EXPT.

7 DETERMINATION OF ASCORBIC ACID

IN A VITAMIN C TABLET
IODIMETRICALLY
Structure
7.1 Introduction
Objectives
7.2 Principle
7.3 Requirements
7.4 Solutions provided
7.5 Procedure
7.6 Observations and Calculations
7.7 Results

7.1 INTRODUCTION
In this laboratory course you have so far learnt about and carried out quantitative
experiments based on gravimetric and volumetric measurements. In the previous
experiment you had learnt about and performed a complexometric titration so as to
determine the hardness of a water sample. In this experiment you are going to learn
about another type of titration called redox titration. As the name suggests these
titrations are based on oxidation-reduction reactions and involve the transfer of
electrons. You would recall from Section 10.7 of Unit 10 of the MCH-001 course that
there are a number of oxidimetric and reductimetric reagents. In oxidimetric titrations
the oxidising agents are used to determine the reducing agents, while in reductimetric
titrations reducing agents are employed for the determination of oxidising agents. You
would also recall from section 10.7.1 of Unit 10 that the I2/2I‒ couple is of medium
oxidising power. The molecular iodine is a weak oxidant, whereas the iodide ions are
relatively weak reductants. Therefore, the I2/2I‒ redox couple can be used for the
determination of both reductants as well as oxidants.

Ascorbic acid, also known as Vitamin C, is an important water-soluble biological

antioxidant and free radical scavenger. Vitamin C is required for the growth and
repair of tissues in all parts of the body. It is necessary to form collagen, an important
protein used to make skin, scar tissue, tendons, ligaments, and blood vessels etc.
Unlike most other mammals, humans cannot synthesize ascorbic acid and thus this
vitamin must be ingested daily. It is found commonly in fruits and vegetables such as
citrus fruits (oranges, lemons, limes, tangerines etc.), melons, tomatoes, peppers,
broccoli, green leafy vegetables such as spinach, potatoes and turnips etc. A regular
balanced diet provides an adequate amount of ascorbic acid needed by the body.
However, the use of regular, supplementary doses of Vitamin C in prophylaxis
(preventive medication) and therapy of the common cold and other medical conditions
has been strongly advocated.

As you are aware, it is desirable to test the shelf life of pharmaceutical products, more
so when they are not very stable. Vitamin C in tablets is inherently unstable, as it
slowly gets oxidized by air. In this experiment you would learn about and perform the
titrimetric determination of ascorbic acid present in a given tablet by using iodine.
Such titrations are termed as iodimetric titrations. The iodine would be generated
in-situ from potassium iodate by acid. In the next experiment you would learn about
using iodide ions for the determination of oxidising agents like, available chlorine in
bleaching powder.

51
 Objectives
After studying and performing this experiment you should be able to:
• define iodimetric titrations,
• state and explain the principle of iodimetric titrations with reference to the
determination of ascorbic acid in vitamin C tablets,
• state the reasons for using potassium iodate in place of iodine in iodimetric
titrations,
• explain the meaning of back titration and state its need in the iodimetric
determination of vitamin C,
• prepare a standard solution of potassium iodate and use it to standradise a
solution of sodium thiosulphate,
• prepare a solution of ascorbic acid from the given tablets of vitamin C,
• perform the determination of ascorbic acid in the prepared solution by
iodimetric method, and
• calculate the amount of ascorbic acid in the prepared solution of vitamin C tablet

7.2 PRINCIPLE
As mentioned above, ascorbic acid is a mild reducing agent and can be determined
with the help of a moderate oxidising agent like iodine in a direct titration with it.
Such a direct titration of reducing agents with iodine is termed as iodimetric titration.
The reaction of ascorbic acid and I2 can be given as:

However, as it is difficult to prepare and store standardized solutions of iodine, a

known excess of iodine is generated in situ by the reaction of known amount of
potassium iodate with an excess of potassium iodide in presence of strong acid as per
the following reaction.
IO3− + 5I − + 6H + → 3I 2 + 3H 2 O (l )
In the presence of excess iodide, dissolved iodine exists primarily as the triiodide ion.
I2 + I− → I 3−
This solution of triiodide ions is then reacted with ascorbic acid. A part of iodine (as
triodide ions) is consumed for the oxidation of ascorbic acid and the remaining excess
of iodine is determined by titrating with a standard solution of sodium thiosulphate.
Such an indirect determination is called back titration.
2S2 O32− + I 2 → S4 O 62− + 2I −
As you are aware, iodine forms a violet coloured complex with starch. Therefore, the
endpoint of the titration accompanied by complete consumption of iodine can be
detected by the disappearance of the color of starch-iodine complex.

52
By knowing the total quantity of iodine formed from potassium iodate and the
quantity of iodine left after reaction with ascorbic acid, the amount of iodine reacted
with the ascorbic acid can be calculated. This can then be used for the determination of
the amount of vitamin C (ascorbic acid).

