氯代甲酸异丙酯含量的测定方法研究

Determination of Isopropyl Chloroformate

建立了一种测定氯代甲酸异丙酯含量的新方法。用 Volhard法预先将酯中水解性 (无机 )氯沉淀下来 ,然后在溶液中加入 40 m L碱性吡啶乙醇溶液 ,在震荡频率为 6 0次 / min的条件下使酯中有效氯全部转化成无机氯 ,反滴定由氯代甲酸异丙酯中有效氯转化的无机氯离子 ,间接求得酯含量。该法直接用于产品测定 ,标准偏差≤ 0 .0 9% ,变异系数≤ 0 .1 %。

A new method for the determination of isopropyl chloroformate is proposed.The hydrolyzed or inorganic chlorine ion in the isopropyl chloroformate sample solution is first completely precipitated with silver nitrate according to the volhard procedure for the purpose of eliminating its interference with the subsequent determination.Then 40 mL alkaline ethanol solution of pyridine is added to the solution to convert the component chlorine of isopropyl chloroformate into inorganic chlorine ion with shaking at a frequence of 60/min.The chlorine ion thus produced is precipitated again by adding silver nirrage soluton.Finally,the isopropyl chloroformate content in samples is determined by following back titration of the excessive silver nitrate,the result being with a standard deviation equal to or less than 0.095 and a coefficient ≤0.1%.