Determination of Ascorbic Acid Determination of Ascorbic Acid in Vitamin C Tablet

Objective
Using a redox titration titration to determine determine the vitamin C (ascorbic acid) in a commercial
tablet. The purpose of this lab was to determine the amount of ascorbic acid in a 200 mg sample of Vitamin
C tablets by starch/ iodine reaction. The back titration and iodometry is applied to overcome various
constraints under the experiment conditions.

Introduction
Vitamin C, is one of the more abundant and easily obtained vitamins in nature. It is a colorless, water‐
soluble acid that, in addition to its acidic properties, It is powerful biochemical reducing agent, meaning it
readily undergoes oxidation, even from the oxygen in the air. In this experiment, the reducing properties of
ascorbic acid were used to analyze its concentration in commercial vitamin C tablets.
In the determination of ascorbic acid, KIO3 methods employ a back titration with a standard
thiosulfate solution of the excess I2 generated by adding a precisely known amount of a primary standard
KIO3 solution to an ascorbic acid solution.
A starch indicator is a special type of visual indicator that is employed in redox titrations that have
iodine as the titrant or the analyte.

I. Safety Precautions when handling chemicals

HCl and H2SO4, in high concentration, is a very strong acid that can cause chemical burns and will
damage clothing. It should be handled with extra care. Spillage of HCl or H2SO4 onto body and eyes could
cause serious injury. Immediate washing with water should be carried in cases of body contact.

Iodine stains both skin and clothing so proper care is advised. If staining does occur, alcohol may
remove skin stains and cleaners are available for fabric stains.

II. Materials
1. potassium iodide (KI) powder
2. KIO3 powder
3. Na2S2O3 ∙5H2O powder
4. H2SO4 (18 M) solution
5. HCl (6M) solution
6. Starch indicator solution
7. Vitamin C Tablets * 2
8. Distilled water
9. Parafilm covers

III. Apparatus
1. 250 mL Erlenmeyer flasks
2. Beakers

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 3. Burette, Clamp and Stand
4. 200 mL volumetric flask
5. 100 mL volumetric flask
6. Pipette
7. 50 mL measuring cylinders

IV. Procedures
Preparation of a 0.1 N Sodium Thiosulfate Solution
1. weight 4.96 g of Na2S2O3 ∙5H2O.
2. Add distilled water and swirl until the solid has dissolved.
3. Transfer quantitatively to a 200 mL volumetric flask, dilute to the mark and mix thoroughly.

Preparation of 0.01 M KIO3 Preparation of 0.01 M KIO3 solution

1. Weigh approximately 0.4280 g (to the nearest 0.1 mg) of dried and cooled reagent grade KIO3.
2. Dissolve the KIO3 in about 50mL of distilled water.
3. Transfer quantitatively to a 200 mL volumetric flask, dilute to the mark and mix thoroughly.

Standardization of 0.10 N sodium thiosulfate Solution

1. Pipette 20.00 mL of the KIO3 solution into a 250 mL Erlenmeyer flask.
2. Add 30mL distilled water.
3. Add 1 g of solid KI until the solid has dissolved.
4. Add 2 mL HCl (6M).
5. Immediately titrate with the thiosulfate solution until the solution has lost its initial reddish brown color
and has become pale yellow.
6. Add 5 mL of starch indicator and complete the titration until blue color disappeared.
7. Calculate the concentration of the Na2S2O3 solution.

Preparation of a 0.5 M Preparation H2SO4

1. Take 2.8 mL of H2SO4 (18M).

2. Add 50mL distilled water to it.
3. Transfer quantitatively to a 100 mL volumetric flask, dilute to the mark and mix thoroughly.

Determination of Ascorbic Acid in Vitamin C tablets

1. Weigh two tablets to the nearest 0.1 mg.
2. Weigh vitamin C tablet 1 (about 2000 mg) Mark it as w1.
3. Weigh vitamin C tablet 2 (about 2000 mg) Mark it as w2.
4. Average the two vitamin C tablet weight ((w1+w2)/2).
5. Grind all of the tablets thoroughly using a clean mortar and pestle.
6. Transfer the ground powder to a clean, dry weighing bottle.
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 7. Weigh to the nearest 0.1 mg a 2.0000g vitamin C and quantitatively.
9. Transfer quantitatively to a 200.0 mL volumetric flask, dilute to the mark and mix thoroughly.
10. Transfer 20 mL Vitamin C solution to a 250 mL Erlenmeyer flask.
11. Add sample 20 mL of 0.5M H2SO4 and 20 mL of water. Some solid binding material in the tablet
formulations may not dissolve completely.
12. Add approximately 2 g KI and exactly 50.00 mL of standard KIO3 to 3 each sample and using parafilm
cover flask mouth.
13. Immediately titrate with thiosulfate until the solution has lost its initial reddish ‐brown color and has
become pale yellow although it may be difficult to see these colors with other components of the tablets.
14. Add 5 mL of starch indicator and complete the titration.
15. calculate the ascorbic acid content (mg/tablet).

V. Results

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 VI. Discussions

Ascorbic acid (Vitamin C) is a relatively cheap, structurally simple, water soluble organic acid - best
known for being commonly found in citrus fruits such as oranges, limes, and lemons. There are other
natural sources for this substance, such as green vegetables and the edible buds of some flower species;
but it is commonly known that fruit juices are the most easily accessible source of this very important
nutrient.

It is a water soluble antioxidant that plays a vital role in protecting the body from infection and
disease. As it is not synthesised by the human body, therefore, it must be acquired from dietary sources.

