By Thomas M. Schmitt
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B) Column chromatography. 500 ppm range. This procedure is suitable for levels of sultone in the 10- Procedure (89) Two grams of an aqueous 40% sample solution is mixed with 20 mL of 2:1 acetone/water and applied to the top of a silica gel column, 50-150 mesh, 20 x 250 mm. The column is eluted with 500 mL petroleum ether. 1 g KOH and again evaporated down. The residue is analyzed colorimetrically: The residue is dissolved in 85 mL water and transferred to a separatory funnel. 5 mL cone. H2SO4 to 1 L water), and 15 mL CHC13 are added.
1 N sodium thiosulfate solution to the starch end point, with vigorous stirring. Determine the reagent blank in the same manner. Calculation: % sodium sulfite = (B-V)(N)63 W where B and V are milliliters of titrant required for the blank and sample titrations, N is the concentration of the titrant (normality), and W is the sample weight in grams. Note: The sample is added to excess reagent to minimize interference from oxygen, which can also oxidize sulfite. The similarities between this procedure and that for unsaturation determination are obvious, and neither parameter can be determined in the presence of the other by this procedure.
A 5-mL buret glassware unit is suitable. Weigh a sample of about 4 g into a 100-mL volumetric flask and dissolve and dilute to volume with 1:1 THF/water. Depending on the expected SC>42~ content, transfer an aliquot of 1 to 10 mL into the Conductometric titration cell. 62) and 5 mL THF as well as 1 or 2 drops of an aqueous suspension of barium sulfate (freshly shaken). If the liquid level of the cell is too low, add 1:1 THF/water as necessary to properly immerse the electrodes. 62 acetate buffer solution) with stirring.