有機溶媒による無機塩中の水分の分別定量法
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Near infrared spectrophotometric method combined with the solvent extraction method or the dissolution method have been presented.<BR>The extraction method utilizes methanol, acetone and methyl ethyl ketone for dipping extraction of moisture, and methanol or dioxane for reflux extraction of moisture and weak bonded water of crystallization.<BR>The extracted water is determined by its near infrared absorption at 1.93 μ. The dipping extraction procedure is useful for the determination of moisture on most inorganic salts except for those with larger water content whereby salts themselves may dissolve partly in methanol or ketones, although the results are slightly higher than theoretical amount in the order, methanol>acetone_??_methyl ethyl ketone. The method is simple, more rapid and near precise than the other conventional methods. The reflux extraction procedure can estimate moisture and weak bonded crystalline water by the same procedure, but it difficult to distinguish between them since the solubility of salts is to large.<BR>The dissolution method utilizes polar aprotic solvents such as dimethyl sulphoxide and dimethyl formamide to dissolve sample salts, where total water can be determined as same accuracy as determination of water in solvents. The method can not be applied to slightly soluble alkali fluoride etc., whereas most inorganic salts are soluble enough to be measured spectrophotometrically. The method was simple, economical and more reproducible than the deuterium oxide dissolution method.
- 社団法人 日本分析化学会の論文
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