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KWAME NKRUMAH UNIVERSITY OF SCIENCE AND TECHNOLOGY

COLLEGE OF ENGINEERING
DEPARTMENT OF CHEMICAL ENGINEERING

TITLE: IODIMETRIC TITRATION VITAMIN C

NAME: SENYO DENNIS A. AKANDE


COURSE: BSC. CHEMICAL ENGINEERING
YEAR: FIRST YEAR
EXPERIMENT NO. : A.1.2.3.
I.D. NO: 1314507
T.A.: BRIGHT KOFI LEONARD
DATE: TH FEBRUARY, 2008.

Aims and Objectives:


1. To generate a known excess of I-3 by the reaction of iodide.
2. To allow the experiment with ascorbic acid to proceed.
3. To back-titrate the excess I-3 with thiosulphate.

INTRODUCTION
This experiment uses a redox titration to determine the weight percent of vitamin C (ascorbic acid) in a
commercial tablet.

The titration of a reducing agent (such as ascorbic acid ) with iodine (I2 , generally present as I3 - , triiodide ion)
to produce iodide ion (I -) is referred to as an iodimetric titration.

A known amount of I2 (or I– 3) is generated by adding an excess of solid potassium iodide to a known volume of
acidified standard potassium iodate (KIO3 ) solution.
IO3 - + 5 I - + 6 H+ à 3 I2 + 3 H2O
L.R excess
The generated I2 is reacted with limited amount of ascorbic acid .

C6 H8 O6 + 2 H2O + I2 à C6 H6 O6 + 2 I - + 2 H3O +
Ascorbic acid (vit –C) excess

Finally, the excess iodine is back-titrated with sodium thiosulphate (Na2S2O3) solution that was already
standardized.

I2 + 2 S2O32- à 2I- + S4O6 2-


Tetrathionate ion

The amount of ascorbic acid is determined by the stoichiometry of the reaction and the difference between the
total amount of I2 present and the amount of I2 that was left over after reaction with ascorbic acid and hence
reacted with thiosulphate.

CHEMICALS AND EQUIPMENT


Starch indicator: Make a paste of 5 g of soluble starch and 5 mg of Hg2I2 in 50 ml of distilled water. Pour the
paste into 500 ml of boiling distilled water and boil until it is clear.
Sodium thiosulphate: 9 g Na2S2O3 . 5H2O/student.
Sodium carbonate: 50 mg Na2CO3/student.
Potassium iodate: 1 g KIO3/student.
Potassium iodide: 12 g KI/student.
0.5 M H2SO4: 30 ml/student.
Vitamin C: Dietary supplement containing 100 mg of vitamin C per tablet is suitable. Each student needs six
tablets.
0.3 M H2SO4: 180 ml/student.

PROCEDURE
1) 0.07M Na2S2O3 was prepared by dissolving 4.35g of Na2S2O3.5H2O in 250ml of freshly boiled distilled
water containing 0.05g of Na2CO3. 0.01M KIO3 was prepared by accurately weighing 1g of the solid
reagent and dissolving it in distilled water and making it to the 500ml mark of the volumetric flask.
2) The thiosulphate solution was standardized as follows:
50ml of KIO3 solution was pipette into a flask. 2g of solid KI and 10ml of 0.5M H2SO4 was added o the
solution. It was immediately titrated with the thiosulphate solution until the solution had lost its entire
colour (pale yellow). 2ml of starch indicator was added and was titrated till the blue colour of the
solution disappeared.

3) Titration with two additional 50ml volumes of KIO3 solution was repeated.

4) Two tablets of vitamin C was dissolved in 600ml of 0.3M H2SO4, using a glass rod to help break the
solid. (Some solid binding material will not dissolve).

5) 2g of the solid KI and 50ml and 50ml of standard solution KIO3 was added and titrated with standard
thiosulphate as above. 2ml of starch indicator was added just before the endpoint titrate until the blue
colour of the solution disappeared.

TABLE OF VALUES

Burette Reading/cm3 1 2 3
Initial volume 0.00 0.00 17.1
Final volume 17.3 17.1 33.2
Titre value 17.3 17.1 16.1

Average titre = 9.70 + 9.70


2
= 9.70cm3

Titration reaction:
H4Y + Ca2+ CaH2Y +2H+

CALCULATION
Mole ratio = 1:1 H4Y= 0.1M If 1000ml=0.1 9.70ml=

If 30ml contains 9.7 250ml=

m (Ca2+) =0.008083 40 =0.323g of Ca in 25g =

DISCUSSION
From the experiment, when dilute HCl was added to the CaCO3 till effervescence ceases, a salt was formed i.e.
CaCO3(aq) + 2HCl(aq) CaCl2(aq) + H2O(l) + CO2(g)

The salt dissociate into ions in the soln i.e.


CaCl2(aq) Ca2+ + Cl-

The EDTA has a structure


O
HO
CH2
OH
CH2CH2N
O
OH CH2C

OH

EDTA can be represented as H4Y. On reaction with the calcium ion, the two ends of EDTA are replace with the
calcium ion and hydrogen ion is released into soln, making the soln slightly acidic i.e.

H4Y + Ca2+ CaH2Y +2H+

In order to obtain good results, buffer solution which resist changes in ph or whose ph remain fairly constant on
addition of small amount of acid or base is added. This gives a natural medium for the reaction to come to a
successful end. Therefore EDTA on reaction with calcium ion react in the ratio 1:1. hence the amount of
calcium ion in the solution can be determined.

DISCUSSION
It can be inferred from the definition of density that density is directly proportional the mass of the substance
but inversely proportional to its volume. Thus as mass increases, density increases and as volume increases,
density decreases. It was observed that the wooden objects were less dense than water.
After comparing the averages of experimental densities to the graphical densities were about the same. The
graph was a scattered graph and thus a line of best fit was drawn for each graph.

CONCLUSION
Since the experiment is a specific one and buffer solution knowing the concentration of the EDTA, the amount
of Ca2+ and % can be calculated.
PRECAUTIONS
 The weighing balance was set to the zero mark before weighing the amount of CaCO3
 Accurate volume of H2O, Buffer soln and indicator was used
 All readings recorded was taken from the meniscus of the liquid.
 All apparatus were wash

 SOURCES OF ERRORS
 The effervescence did not entirely dissolve in the HCl before proceeding the experiment
 Too much of the indicator can affect the result of the reading

 REFERENCE
 BENERAL CHEMISTRY by RAYMOND
 HEALTH CHEMISTRY(teachers annoted solution)
 INTRODUCTORY CHEMISTRY by JOHN P. SEVENGOR

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