Perchloric acid exhibits increased acidic behavior in the presence of acetic anhydride, permitting titration of amides as bases. Analytical data are given for a representative number of amides, acetylated amines, and formylated amines. Perchloric acid in acetic acid, or dioxane, is used as the titrant. End points of the titration curves are readily detected with a modified calomel-glass electrode couple. The method is rapid, reproducible, and more convenient for routine use than previously reported amide procedures. The experimental results are discussed in relation to the probable equilibria involved. Evidence for an increased acidity function is presented, and a reaction mechanism postulated. Certain amides cannot be titrated in acetic anhydride. These are discussed with regard to configuration.
This amount was recovered in the first 25 ml. of effluent. Only traces could be detected spectrophotometrically in the next 25 ml. of effluent, after which blank increases due to thorium were noted. No loss of rare earth occurred in the steps after the ion exchange.By the procedure described here, 6 to 12 determinations may be conveniently carried out simultaneously in 12 to 14 hours. The coprecipitation and separation procedures of Lerner and Pinto (6)
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