EJ Habina Quantitative Anal. Lab MW 2:00 Experiment 5: Iodimetric Determination of Vitamin C Purpose: The purpose of this experiment is to determine the manufacturer’s claim for the specifications of a source of Vitamin C are correct or not. We will determine the validity of the claims through determining the content of ascorbic acid (vitamin C) in an unknown sample and compare that to the known content in a supplemental source. Procedure: 1. Standardization of Thiosulfate Solution: a. As a group, a starch indicator as well as 0.07 M sodium thiosulfate (approx. 8.7 g in 500 mL boiled water w/ 0.05 g sodium carbonate) solution. Another solution of 0.01 M KIO3 was made using 1 g of solid reagent and dissolving in 500 mL flask. The thiosulfate was then standardized by pipetting 50 mL of KIO3 into an Erlenmeyer with 2 g solid KI and 10 mL of 0.5 M sulfuric acid and titrated until solution lost all of its color. 2 mL of starch indicator was then added to each and the titration is repeated. 2. Analysis of Vitamin C: a. A sample of ascorbic acid required for a 30 mL titration is weighed and then dissolved into 50 mL of 0.3 M H2SO4. 2 g of KI and 50 mL of standard KIO3 is added and the sample was then titrated as before until endpoint. This procedure was then repeated again for a vitamin C tablet. Reactions: ๐ผ๐3− + 8 ๐ผ + 6 ๐ป + → 3 ๐ผ3− + 3 ๐ป2 ๐ ๐ผ3− + 2 ๐2 ๐3−2 → 3 ๐ผ − + ๐4 ๐6−2 ๐ถ6 ๐ป8 ๐6 + ๐ผ3− + ๐ป2 ๐ → ๐ถ6 ๐ป8 ๐7 + 3 ๐ผ − + 2 ๐ป + Data: Mass of KIO3 = 1.0116 g Mass of Thiosulfate = 8.7049 g Mass of Na2CO3 = 0.0548 g Standardization of Thiosulfate Solution: Trial # 1 2 3 KI (g) 2.0290 2.0022 2.0101 Thiosulfate Added (mL) 36.50 40.31 39.75 Average Molarity of Thiosulfate Solution 0.0777 0.0703 0.0714 0.07313 Analysis of Vitamin C: Ascorbic Acid w/ Sulf. Acid Trial # Ascorbic Acid (g) 1 KI (g) 0.1871 Thiosulfate Added (mL) Wt. % of Ascorbic Acid 2.0052 12.40 90.85% KI (g) 2.0900 2.0220 2.0042 Thiosulfate Added (mL) 14.8 14.8 14.9 Wt. % of Vitamin C 82.32% 82.32% 82.32% KIO3 & KI w/ Thiosulfate Trial # 1 2 3 Vitamin C (g) 0.1878 0.1875 0.1874 Calculations: Molarity of KIO3: ๐๐๐ ๐ ๐พ๐ผ๐3 × Ex: 1.0116 ๐ ๐พ๐ผ๐3 × 1 ๐๐๐ ๐พ๐ผ๐3 1 × = ๐ ๐พ๐ผ๐3 214.00 ๐ 0.05 ๐ฟ 1 ๐๐๐ ๐พ๐ผ๐3 1 × = 0.009454 ๐ ๐พ๐ผ๐3 214.00 ๐ 0.05 ๐ฟ Molarity of Sodium Thiosulfate: ๐ ๐พ๐ผ๐3 × 0.05 ๐ฟ × Ex: 0.009454 ๐ × 0.05 ๐ฟ × 3 ๐๐๐ ๐ผ3 1 ๐๐๐ ๐โ๐๐. 