Analysis of Vitamin C Using Iodine. Introduction

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1 Analysis of Vitamin C Using Iodine Introduction Vitamin C (ascorbic acid) is oxidized to dehydroascorbic acid using a mild oxidizing agent such as iodine. The oxidation is a two- electron process, following the reaction: H + I 2 (ascorbic acid) H + 2I - + 2H + (dehydroascorbic acid) Vitamin C in water solution is readily oxidized by dissolved oxygen; therefore samples should be dissolved immediately before analysis. Long- term storage of vitamin C solutions must be avoided. During titration, a small amount of oxidation from oxygen already dissolved in the solution is unavoidable, but is usually not significant. However, continuous shaking of an open flask will bring about enough absorption of oxygen to cause a significant error. 1

3 Therefore, g arsenic (III) oxide produces moles of arsenic (III) oxide, which produces moles of arsenious acid. When diluted to ml, the resulting solution is M, or N. f course, a different mass of arsenic (III) oxide produces a different normality of solution. Calculate the normality of your solution based on the mass of arsenic (III) oxide that you used. 3. Pipette ml of the arsenious acid into each of three Erlenmeyer flasks (~125 ml size). Add 25 ml of DI water and 3.5 grams of sodium bicarbonate (a solid material) to each flask. Check the ph of each solution with ph paper (NT litmus paper). If necessary, add additional small amounts of sodium bicarbonate until the ph is between 7 and 8. If you overshoot ph 8, add small amounts of hydrochloric acid to reduce the ph. ph Test Paper color chart: 4. Add 5 ml of starch indicator to each flask and titrate with iodine solution until the first, stable, blue starch- triiodide color is achieved. Calculate the average normality of the iodine solution. Normality is calculated below. Label the iodine titrant with the normality, and record the normality in your notebook. N I2 = N H3 As 3! ml H 3 As 3 ml I2 3

4 Titration of vitamin C unknown: 1. Weigh ~0.5 grams of your unknown vitamin C sample to 4 decimal places, record the mass, and transfer to a ml volumetric flask. QS with DI water and mix by inversion several times. (NTE: a small amount of binder present in the vitamin C will not dissolve, and gives the solution a slightly cloudy appearance. This binder does not affect the results.) 2. Pipette ml of the vitamin C solution into a 250 ml Erlenmeyer flask and add 5 ml of starch indicator. Titrate the unknown with iodine titrant rapidly but accurately, to the first appearance of a stable blue starch- triiodide color. The entire contents of the Erlenmeyer flask should be the same blue color, and should maintain its color for at least 10 seconds. 3. Analyze 2 additional ml aliquots of vitamin C solution. 4. Your instructor will provide you with details concerning how to report the vitamin C concentration. Lab report A sample report is shown at the end of this procedure. WASTE DISPSAL: All solutions containing arsenic must be disposed of in the aqueous metals waste container. All other solutions may be poured down the sink. 4

5 SAMPLE REPRT: ALL VALUES ARE FICTINAL AND ARE USED FR ILLUSTRATIN NLY!! Standardization of Iodine titrant: Vitamin C Unknown # Robert Bud Fisher 1 st 2 nd 3 rd Vol. Arsenious acid, ml N Arsenious acid Volume Iodine titrant, ml N Iodine titrant N Iodine titrant (average) = Titration of vitamin C unknown: Mass of vitamin C sample: grams Vol. Vitamin C solution, ml Vol. Iodine titrant, ml Normality, vitamin C Molarity, vitamin C Moles, vitamin C mg, Vitamin C Average mg. Vitamin C in sample: Vitamin C in Sample: mg/g sample NTE: results are not rounded until the final answer!! Sample calculations shown on following pages. 5

6 Sample calculations: Normality of iodine: = ( N Iodine = ml! N arsenious _ acid arsenious _ acid ) ml Iodine ( 25.00mL! N) = N 25.04mL Normality of vitamin C: = ( N VC = ml! N Iodine Iodine) ml VC _ solution ( 4.85mL! N) = N 25.00mL Molarity vitamin C: M VC = N VC 2 = N 2 = M Moles vitamin C in sample: moles VC = M VC!V VC _ solution = M! L = moles 6

7 mg. Vitamin C in sample: mg VC = moles VC! grams mole! 1000mg g = moles! grams mole! 1000mg gram = mg Vitamin C in sample: = mg VC,average mass VC,sample,grams = mg g = 85.9 mg g Note: in final answer, volume of iodine titrant was known to 3 SF, sample mass was known to 4 SF, therefore 3 SF governs number of SF in answer. 7

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