液状アマルガムを使用するN,N-dimethyl-formamide中の微量水分の定量法

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Reduction of trace water in N, N-dimethylformamide (DMF) by the use of liquid sodium amalgam (Na-Hg) and potentiometric and conductimetric titration with acetic acid was investigated. It was well known that sodium amalgam reacted with water and formed equivalent sodium ion. In this report, therefore, DMF solution after reduction by sodium amalgam was titrated by potentiometry or conductimetry using acetic acid dissolved in DMF as a standard titrant Na-Hg reacted with H2O but not with DMF owing to basic of DMF. DMF was stirred. with Na-Hg about 5 minutes and amalgam was separated. A separated DMF solution was titrated with acetic acid dissolved in DMF. As the results, less than 10-3% H2O in DMF was measured accurately in comparison with Karl-Fischer method. This method was applied to determine the H2O in other solvent such as petroleum ether, MIBK, carbon tetrachloride, and acetone, and obtained satisfactory results.
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