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Vitamin C
Vitamin C
Harold
LEARNING OBJECTIVES
The objectives of this experiment are to...
1. prepare a solution of potassium iodate with a precisely known concentration, using primary
standard KIO 3 (s).
2. prepare a solution of sodium thiosulfate and standardize it by titration with portions of the above
potassium iodate solution.
3. use the iodate and thiosulfate solutions to analyze a vitamin C tablet to determine how many mg
of ascorbic acid it contains.
BACKGROUND
Many analytical methods are based on the redox properties of the iodide ion. In iodometric
titrations, excess iodide ion is added to the substance to be analyzed. The iodide ion acts as a reducing
agent and is itself oxidized to iodine. The iodine so produced is then titrated with standard sodium
thiosulfate solution (Na 2 S 2 O 3 ).
In this experiment, potassium iodate (KIO 3 ) is used to standardize the Na 2 S 2 O 3 . When
potassium iodide is added to potassium iodate, the following net ionic reaction occurs:
IO 3 + 5 I + 6 H+
3 I2
+ 3 H2O
Potassium iodide is added in excess so the iodate ion, IO 3 , is the limiting reactant and, therefore,
determines the amount of I2 produced. The I2 formed reacts with excess iodide ion to form the tri-iodide
ion, I3 , which is then titrated with sodium thiosulfate, Na 2 S 2 O 3 . The net ionic equations for these
reactions are as follows:
I2
+ I
2 S 2 O 3 2 + I3
I3
S 4 O 6 2 + 3 I
There are three parts to this experiment. The first is preparation of an approximately 0.07 M
solution of Na 2 S 2 O 3 and preparation of a 0.02 M solution of KIO 3 whose molarity is accurately known
(0.02xxx M). The second part is the standardization of the Na 2 S 2 O 3 solution using the known KIO 3
solution. The final part involves the use of both solutions to analyze a vitamin C tablet to determine its
ascorbic acid content.
The vitamin C analysis is based on the fact that I3 oxidizes ascorbic acid as follows:
ascorbic acid
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Chemistry 163
Harold
A known amount of iodate, IO 3 , is added to excess iodide ion, I, producing a known amount of
I3 , which then reacts with the ascorbic acid in the vitamin C tablet. The amount of I3 that does not
react with the ascorbic acid is then titrated with the standard Na 2 S 2 O 3 . From the data obtained, the
amount of ascorbic acid originally present can be determined.
Chemistry 163
Harold
Chemistry 163
Harold
up!).
3. Add approximately 2 g of KI to the mixture.
4. Pipet 25.00 mL of standard iodate solution into the flask. Swirl the flask to ensure complete mixing of
the contents.
5. Immediately titrate this mixture with your standardized sodium thiosulfate solution as described in
step 4 of the standardization procedure. Note that less sodium thiosulfate will be used because of the
partial consumption of tri-iodide ion by the ascorbic acid.
Some brands of vitamin C tablets use starch as the binder and this starch will also act as an
indicator, giving the solution an initial blue color. If this occurs, add the indicator starch anyway (but
less is OK). Make this addition when the original blue color is somewhat faded (the exact point is not
critical). Also, the binder starch particles tend to irreversibly retain a small amount of tri-iodide ion and
will appear dark at the end-point. This effect can be ignored, but is one of the reasons we can only
expect 3 S.F. accuracy in the weight of the Vitamin C determination.
6. Calculate the milligrams of ascorbic acid found in your tablet. Your result should be considered valid
to 3 significant figures. Complete the analysis in triplicate (3x) for in this experiment. If any
problems were encountered, such a overshooting an end-point, you should do another sample. The pill
is such that the results should yield ~100 mg of ascorbic acid as indicated by the manufacturer.
7. The reason for weighing the pill before and after grinding is that you likely will not be able to recover
100% of the powder. By dividing powder weight by pill weight you will have an accurate measure of
the fraction of the pill you will actually titrate. This fraction divided into the actual mass of Vitamin C
determined by titration will standardize the Vitamin C mass to what it would have been if 100% of
the pill had been used. Thus, we can determine the validity of the manufacturers claim that each pill
contains 100 mg of Vitamin C.
Recommended strategy
The lab day prior to the beginning of this lab (Day 0) you will (1) boil the deionized water and
prepare your solution of sodium thiosulfate; (2) dry the sample of pure KIO 3 and prepare its standard
solution. Two periods have been allotted for the remainder of this experiment. It is recommended that
during the first period you do the following: begin the standardization titrations, using these prepared
solutions. The end-point in this titration is tricky, so some experience with it prior to collecting real data
is helpful (that is, do at least one practice titration). You likely will not complete the three
standardization titrations in the first period.
In the second day then will be the completion of the three standardization titrations (if not
accomplished) and the three vitamin C pill analyses titrations should also be done as described in the
procedure.
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