顶空气相色谱法同时测定铀产品中痕量氯、溴、碘

SIMULTANEOUS DETERMINATION OF TRACE CHLORIDE, BROMIDE AND IODIDE IN URANIUM PRODUCTS USING HEAD SPACE GAS CHROMATOGRAPHY (HSGC)

本工作研究了一种灵敏简便的同时测定氯、溴,碘的顶空气相色谱法,并成功地应用于铀产品中氯、溴、碘的分析。 方法基于氯、溴、碘在中性或酸性介质中与硫酸二甲酯反应,生成氯甲烷、溴甲烷、碘甲烷;应用顶空气相色谱法,不需经分离手续,即可同时测量这些卤代甲烷,在样品分析时用标准加入法定量。本方法较液体进样的气相色谱法提高灵敏度1至2个数量级,可以用于测定铀产品中ppm数量级的氯,ppb数量级的溴和碘。三个元素的回收率均大于90％。

A sensitive and simple method for simultaneous determination of tiace chloride, bromide and iodide is developed and applied successfully to the analysis of uranium products. This method is based on the reaction of halides with dimethyl sulphate in neutral or acidic solution resulting methylchloride, methylbromide and methyliodide. And it is unnecessary for the HSGC method to separate the methylhalides from the matrix. In routine analysis the standard addition method is adopted as quantitative method. Compared with the common Gc, the sensitivity of the HSGC method has increased by one or two powers of 10. The method is used for quantitative analysis of ppm levels of chloride and ppb levels of bromide and iodide in uranium products. The results reveal that the recoveries are over 90% for the three halides.