KNUST chemistry laboratory manual for second year, CHEM 269 & 270