1๐ × × = ๐ ๐โ๐๐๐ ๐ข๐๐๐๐ก๐ 1 ๐๐๐ ๐ผ๐3 1 ๐๐๐ ๐ผ3 ๐โ๐๐. ๐ด๐๐๐๐ 3 ๐๐๐ ๐ผ3 1 ๐๐๐ ๐โ๐๐. 1๐ × × = 0.0777 ๐ ๐โ๐๐๐ ๐ข๐๐๐๐ก๐ 1 ๐๐๐ ๐ผ๐3 1 ๐๐๐ ๐ผ3 0.0365 ๐ฟ Amount of Ascorbic Acid Required: 1 ๐๐๐ ๐ผ3− 1 ๐๐๐ ๐ด๐ ๐๐๐๐๐๐ ๐ด๐๐๐ 176.12592 ๐ ๐ ๐โ๐๐๐ ๐ข๐๐๐๐ก๐ × 0.03 ๐ฟ × × × − 2 ๐๐๐ ๐โ๐๐. 1 ๐๐๐๐ ๐ผ3 1 ๐๐๐ ๐ด๐ ๐๐๐๐๐๐ ๐ด๐๐๐ = ๐ ๐ด๐ ๐๐๐๐๐๐ ๐ด๐๐๐ Ex: 1 ๐๐๐ ๐ผ3− 1 ๐๐๐ ๐ด๐ ๐๐๐๐๐๐ ๐ด๐๐๐ 176.12592 ๐ × × − 2 ๐๐๐ ๐โ๐๐. 1 ๐๐๐๐ ๐ผ3 1 ๐๐๐ ๐ด๐ ๐๐๐๐๐๐ ๐ด๐๐๐ = 0.18757 ๐ ๐ด๐ ๐๐๐๐๐๐ ๐ด๐๐๐ 0.07313 ๐ × 0.03 ๐ฟ × Weight % of Ascorbic Acid (also for Vitamin C): ๐ฟ ๐โ๐๐. ๐ด๐๐๐๐ ๐ ๐โ๐๐. 1 ๐๐๐ ๐2 ๐3 1 ๐๐๐ ๐ผ3 × × × = ๐๐๐๐๐ ๐ผ3 1 1 1 ๐๐๐ ๐โ๐๐. 1 ๐๐๐ ๐2 ๐3 ๐ ๐พ๐ผ๐3 × 0.05 ๐ฟ × 3 ๐๐๐ ๐ผ3 = ๐๐ฅ๐๐๐ ๐ ๐๐๐๐๐ ๐๐ ๐ผ3 1 ๐๐๐ ๐พ๐ผ๐3 ๐๐ฅ๐๐๐ ๐ ๐๐๐๐๐ ๐๐ ๐ผ3 − ๐๐๐๐๐ ๐ผ3 = ๐๐๐๐๐ ๐ผ3 ๐๐๐๐๐๐๐๐๐ ๐๐๐๐๐ ๐ผ3 ๐๐๐๐๐๐๐๐๐ × 1 ๐๐๐ ๐ด๐ ๐๐๐๐๐๐ ๐ด๐๐๐ 176.1256 ๐ × = ๐ ๐ด๐ ๐๐๐๐๐๐ ๐ด๐๐๐ 1 ๐๐๐ ๐ผ3 1 ๐๐๐ ๐ด๐ ๐๐๐๐๐๐ ๐ด๐๐๐ ๐ ๐๐ ๐ด๐ ๐๐๐๐๐๐ ๐ด๐๐๐ × 100 = ๐๐ก. % ๐๐๐ ๐ ๐๐ ๐ ๐๐๐๐๐ Ex (using Trial 1 data): 0.0124 ๐ฟ 0.07313 ๐ 1 ๐๐๐ ๐2 ๐3 1 ๐๐๐ ๐ผ3 × × × = 0.000453 ๐๐๐๐๐ ๐ผ3 1 1 1 ๐๐๐ ๐โ๐๐. 1 ๐๐๐ ๐2 ๐3 0.009454 ๐ ๐พ๐ผ๐3 × 0.05 ๐ฟ × 3 ๐๐๐ ๐ผ3 = 0.001418 ๐๐ฅ๐๐๐ ๐ ๐๐๐๐๐ ๐๐ ๐ผ3 1 ๐๐๐ ๐พ๐ผ๐3 0.001418 ๐๐ฅ๐๐๐ ๐ ๐๐๐๐๐ ๐๐ ๐ผ3 − 0.000453 ๐๐๐๐๐ ๐ผ3 = 0.000965 ๐๐๐๐๐ ๐ผ3 ๐๐๐๐๐๐๐๐๐ 1 ๐๐๐ ๐ด๐ ๐๐๐๐๐๐ ๐ด๐๐๐ 176.1256 ๐ × 1 ๐๐๐ ๐ผ3 1 ๐๐๐ ๐ด๐ ๐๐๐๐๐๐ ๐ด๐๐๐ = 0.16997 ๐ ๐ด๐ ๐๐๐๐๐๐ ๐ด๐๐๐ 0.000965 ๐๐๐ ๐ผ3 × 0.16997 ๐ ๐๐ ๐ด๐ ๐๐๐๐๐๐ ๐ด๐๐๐ × 100 = 90.85 % 0.1871 ๐ Claimed Manufacturer Wt. %: 0.25 ๐ก๐๐๐๐๐ก × ๐๐๐ ๐ ๐๐ ๐ก๐๐๐๐๐ก × 0.25 ๐ก๐๐๐๐๐ก × 0.52 ๐ × 1 × 100 = ๐๐ก. % 0.303 ๐ 1 × 100 = 42.9 % 0.303 ๐ Conclusion: The purpose for this experimental procedure was to determine the content of both commercial Vitamin C tablet as well as reagent grade ascorbic acid. After completing the procedure, the results for the amount of reagent grade ascorbic acid was calculated to be 90.85 %, which is a desired value due to the assumed purity of a reagent grade chemical. As for the accuracy of the commercial vitamin C tablet results, the value of 82.3 % from the data in this procedure was much higher than the calculate manufacturer claimed weight percent of 42.9 %. As for the particles that did not dissolve, they are what are known as fillers. These act as a supplemental substance in tablets so that the tablet can reach a desired size, weight, etc.