卡尔·费休滴定法测定异丙醇中水分含量
Determination of Moisture in iso-Propanol by Karl Fischer Titration
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摘要: 提出了适用于含醛、酮化学品的水分测定的新卡氏试剂,常规卡尔·费休测水分方法中所用甲醇及吡啶,在新方法中分别用乙二醇甲醚及N-甲基二乙醇胺代替。新卡氏试剂由两部分组成:① 卡氏溶液A(将N-甲基二乙醇胺269 mL与乙二醇甲醚700 mL混合后置于冰浴中,通入二氧化硫至总质量增加64 g为止);② 卡氏溶剂B(将碘84.7 g溶于乙二醇甲醚500 mL中)。上述2种溶剂等体积混合后作为滴定剂,将提出的新卡氏试剂用于测定异丙醇中水分的含量,所得水分测定值与用市售试剂所得测定值相符。新卡氏试剂具有高效、低毒以及性能稳定等优点。Abstract: A new Karl Fischer reagent (abbr. as K.F. reagent) was proposed as titrant for determination of moisture in chemicals containing aldehydes and/or ketones. Methanol and pyridine used in the K.F. reagent of conventional Karl Fischer titrimetric determination of moisture were replaced by ethylene glycol monomethylether (EGME) and N-methyl-diethanolamine (MDEA) respectively. The new K.F. reagent consists of 2 parts: ① K.F. solvent A: mix 269 mL of MDEA with 700 mL of EGME, cool in an icebath and pass in SO2 gas until a surplus mass of 64 g to the total mass was attained; ② K.F. solvent B: dissolve 84.7 g of iodine in 500 mL of EGME. Equal volumes of the above mentioned 2 K.F. solvents were mixed and used as titrant in the Karl Fischer titrimetry. The new K.F. reagent proposed was used in the determination of moisture in iso-propanol, the results obtained were in conformity with the results obtained by using K.F. reagent sold on market. The proposed new K.F. reagent was proved to have the advantages of high efficiency, low toxicity and good stability.