Project 3:

Determination of Vitamin C (Ascorbic Acid) in Juices by Titrimetric Method

Cokie Gaich and Taylor Hammond

Methods
Standardization of Sodium Thiosulfate
A 200 mL solution of 0.1M sodium thiosulfate was prepared. A 200 mL of 1M
hydrochloric acid aqueous solution and a 200 mL 0.1M potassium iodide solution was prepared.
A burette was filled with 0.1M sodium thiosulfate solution. 0.1g of potassium iodate was
weighed into five beakers and the actual weight of potassium iodate used was recorded for each
beaker. When ready for the titration, 10 mL of 1M hydrochloric acid and 10 mL of potassium
iodate was added to the beaker. The solution was titrated to a light yellow color. One spray of
spray starch (Faultless® Professional Formula Heavy Starch) was added to the solution to obtain
a blue-black color. The solution was titrated to colorless. The volume of sodium thiosulfate used
was recorded and the concentration calculated.

Standardization of Potassium Iodate

A 1 L solution of 0.002M potassium iodate and was prepared. A 200 mL solution of
0.001M aqueous solution from the standardized sodium thiosulfate was prepared by gravimetric
method. A burette was filled with the sodium thiosulfate solution. 10 mL of the 0.002 potassium
iodate was pipetted into five clean beakers, and when ready for the titration 10 mL of 1M
hydrochloric acid and 10 mL of 1M potassium iodide was added to the beaker. The solution in
the beaker was titrated to a light yellow color. One spray of spray starch (Faultless® Professional
Formula Heavy Starch) was added to the solution to obtain a blue-black color. The solution was
titrated further to colorless. The volume of sodium thiosulfate used for the titration was recorded
and the concentration of the potassium iodate solution was calculated.

Method Validation
In order to validate our method, we needed to spike a surrogate (Tropicana ® Trop50
with Calcium and Vitamin D) with an aqueous ascorbic acid solution whose known
concentration would allow us to titrate a certain volume of potassium iodate. In order to
accomplish this, we calculated the concentration of the ascorbic acid solution that would allow
us to titrate 5.75 mL of potassium iodate. 5.75 mL is 1.5x the average volume of potassium
iodate titrated for the unspiked sample, 3.83 mL. We calculated that we needed to add 0.01mL of
a 1.15M solution of ascorbic acid to each sample. We prepared three samples consisting of 10mL
of juice (Tropicana ® Trop50 with Calcium and Vitamin D), 75mL of distilled water, 2.5mL of
0.1M potassium iodide, 2.5mL of 1M hydrochloric acid, and 0.5mL of starch indicator solution
and spiked each one with the calculated volume needed of the ascorbic acid solution.
 Gaich/Hammond 2

Data

Table 1: Standardization of Sodium Thiosulfate:

Replicate Number
1 2 3 4 5 Average
Mass of
KIO3 used 0.1003 0.1015 0.1003 0.0985 0.1021 0.10054
(g)
Moles of
4.687x10-4 4.743x10-4 4.687x10-4 4.603x10-4 4.771x10-4 4.698x10-4
KIO3 used
Volume of
Sodium
14.1 17 16.2 15.4 18.9 16.32
Thiosulfate
used (mL)
Conc. of
Sodium
0.1994 0.1674 0.1736 0.1793 0.1515 0.1742
Thiosulfate
(M)
Standard
Deviation
Of Sodium 0.01752
Thiosulfate
Conc.

Five replicate titrations were complete for the standardization of sodium thiosulfate (see Table
1). The average mass of potassium iodate used was 1.0054g and the average volume of sodium
thiosulfate used in the titration was 16.32 mL. Therefore the average concentration of sodium
thiosulfate was 0.1742M with a standard deviation of 0.01752M. The average accuracy for the
standardization of sodium thiosulfate is 87.1% with an RSD of 10.1%.
 Gaich/Hammond 3

Table 2: Standardization of Potassium Iodate:

Replicate Number
1 2 3 4 5 Average
Concentration of 0.001 0.001 0.001 0.001 0.001 0.001
Sodium
Thiosulfate (M)
Volume of 111.5 124 124.6 117 114 118.22
Sodium
Thiosulfate used
(mL)
Volume of KIO3 10 10 10 10 10 10
used (mL)
Concentration of 0.0018583 0.0020667 0.00208 0.00195 0.0019 0.001971
KIO3 (M)
Standard 9.90237E-
Deviation Of 05
KIO3
Concentration

Five replicate titrations were completed for the standardization of potassium iodate (see Table 2).
The average volume of 0.001M sodium thiosulfate used was 118.22 mL. The average
concentration of potassium thiosulfate was 0.00197M with a standard deviation of 9.90 x 10-5M.
The average accuracy for the standardization of potassium iodate is 98.6% with an RSD of
5.02%.

Table 3: Vitamin C Method Validation

Volume of KIO3 used (mL)

Average
Standard
1 2 3 volume used
Deviation
(mL)
Unspiked 3.95 3.85 3.7 3.83 0.126
1.15M
Ascorbic
5.8 5.85 5.8 5.82 0.0289
Acid
Spike
Moles
Ascorbic
2.30E-05
Acid of
Unspiked
Moles of Average
3.48E-05 3.51E-05 3.48E-05
spiked accuracy
Accuracy 34.3 35.1 34.3 34.6
 Gaich/Hammond 4

The volumes of potassium iodate needed to titrate to a purple-black color were 5.80 mL, 5.85
mL, and 5.80 mL respectively, with an average of 5.82 mL. The average accuracy for the method
validation was 34.6% with an RSD of 0.0835%.

Sources of Error

The experiment of standardization of both the sodium thiosulfate solution and potassium
iodate solution has an average of 0.174M and 0.00197M respectively. One source of error could
have occurred when the burette wasn’t read properly after each volume was measured and
another source of error could be when determining the endpoint for the titrations as this was
determined qualitatively rather than quantitatively which could have led to overshooting the
titration. Error for method validation could have resulted from human error (reading the
instrument wrong, over-titrating, etc.), or instrument error. Overall, we had good results, with
accuracies of 87.1% and 98.6% respectively, and RSDs of 10.1% and 5.02% respectively. These
accuracies and RSDs indicate we have good accuracy and precision, which helps to validate our
method. A possible improvement for this experiment would be to use a colorimeter to determine
the endpoint of the titration quantitatively.