Ascorbic acid has the chemical formula of C6H8O6 and molecular structure as follows:

In this experiment for determination of amount of ascorbic acid, we employ the method of iodometry.
Iodometry is usually used for determine the amount of oxidizing agents. In an iodometric titration, it is
based on the oxidation of iodide into iodine. The iodide ion acts as a reducing agent. The iodine so
produced is then titrated with standard sodium thiosulfate solution (Na2S2O3).

As what we would like to determine is the amount of the reducing agent Ascorbic acid, this
experiment also involves a back titration. We employ a back titration with a standard sodium thiosulfate
solution of the excess I2 generated by adding a precisely known amount of a primary standard KIO 3 solution
and excess KI solution to an ascorbic acid solution.

Generation of I2 is by mixing the KIO3 with KI. It is generated by adding an excess amount of KI to an
acidified solution of potassium iodate according to the following reaction:

IO3‐ (aq) + 6 H+(aq) + 5I‐ (aq) → 3 I2(aq) + 3 H2O(l)

Known amount In excess 

The KIO3 is the limiting agent while KI is in excess. Thus, the total number of mole of I2 generated in this
process can be calculated.

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 The I2 generated then undergo Redox reaction with vitamin‐C (C6H8O6) in which I2 is reduced while vitamin‐
C is oxidized:

C6H8O6 (aq) + I2 (aq) → C6H6O6 (aq) + 2I‐ (aq) + 2H+ (aq)

To be determined

The C6H8O6 is the limiting agent while I2 is in excess. After this reaction, there is some I2 remaining in the
solution. The number of mole of the remaining I2 can be determined by undergoing another Redox titration
with sodium thiosulfate in which I2 is reduced while sodium thiosulfate is oxidized:

I2 (aq) +2S2O32- (aq) → 2I‐ (aq) + S4O62- (aq)

 Known amount

A small amount of starch solution has been added to the solution for showing the end point in which all the
I2 (aq) in the solution is being reduced. The number of mole of the remaining I2 after the vitamin‐C Redox
reaction thus can be determined from the amount of S2O32- used.

Finally, we could do the calculation for the no of mole of I2 used in the reaction with vitamin C by:

Number of mole of I2 in  = Number of mole of I2 in  - Number of mole of I2 in 

Number of mole of vitamin C = Number of mole of I2 in 

You should remember that the I2 (aq) is actually in the form of the triiodide ions in the presence of excess KI
due to the following reaction:

I2 (aq) + I‐ (aq) I3‐ (aq)

In precise, the reaction of I2 (aq) +2S2O32- (aq) → 2I‐ (aq) + S4O62- (aq) should be rewrited as:

I3‐ (aq) + 2S2O32- (aq) → 3I‐ (aq) + S4O62- (aq)

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 VII. Discussions (In Q&A Format)
Question 1: What is the function of the starch solution? Why it has to be added only when the reaction
mitxure becomes pale yellow?
Answer:
Starch solution is added to the solution for showing the end point in which all the I2 (aq) in the solution
is being reduced.
Starch is partially decomposed by large excesses of iodine, so the starch is added only after most of
the I3− ion has been reduced.

Question 2: Why the titrations have to be carried out immediately after the addition of acid?
Answer:
Ascorbic acid is susceptible to oxidation by atmospheric oxygen over time. For this reason, the samples
should be prepared immediately before the titrations.

Question 3: Why solution of Na2S2O3 is generally stored in dark reagent bottle?

Answer:
The thiosulfate ion can decompose into the sulfite ion and a colloidal suspension of sulfur, which is
opaque. The equation for this reaction is as follows:
S2O32- (aq) → S O32- (aq) + S(s)
As the decomposition of thiosulfate is catalyzed by light, thus dark reagent bottle should be used.

Question 4: What is the difference between iodometry and iodimetry?

Answer:
When an analyte that is a reducing agent is titrated directly with a standard iodine solution, the
method is called "iodimetry". When an analyte that is an oxidizing agent is added to excess iodide to
produce iodine, and the iodine produced is determined by titration with sodium thiosulfate, the method is
called "iodometry".

Question 5: Describe how starch can be used for end point detection during an iodometric and iodimetric
titration. What the chemical basis for this means of end point detection.
Answer:
Starch is used as indicator. At the end point, the blue color of starch indicator disappears due to
change of iodine to iodide in both iodometric and iodimetric titration.
An iodide ion (I‐) has no reaction with starch, but iodine (I2, probably in the form of the linear I3‐ ion)
can insert itself into the helical structure of starch to form a complex that has an intense blue color. When
iodine reduced, the color would then disappear.

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 VIII. Conclusion

In conclusion, we have preformed the following: (1) Prepare a solution of potassium iodate with a
precisely known concentration, using primary standard KIO 3 ; (2) Prepare a solution of sodium thiosulfate
and standardize it by titration with portions of the above potassium iodate solution; and (3) use the iodate
and thiosulfate solutions to analyze a vitamin C tablet to determine how much ascorbic acid it contains.

The experiment result reveals that the ascorbic acid content in the Vitamin C Tablet is higher than the
amount stated (500 mg/ tablet) on the product description. This may due to the fact that the content is
actually higher than the specified one or from experiment errors. One of the possible errors is the molarity
of Na2S2O3 used is higher than the desired one. Another possible error is that the amount of KIO3 used is
more than the desired one. Both will lead to the exaggeration of the ascorbic acid content in the Vitamin C
Tablets tested.

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