N-メチル基微量定量分析の一改良法

概要

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Quantitative microdetermination of N-methyl groupe is one of the most difficult analysis in structural analysis and although many improved methods are proposed, these require careful attention and high skill, furthermore, their accuracies are rather obscure and the data of practical operations are lacking in numbers. Attempts have been made to test on heretofore known quantitative microdetermination methods of N-methyl group with the result of considarable + errors due to an incomplete removal of obstructive gases. Although this difficuly was removed by lowering the rate of gaseous flow to 1 bubble/2-3 seconds, but the operation was rather difficult, The authors used a washing tube containing solid sodium thiosulfate and an improved liquid washer in order to remove iodine vapor and hydrogen iodide which cause + error. Further improvement is made by setting a double distilling system. The result of testing on 11 kinds of samples indicated that the average error was -0.12% and the square root of unbiased estimate of variance was 0.18%. This improved method has merits in accuracy, shortening the time of operation and simplification of the operation than the other methods, especially, the rate of flow of carbon dioxide can be increased several times more than the other methods; also it can be operated 2 sets at the same time.
社団法人日本分析化学会の論文