7.3 REQUIREMENTS
Apparatus Chemicals
Volumetric flask (100 cm3, 500 cm3) – 1each Vitamin C tablets
Burette (50 cm3) –1 Potassium iodate
Pipette (10 cm3) –1 Potassium iodide
Sodium thiosulphate
Weighing bottle –1
Sulphuric acid
Burette stand with clamp –1
Sodium carbonate
Conical flasks (100 cm3) –2
Starch
Funnel –1
Beakers (250 cm3) –2

7.4 SOLUTIONS PROVIDED

1. ~0.03 M Sodiun thiosulphate: It is prepared by dissolving about 7.5g of
sodium thiosulfate pentahydrate in about 200 cm3 of distilled water taken in a
1.0 dm3 volumetric flask and adding about 0.1 g of sodium carbonate to it.
The solution is then diluted to the mark with distilled water.

2. 0.5% Starch indicator solution: It is prepared by mixing 0.25g of soluble

starch with 50 cm3 of distilled water taken in a 100 cm3 conical flask or beaker
heating it with stirring at about 80oC for about 5 minutes. The solution and is
then allowed to cool to room temperature.

3. 10% Potassium iodide solution: It is prepared by dissolving 100g of KI in

about 200 cm3 of distilled water taken in a one litre beaker or conical flask and
stirring well to dissolve it. It is followed up by making up the volume to 1 litre
by adding more distilled water.

4. 0.3M Sulphuric acid: It is prepared by diluting about 4.2 cm3 of conc. sulphuric
acid to 250.0 cm3 with distilled water in a conical flask or beaker.
(Caution: The acid should be added slowly to water accompanied by constant
stirring)

7.5 PROCEDURE
The determination of the ascorbic acid in vitamin C tablets using iodimetric consists of
the following steps:
a) Preparation of the solution of the given ascorbic acid tablets
b) Preparation of potassium iodate primary standard
c) Standradisation of sodium thiosulphate
d) Determination of ascorbic acid in the above solution by back titration

53
 Follow the steps as directed below:

a) Preparation of the solution of the given ascorbic acid tablets

• Accurately weigh a vitamin C tablet and grind to a powder in a clean
mortar with the help of a pestle.
• Dissolve the powder in about 20 cm3 of 0.3M H2SO4 solution and
carefully transfer to a 500 cm3 volumetric flask. Dilute to the mark with
distilled water.
(You may need to repeatedly wash the mortar and transfer the washings to
the volumetric flask before making up the volume)

b) Preparation of potassium iodate primary standard

• Accurately weigh about 0.6 g of KIO3 (Mm, 214 g mol-1) and
quantitatively transfer to about 30 cm3 of distilled water taken in a 100
cm3 volumetric flask. Stir to dissolve and dilute to the mark with distilled
water.

c) Standardization of sodium thiosulphate solution

• Pipet out 10 cm3 of KIO3 solution into a 100 cm3conical flask and add
about 8-10 cm3 of 10% KI solution and 10 cm3 of 0.3M H2SO4 solution.
• Titrate the solution of potassium iodate by adding Na2S2O3 solution from
the burette. Continue addition till the solution becomes pale yellow.
• Add about 2 cm3 of starch solution and continue adding sodium
thiosulphate dropwise until the violet colour of the starch iodine
complex just disappears.
• Repeat the standardization procedure at least three times and record your
observations in Observation Table 7.1.

d) Determination of ascorbic acid in the solution prepared at ‘a’ above by

back titration
• Pipette out 10 cm3 of the ascorbic acid solution ( CAUTION: DO NOT
SUCK THE SOLUTION) and transfer to a 100 cm3 conical flask.
• Pipette out 10 cm3 of KIO3 solution to the conical flask containing
ascorbic acid solution (you may use a burette to transfer potassium iodate
solution)
• Add about 8-10 cm3 of 10% KI solution and 10 cm3 of 0.3 M H2SO4
solution, and titrate the solution by adding Na2S2O3 solution from the
burette. Continue addition till the solution becomes pale yellow.
• Add about 2 cm3 of starch solution and continue adding sodium
thiosulphate dropwise until the violet colour of the starch iodine complex
just disappears.
• Repeat the procedure at least three times and record your observations in
Observation Table 7.2.

7.6 OBSERVATIONS AND CALCULATIONS

a) Preparation of standard solution of potassium iodate
Mass of weighing bottle + potassium iodate = m1 g = ..............g

54
 Mass of weighing bottle (after transferring potassium iodate) = m2 g = ......... g
Amount of potassium iodate transferred = m1 – m2 = m g = ............. g
Molar mass (Mm) of potassium iodate = 214 g mol−1
Volume of potassium iodate prepared = 100 cm3
Molarity of potassium iodate solution =

m × 1000 10m
M KIO = = = ...........M
3 100 × 214 214

b) Standardisation of sodium thiosulphate solution

Volume of standard KIO3 solution taken in conical flask, Viodate = …cm3
Volume of 10% KI added : 8-10 cm3
Volume of 0.3 M H2SO4 added : 10 cm3
Solution in the burette: Sodium thiosulphate
Indicator used: Starch

Observation Table 7.1: Standardisation of sodium thiosulphate

S.No. Volume of potassium Burette reading Titre value (in cm3)
iodate (in cm3) Initial Final (Final-initial reading)
1
2
3
Concordant reading

The concentration of the given sodium thiosulphate solution can be determined as

follows.

