摘要
用改进的方法合成了对甲苯磺酰肼基二硫代甲酸钾(化合物1).以它作模型化合物,在酸性条件下加热分解,放出二硫化碳,被二乙胺及醋酸铜的混合液吸收,生成黄色荒氨酸铜,在430nm波长比色,从而建立了定量测定磺酰肼基二硫代甲酸基团的方法.并首次合成了苯磺酰肼基二硫代甲酸钾(化合物2)和对甲苯磺酰肼基二硫代甲酸三乙胺盐(化合物3)的纯品,与化合物1—起作标样,用外标法对测定方法进行了验证.测得二硫化碳回收率为99.2—100.5%,相对标准偏差≤2.0%.以此方法测定了用交联度和颗粒度不同的两种聚苯乙烯白球在相同条件下合成的聚苯乙烯磺酰肼基二硫代甲酸盐树脂的功能化程度,分别为1.62mmol·g^(-1)及1.29mmol·g^(-1).
A colorimetric analytical method was established for the determination of degree of functionalization of the salt of polystyrylsulfonylhydrazinecarbodithioic acid resin prepared from polystyrene beads. Therefore, potassium salt of tosylhydrazenecarbodithioic acid (1) synthesized by a improved method was used as model compound. It decomposed when heated in acid condition and evolved carbon disulfide. The gas was absorbed in alcoholic solution containing diethylamine, cupric acetate and triethanolamine to produce yellow cupric diethyldithiocarbamate. This color intensity, proportional to the amount of carbon disulfide absorbed,was measured spectrophotometrically at 430nm. potassium salt of phenylsulfonylhydrazinecarbodithioic acid (2) and triethylammonium salt of tosyl-hydrazinecarbodithioic acid (3) were also prepared firstyl and, together with compound l, were used as standards to check the analytical method. The recovery of CS2 is 99. 2-100.5%, RSD<2.0%. The degree of functionalization of the polystyryl-sulfonylhydrazinecarbodithioic acid resins prepared in same condition with two different polystyrene beads as starting materials were determined as 1.62mmol·g-1 and 1. 29mmol·g-1,respectively, by this method.
出处
《环境化学》
CAS
CSCD
北大核心
1998年第5期467-472,共6页
Environmental Chemistry
基金
国家自然科学基金资助项目:59478020
关键词
聚苯乙烯
磺酰肼基
二硫代甲酸盐
分光光度法
polystyrylsulfonylhydrazinecarbodithioic acid resin, spectrophotometry, degree of functionalization.
