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前言 离子交换树脂生产过程中,要求快速测定苯乙烯二乙烯苯共聚物氯甲基化珠休(下面简称氯甲基化珠体)的含氯量。目前有些地方采用有机溶剂和水反复洗滌珠体内外吸着的氯化物,然后用氢氧化钠熔融法分解样品后测定含氯量。但这方法花时间长。国外关于氯甲基化珠体含氯量测定的报导不多,主要有示波法〈1〉、ASTM采用的消化法〈2〉、相类似的有机化合物含氯量测定的方法见〈3〉、近年来多采用氧瓶燃烧法〈4〉、及半熔法〈5〉〈6〉等。氧瓶燃烧法要特殊装置,主要用于微量分析。文献〈5〉介绍了艾士卡混合物(2份MgO+1份Na_2CO_3)加热分解样品,再用伏尔哈德法测定塑料含氯量。该法优点在于使用仪器简单,只要小心操作,测定结果的精密度和准确度较好,唯该法将有机物分解和灰化需要的时间较长。文献〈6〉介绍用Na_2CO_3、K_2CO_3、MgO与样品混合,采用短时间灼烧混合物以分解样品,用热水从混合物中把氯化物抽提出来,并通过过滤洗净等操作,手续较繁。本文采用的方法:(1)把珠体粉碎用热水迅速把吸附的氯化物洗净、(2)用含KNO_3的混合物(简称混合试剂)加热迅速分解试样,然后用摩尔法测定氯甲基化珠体含氯量。缩短了分解及灰化的时间,又省了文献〈6〉过滤和抽提氯化物手续,适用于氯甲基化珠体氯量快速?
Preface ion exchange resin production process, the rapid determination of styrene divinylbenzene copolymer chloromethylation beads off (hereinafter referred to as chloromethylated beads) chlorine content. At present, some places use organic solvents and water to repeatedly wash the adsorbed chloride inside and outside the beads, and then measure the chlorine content after decomposing the sample by the sodium hydroxide melting method. But this method takes a long time. Foreign reports on the determination of chloride content of chloromethylated beads are few, mainly by the oscillometric method <1>, digestion method ASTM <2>, similar to the determination of chlorine content of organic compounds see <3> In recent years, more use of oxygen flask combustion method <4>, and half-melting method <5> <6> and so on. Oxygen flask combustion method to a special device, mainly for trace analysis. Literature <5> introduced the mixture of Acacia (2 parts of MgO + 1 part of Na 2 CO 3) to thermally decompose the sample, and then determine the chlorine content of the plastic by the Volkhard method. The method has the advantage of using the instrument is simple, as long as careful operation, the determination of the accuracy and accuracy of the better, only the law of organic matter decomposition and ashing takes longer. Literature <6> describes the use of Na_2CO_3, K_2CO_3, MgO mixed with the sample, the mixture was burned with a short time to break down the sample, with hot water from the mixture of chloride extraction, and washed by filtration operation more complicated. In this paper, the method used: (1) the beads crushed with hot water to quickly wash the adsorption of chloride, (2) with a mixture containing KNO_3 (referred to as mixed reagent) heating rapid decomposition of the sample, Baseline beads contain chlorine. Shorten the decomposition and ashing time, but also save the literature <6> filtration and extraction of chloride procedures for chloromethylated beads fast chloride?