The reactions involved:

IO3− + 5I − + 6H + → 3I 2 + 3H 2 O (l )
(
3 2S2 O 32− + I 2 → S4 O 62− + 2I − )
IO + 6H + 6S2 O → 3S4 O + I − + 3H 2 O
−
3
+ 2−
3
2−
6

Molarity equation: 6MIodateVIodate = M Thiosulphate V Thiosulphate

6 M IodateVIodate
M Thiosulphate =
VThiosulphate

Substituting the values, the molarity of thiosulphate = ......M

Determination of ascorbic acid in the prepared solution of vitamin C tablet

Volume of ascorbic acid sample taken in conical flask, VAsc. = …cm3
Volume of standard KIO3 solution taken in conical flask, Viodate = …cm3
Volume of 10% KI added : 8-10 cm3
Volume of 0.3 M H2SO4 added : 10 cm3

55
 Solution in the burette: Sodium thiosulphate
Indicator used: Starch

Observation Table 7.2: Determination of the amount of potassium iodate left

after the oxidation of ascorbic acid [Back titration]
S.No. Volume of iodate Burette reading Titre value (in cm3)
solution (in cm3) Initial Final (Final-initial reading)
1
2
3
Concordant reading

The molarity of the potassium iodate solution back titrated after the oxidation of
ascorbic acid can be determined as follows.

The reaction involved:

IO3− + 5I − + 6H + → 3I 2 + 3H 2 O (l )
(
3 2S2 O32− + I 2 → S4 O 62− + 2I − )
IO + 6H + 6S2 O → 3S4 O + I − + 3H 2 O
−
3
+ 2−
3
2−
6

Molarity equation: 6MʹIodateVIodate = M Thiosulphate V Thiosulphate

M Thiosulphate VThiosulphate
'
M Iodate =
6 VIodate

Substituting the values, of the molarity and the volume of thiosulphate used, the
molarity of back titrated KIO3
′
= M Iodate = ......M
We can calculate the amount of iodine used for the oxidation of ascorbic acid as
follows:

a) The amount of iodine generated in the reaction mixture

Let the molarity of standard potassium iodate = M iodate M
This implies that the amount per cm3 of the standard solution
= Miodate mM per cm3
Volume of standard potassium iodate used = 10.0 cm3
The amount of potassium iodate taken = 10.0 × Miodate mM
As each mole of potassium iodate provides three moles of iodine (I2) therefore
the amount of iodine produced = 3 × 10.0 × Miodate mM = 30.0 × Miodate mM

b) The amount of iodine remaining in the reaction mixture after the oxidation
of ascorbic acid
Let the molarity of potassium iodate back titrated = M ′iodate M

56
 This implies that the amount per cm3 of the iodate solution back titrated = M′iodate
mM
Volume of potassium iodate used = 10.0 cm3
The amount of potassium iodate back titrated = 10.0 × M ′iodate mM
As each mole of potassium iodate provides three moles of iodine (I2) therefore
the amount of iodine left (or back titrated)
= 3 × 10.0 × M′iodate mM = 30.0 × M ′iodate mM
• The amount of iodine used for the oxidation of 10.0 cm3 solution of
ascorbic acid = 30.0 (Miodate − M ′iodate ) mM
• The amount of iodine used for the oxidation of 1.0 cm3 solution of
ascorbic acid = [30.0 (Miodate – M ′iodate )] / 10 mM
= [3.0 (Miodate – M ′iodate )] mM
Therefore the molarity of the ascorbic acid solution = [3.0 (Miodate – M ′iodate )] M
The amount of ascorbic acid per litre = Molarity × molar mass
= [3.0 (Miodate – M ′iodate )] M × 176.1 g mol−1
= [3.0 (Miodate – M ′iodate )] × 176.1 g dm−3
As the vitamin C tablet was dissolved to make 500 cm3 of solution, we need the
amount of ascorbic acid in 500 cm3.
The amount of ascorbic acid in 500 cm3 of the solution =
[1.5 (Miodate – M ′iodate )] × 176.1 g
= [264.15 (Miodate – M ′iodate )] g
Substituting the values of the molarities of standard and back titrated potassium iodate
respectively in the expression we get, the amount of ascorbic acid in the given tablet
of Vitamin C =….g

[ Compare the result with the amount marked on the strip of the vitamin tablet]

7.7 RESULT
The amount of ascorbic acid in the given tablet of Vitamin C =….g

57