Chemistry 1156 Chemistry of Vitamin C Purpose In this experiment, you will observe the oxidation-reduction reaction that takes place between vitamin C (ascorbic acid, C6H8O6) and iodine, wherein vitamin C is the reducing agent and iodine is the oxidizing agent. One objective of this experiment is to use the quantitative redox titration to determine the amount of ascorbic acid in a commercial vitamin C tablet. Introduction While the importance of vitamin C in preventing scurvy was recognized as early as 1795 by the British Navy, it was not until 1928 that ascorbic acid was isolated and identified as the vital anti-scurvy factor. Since that time, vitamin C consumption has also been attributed to prevention of the common cold. Vitamin C is one of the water-soluble vitamins, capable of significant hydrogen bonding with water. Because it is watersoluble, vitamin C is continually excreted from the body, unlike the fat-soluble (nonpolar) vitamins which are stored in the body’s fat deposits. As a result, the body’s supply of vitamin C must continually be replenished through ingestion of foods high in vitamin C and vitamin supplements. Since excess vitamin C is rapidly excreted in the urine, there is little risk in consuming more vitamin C than required by the body. This experiment takes advantage of ascorbic acid’s watersolubility and strong reducing ability to quantitatively determine the amount of ascorbic acid present in a commercially available vitamin C tablet. In particular, ascorbic acid’s ability to reduce iodine to the iodide ion will be exploited to determine the amount of vitamin C present in the sample. Following the procedure of R. W. Ramette (R. W. Ramette, Chemical Equilibrium and Analysis, 1981), iodine will be produced in solution through the reaction of iodide ion with iodate ion in acidic solution. To this end, our experiment combines solid potassium iodide (KI), hydrochloric acid, and starch solution with the solution of ascorbic acid. This solution is titrated with potassium iodate, (KIO3), which reacts with the iodide ion as follows: IO3–(aq) + 5 I–(aq) + 6 H+(aq) 3 I2 + 3 H2O Eqn. 1 As quickly as the iodine is produced, it is reduced back to iodide ion by the ascorbic acid (equation 2, below). When all of the ascorbic acid has been oxidized, the iodine concentration will increase to the point where it will react with iodide ion to form the triiodide ion, I3– I2 + I– I3– Eqn. 3 The triiodide ion in turn combines with the starch to form the dark blue triiodide-starch complex. The appearance of this dark blue color signals the endpoint of the titration. MATERIALS Supplies: None Reagents: vitamin C tablets (cut in half), 0.03 M KIO3, solid KI, 1.0% starch solution, 1.0 M HCl (diluted from stock solution) 1|Page General Chemistry II Lab for Majors Chemistry of Vitamin C Procedure 1. Prepare 50-mL buret for redox titration of vitamin C. Rinse the buret 2–3 times with distilled water, making sure that the stop-cock and tip are both free of obstructions. Rinse the buret twice with 10–15 mL portions of 0.03 M KIO3 solution. After the buret has been rinsed thoroughly, fill the buret with the 0.03 M KIO3 solution. Read the initial volume of KIO3 solution to the nearest 0.01 mL and record this initial volume in your laboratory notebook. 2. Prepare vitamin C solution. Weigh ½ of a vitamin C tablet. Place this half tablet in a 125 mL Erlenmeyer flask and carefully crush the tablet with a glass stirring rod. Once the tablet is crushed, dissolve it in 50 mL of distilled water. Any undissolved material that remains after 2–3 minutes is inert binder material that does not need to dissolve. Rinse the stirring rod with a small amount of distilled water as you remove it from the vitamin C solution. To the vitamin C solution, add 1 gram of solid potassium iodide and 5 mL of 1.0 M HCl. Swirl the flask until all of the potassium iodide dissolves. Finally, add 1–2 drops of 1% starch solution. 3. Titration. Titrate the vitamin C solution with the potassium iodate (KIO3) solution until the dark blue color persists. As the redox titration reaches completion, excess iodine (I2) reacts with iodide ion (I–) to form the triiodide ion (I3–). Triiodide ion in turn reacts with starch, forming the dark blue starchtriiodide ion complex, signaling the endpoint of the titration. Record the final volume of titrant (in the buret) to the nearest 0.01 mL in your laboratory notebook. Each lab partner should conduct one titration until your values for the percentage of vitamin C per gram agree to within 10% of each other. In other words, if your first two titrations do not agree to within 10%, both students should repeat the titration a second time, striving for better accuracy. 4. Disposal. When you are finished with the experiment, all of the solutions may be flushed down the drain. 2|Page Chemistry 1156 Chemistry of Vitamin C Vitamin C Content of Commercial Tablets Data Trial 1 Trial 2 Mass of tablet Trial 3 Trial 4 g g g g mL mL mL mL Initial buret reading mL mL mL mL Net volume of 0.03 M KIO3 solution mL mL mL mL Volume of 0.03 M KIO3 Final buret reading Calculate the mass of vitamin C (ascorbic acid) present in each ½ tablet, taking into account the reaction stoichiometry shown in equations 1 and 2. Show a sample calculation in the space provided below. Data Mass of vitamin C Trial 1 mg Trial 2 Trial 3 mg Average mass mg Trial 4 mg mg Post-Lab Questions 1. Calculate the percent purity of ascorbic acid for each trial. Are the tablets pure ascorbic acid, or is there evidence that they contain some inert material? Record your observations made when dissolving the tablets, and compare the mass of the ½ tablet with the mass of vitamin C found in the tablet. mass C6 H 8O6 100 % purity mass of tablet 2. Sodium nitrite is used as a meat preservative. The amount of NO2– in a sample can be determined by acidifying the solution to form nitrous acid, HNO2, allowing the nitrous acid to react with an excess of iodide ion, and then titrating the triiodide ion (I 3–) in the resulting solution with thiosulfate solution in the presence of a starch indicator. The balanced equations are: 2 H+ + 2 HNO2 + 3 I– → 2 NO + I3– + 2 H2O I3– + 2 S2O32– → 3 I– + S4O62– When a nitrite containing sample with a mass of 3.000 g was analyzed, 16.65 mL of 0.1500 M Na 2S2O3 solution was required to completely titrate the sample. What is the mass percent of NaNO2 in the sample? 3|Page
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