Exp. 8 (Iodimetric Analysis For Vitamin C)

Exercise No.
8
Iodimetric Analysis for Vitamin C
Introduction
Vitamin C, known chemically as ascorbic acid, is an important component of a
healthy diet. Humans are one of the few members of the animal kingdom unable to
synthesize vitamin C, resulting in the need for regular ingestion in order to prevent the
malady called scurvy and to remain healthy. The National Academy of Sciences has
established the threshold of 60 mg/day for adults as the Recommended Dietary
Allowance (RDA). Linus Pauling, a chemist whose many contributions to chemical
bonding theory should be well-known to you, recommended a level of 500 mg/day to
help ward off the common cold. He also suggested that large doses of vitamin C are
helpful in preventing cancer.
The vitamin C content of foods can easily be determined by oxidizing ascorbic
acid, C6H6O6:
C6H8O6
C6H6O6 + 2H+ + 2eThis reaction is very slow for ascorbic acid in the dry state, but occurs readily when in
contact with moisture. A reagent that is particularly good for the oxidation is an aqueous
solution of iodine, I 2. Since iodine is not very soluble in water, we dissolve it in a
solution of potassium iodide, KI in which the I 2 exists mainly as I3-, a complex ion. The
reaction with ascorbic acid involves I2, which is reduced to I- ion.
2e- + I2
2I-
In the overall reaction, one mole of ascorbic acid requires one mole of I 2 for complete
oxidation. In fact, iodimetry is one of the most accurate of volumetric processes
When the red-colored I2 solution is added to the ascorbic acid solution, the
characteristic iodine color disappears because of the above reaction. Although we
could use the first permanent appearance of the yellow color of dilute iodine to mark the
endpoint of the titration, better results are obtained when starch is added as an
indicator. Starch reacts with I2 preferentially with ascorbic acid, and so its concentration
remains very low until the ascorbic acid is all oxidized. At that point, the I 2 concentration
begins to go up and the reaction with the indicator occurs.
I2 + starch
yellow
starch I2 complex
blue
Because an I2 solution cannot be prepared accurately by direct weighing, it is

necessary to standardize the I 2 against a reference substance of known purity. We will
use pure ascorbic acid for this reference, or primary standard. After standardization you
can use the iodine solution for the direct determination of vitamin C in any kind of
sample.
Objectives
1. To prepare and standardize an iodine solution;
2. To analyze an unknown sample containing vitamin C through titration method.
Materials
aluminum foil
ascorbic acid
analytical balance
buret
250-mL Erlenmeyer flasks
used carbon paper
distilled water
1-L volumetric flask
solution container
400-mL beaker
I2 crystals
starch indicator
iron stand and buret clamp
wash bottle
funnel
filter paper
Procedure
A. Standardization of the iodine solution
Obtain from the stockroom a buret and an unknown vitamin C sample. Weigh
out accurately on the analytical balance three ascorbic acid samples of
approximately 0.10 g into clean 250-mL Erlenmeyer flasks Dissolve each sample in
about 100 mL of water.
Clean the buret thoroughly. Weigh about 10-20 grams of I 2 crystals in a 400
mL beaker and add approximately 150 mL of distilled water. Stir thoroughly and
cover with a piece of aluminum foil. Rinse the buret with a few milliliters of the I 2
solution three times. Drain and then fill the buret with the I 2 solution.
Take the initial reading of the buret, add 1 mL of starch indicator to the first
ascorbic acid sample and titrate with the iodine solution. Note the change of the I 2
color as you swirl the flask gently and continuously during the titration. Continue
adding the iodine solution, using progressively smaller volume increments, until the
sample solution just turns a distinct blue. After reading the buret, titrate the other
two samples being sure to add the starch indicator and to read your buret before and
after each titration.
B. Analysis of an unknown containing Vitamin C
Given your experience with the standardization process, devise an analogous
procedure to determine the vitamin C content of your unknown sample. You will
need to select a sample size, and you may need to carry out an initial treatment of
the sample. For example, if your instructor assigns you a fruit juice sample, it is but
desirable to first filter the sample through cheese cloth, followed by rinsing of the
filter with water.
It may be helpful in choosing the sample sizes to calculate an iodine solution
parameter called the titer-the number of mg of ascorbic acid which reacts with 1 mL
of iodine solution. This number is easily found from the I 2 concentration and the
mass relationship in the reaction. It is desirable to have the volume of I 2 for each
titration be at least 15 mL. Using a small initial sample will give you an indicator of
how much to scale up for your final titrations.
Report your results in percent vitamin C, if a solid sample is used. For liquid
samples, report mg of vitamin C per 100 mL. In each case, calculate the sample
size required to give the RDA of vitamin C.
C. Disposal of Reaction Products
All reaction products may be diluted with water and poured down the drain.
Questions
1. Write a balanced equation for the reaction between I 2 and ascorbic acid. Identify
the oxidizing agent and the reducing agent.
2. A solution of I2 was standardized with ascorbic acid. Using a 0.100 g sample of
pure ascorbic acid, 25.32 mL of I2 were required to reach the starch end point.
(a) What is the molarity of the iodine solution? (b) What is the titer of the iodine
solution?
3. A sample of fresh grapefruit juice was filtered and titrated with the above I 2
solution. A 100-mL sample of the juice took 9.85 mL of the iodine solution to
reach the starch end point. (a) What is the concentration of vitamin C in the juice
in mg vitamin C/100 mL of juice? (b) What quantity of juice will provide the RDA
amount of vitamin C?
Data and Calculation

A. Standardization of Iodine Solution
Sample
Mass of Ascorbic acid sample, g
Moles of Ascorbic acid (MM = 176 g)
Initial buret reading, mL
Final buret reading, mL
Volume of I2 added, mL
Moles of I2 consumed
Molarity of I2, mol/L
Titer of I2, mg Asc/mL I2
I
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II
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III
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B. Analysis of an unknown containing Vitamin C

Sample
Mass or volume of unknown
Initial buret reading, mL
Final buret reading, mL
Moles of iodine added
Moles of vitamin C in sample
Mass of vitamin C in sample, mg
Percent vitamin C in solid sample
Conc of vitamin C in liquid sample, mg/100 mL
RDA, mL or mg
I
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II
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III
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Exercise No.

Because an I2 solution cannot be prepared accurately by direct weighing, it is

Data and Calculation

B. Analysis of an unknown containing Vitamin C

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