Scribd
Upload
3K views

Assay of Ascorbic Acid by Iodometry

1) The document describes the iodometric titration method for determining ascorbic acid concentration. Ascorbic acid reduces iodine which is generated in situ from potassium iodate and potassium iodide. 2) Excess iodine is then back titrated with sodium thiosulphate using starch indicator. The amount of iodine reacted with ascorbic acid is used to calculate the concentration of ascorbic acid. 3) The procedure involves preparing standard solutions of potassium iodate and sodium thiosulphate, and then titrating an ascorbic acid sample solution against the iodine generated, with the excess iodine back-titrated to determine the

Uploaded by

Moona Sonika
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as DOCX, PDF, TXT or read online on Scribd
3K views

Assay of Ascorbic Acid by Iodometry

1) The document describes the iodometric titration method for determining ascorbic acid concentration. Ascorbic acid reduces iodine which is generated in situ from potassium iodate and potassium iodide. 2) Excess iodine is then back titrated with sodium thiosulphate using starch indicator. The amount of iodine reacted with ascorbic acid is used to calculate the concentration of ascorbic acid. 3) The procedure involves preparing standard solutions of potassium iodate and sodium thiosulphate, and then titrating an ascorbic acid sample solution against the iodine generated, with the excess iodine back-titrated to determine the

Uploaded by

Moona Sonika
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as DOCX, PDF, TXT or read online on Scribd
You are on page 1/ 5

Assay of Ascorbic Acid by Iodometry

Principle:
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.

In the presence of excess iodide, dissolved iodine exists primarily as the triiodide ion.

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.

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 colour of starch-iodine complex. 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)
Apparatus:
Volumetric flask, Burette, Pipette, Weighing bottle with clamp, Conical flasks, Funnel,
Beakers
Chemicals:
Vitamin C tablets, Potassium iodate, Potassium iodide, Sodium thiosulphate,
Sulphuric acid, Sodium carbonate, Starch

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.
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)
Preparation of 0.1 N Potassium Iodate:
IO3- + 6e- + 6H+--------------- I- + 3H2O
Therefore, KIO3= 6e-
Molecular weight of KIO3 is: 214 gm/mole
Therefore, the equivalent weight of KIO3= 214/6 = 35.6
So 35.6 gm of KIO3 is required for the preparation of 1 N KIO3
 3.56 gm of 0.1 N for 1000 ml of KIO3
 0.356 gm of 0.1 N for 100 ml of KIO3
Weigh accurately about 356 mg of KIO3 and dissolve in 100 ml distilled water
Normality of KIO3= weight taken
___________ * 0.1 N
Required weight
Preparation of 0.1 N Sodium thiosulphate:
2S2O32- ----------------- S4O62- + 2e-
Two thiosulphate (S2O32) ions are transformed to tetrathionate (S4O62) ion in the Redox
reaction by the loss of two electrons. Therefore, the equivalent weight of Sodium thiosulphate
is equal to its molecular weight, 248.18.
Therefore, Na2S2O3. 5H2O= e-
Molecular weight of Na2S2O3.5H2O is= 248.18 g/mol.
Therefore, the equivalent weight of Na2S2O3. 5H2O = 248.18 /1 = 248.18.
So 248.18 gm of Na2S2O3. 5H2O is required for the preparation of 1 N Na2S2O3. 5H2O
 24.8 gm ------- 0.1 N --------for 1000 ml of Na2S2O3. 5H2O
 2.48 gm --------0.1 N --------for 100 ml of Na2S2O3. 5H2O
Take 24.8 g of sodium thiosulphate (Na2S2O4.5H2O) and dissolve in 200 ml of distilled water
in a volumetric flask, and properly mix it. Once it has completely dissolved, make up the
volume to 1000 ml.
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 800 C for about 5
minutes. The solution and is then allowed to cool to room temperature.
c. Standardisation of 0.1N sodium thiosulphate:
Take 10 ml of Potassium Iodate solution and pour into an iodine flask. Add 2 gm of Potassium
Iodide and 5 ml of dilute H2SO4, keep it in dark for 10 minutes, add 2 to 3 drops of starch
indicator and titrate with sodium thiosulphate using starch solution as indicator until the blue
colour is disappeared.
 To get accurate results, repeat the titration three times.
 Properly record the readings of the burette.
Take their mean and calculate the normality of sodium thiosulphate solution

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.

You might also like