Chemistry 232 Determination of Vitamin C by an Iodometric Titration

Purpose: The goal of this lab is to determine the concentration of vitamin C in juices and Real Lemon.
A redox titration, involving an iodometric method, will be used to do the analysis. The samples will be classified by their Vitamin C content.

Introduction: Although most mammals can synthesize vitamin C, or ascorbic acid (C6H8O6), from
sugars, man must ingest considerable quantities of this substance. The National Academy of Sciences recommends the consumption of 60 mg of ascorbic acid per day. Vitamin C deficiency, which typically causes abnormalities in bones and teeth, was first characterized in sailors in the eighteenth century. These abnormalities were eliminated by compelling sailors to eat limes, a source of vitamin C. Many vegetables also contain large quantities of vitamin C, but ascorbic acid is commonly destroyed by many cooking processes, and hence citrus fruits are regarded as the most reliable source of vitamin C. Vitamin C can be determined in food by use of an oxidation-reduction reaction. The redox reaction is preferable to an acid-base titration because a number of other species in juice can act as acids, but relatively few interfere with the oxidation of ascorbic acid by iodine. The solubility of iodine is increased by complexation with iodide to form triiodide: I2(aq) + I- I3Triiodide then oxidizes vitamin C to dehydroascorbic acid: C6H8O6 vitamin C + I3- + H2O C6H6O6 + 3I- + 2H+ dehydroascorbic acid (2) (1)

The endpoint is indicated by the reaction of iodine with starch suspension, which produces a blue-black product. As long as vitamin C is present, the triiodide is quickly converted to iodide ion, and no blue-black iodine-starch product is observed. However, when all the vitamin C has been oxidized, the excess triiodide (in equilibrium with iodine) reacts with starch to form the expected blue-black color.

Experimental Procedure:
1. Preparation of iodine solution. Dissolve 5.00 g potassium iodide (KI) and 0.268 g potassium iodate (KIO 3) in 200 mL of distilled water in a 400 mL beaker. Add 30 mL of 3 M sulfuric acid. Then pour the solution into a 500 mL graduated cylinder, and dilute to a final volume of 500 mL with distilled water. Mix thoroughly and transfer to a 600 mL beaker. Do not put this solution in a volumetric flask!!!! 2. Preparation of vitamin C standard solution. Dissolve 0.250 g vitamin C in 100 mL water. Dilute to volume in a 250 mL volumetric flask.

Determination of Vitamin C by an Iodometric Titration 3. Standardization of the iodine solution with the vitamin C standard solution. Add 25.00 mL of vitamin C solution into a 125 mL Erlenmeyer flask. Add 10 drops of 1 % starch solution. Rinse your buret twice with 5 -10 mL of iodine solution, and then fill it. Record your initial buret volume. Titrate the solution until the endpoint is reached (the first sign of blue color that remains after at least 20 s of swirling). Record the final volume. Repeat this titration at least three times. Results should agree to 0.1 mL. 4. Titration of juice samples. Add 25.0 mL of your beverage sample into a 125 mL Erlenmeyer flask. Repeat the iodimetric titration until you have three good measurements (again to 0.1 mL). Use the Q-test to check for bad data. 5. Titration of Real Lemon. Add 10.0 mL of Real Lemon into a 125 mL Erlenmeyer flask. Repeat the iodimetric titration until you have three good measurements (again to 0.1 mL). Use the Q-test to check for bad data.

Data Analysis:
1. What is the reaction to produce iodine from iodate and iodide? Draw the structures of the organic compounds given in Equation (2). 2. (a) Prepare tables of all your titration data. Include the mass of vitamin C used, and the volume of titrant used for each titration. Calculate the molarity of the standardized iodine solution based on each titration. Average your concentration results to obtain the most accurate value and determine the standard deviation. (b) Calculate the amount of vitamin C in your beverage and Real Lemon including the volume of titrant used, the moles of vitamin C present, the molarity of vitamin C, and the concentration of vitamin C in g/L 3. Collect data from all the other groups in the class. Rank each beverage from lowest to highest vitamin C concentration. 4. Average all of the data for the Real Lemon for the whole class and compare that data with the manufacturers data.

Additional Problems:
1. (a) A standard iodine solution was standardized against a 0.4123 g primary standard As4O6 by dissolving the As4O6 in a small amount of NaOH solution, adjusting the pH to 8, and titrating, requiring 40.28 mL iodine solution. What is the concentration of the iodine solution? As4O6 (s) + 6 H2O 4 H3AsO 3 H3AsO 3 + I3- + H2O H3AsO 4 + 3I- + 2H+ (b) The purity of a hydrazine (N2H4) sample is determined by titration with triiodide. A sample of the oily liquid weighing 1.4286 g is dissolved in water and diluted to 1 L in a volumetric flask. A 50.00

Determination of Vitamin C by an Iodometric Titration mL aliquot is taken with a pipette and titrated with the standard iodine solution in (a), requiring 42.41 mL. What is the percent purity by weight of the hydrazine? N2H4 + 2 I3- N2 + 6 I- + 4 H+ 2. A 0.200 g sample containing copper is analyzed iodometrically. Copper(II) is first reduced to copper(I) by iodide according to the following reaction: 2Cu2+ + 4I- 2CuI (s) + I2 and the liberated I2 is titrated against thiosulfate. What is the percent copper in the sample if 20.0 mL of 0.100 M Na2S2O3 is required for titration of the liberated I2 according to the following reaction? I2 + 2S2O32- 2I- + S4O623. Triiodide ions are generated in solution by the following reaction: IO 3- + 6 H+ + 8 I- 3 I3- + 3 H2O If a 25.00 mL sample of 0.0100 M KIO 3 is reacted with an excess of KI and it requires 32.04 mL of Na2S2O3 solution to titrate the I3- ions formed, what is the molarity of the Na2S2O3? Use the equation below. I3- + 2 S2O32- 3 I- + S4O62-

Report: This is a short report. Be sure to include the following:

Tabulate results for standardization and juice analysis (including statistics). Class results for various juices. Answers to questions Signed pledge

PLEDGE: My signature at the end of this report is my pledge that this work is my own. I have neither given nor received help from other students. Signature ________________________________________ Date _____________