高温裂解在线测试高氯酸盐氧同位素方法研究  

High Temperature Convertion Online Measurement of Oxygen Isotopic Composition of Perchlorate

作　　者：方玲[1] 周爱国[1,2] 李小倩[1,2] 刘运德[2] 张梦南[3] 

机构地区：[1]中国地质大学(武汉)环境学院,武汉430074 [2]中国地质大学(武汉)生物地质与环境地质国家重点实验室,武汉430074 [3]中国地质调查局水文地质环境地质调查中心,河北保定071051

出　　处：《地质学报》2015年第10期1832-1840,共9页Acta Geologica Sinica

基　　金：国家自然科学基金项目(编号:41202169;41402218);中央高校基本科研业务费专项资金项目(编号:CUGL140407)项目的成果

摘　　要：高温裂解在线测试高氯酸盐氧同位素的方法与技术,能够为环境介质中高氯酸盐来源的识别、迁移转化过程的示踪及其污染的防治提供重要的分析工具。采用单因子试验系统研究了方法的裂解温度、样品质量和样品类型对高氯酸盐氧同位素测试精度的影响,并采用阴离子交换树脂法进行高氯酸盐环境样品的预处理,探讨测试方法的应用。实验结果表明,反应温度对方法测试精度的影响显著,反应温度必须严格控制在1325℃;样品质量对测试精度不产生显著影响,但最小样品量不低于0.25μmol ClO-4;测试方法适用于不同类型的高氯酸盐,测试精度均优于0.5‰。测试结果不同的校正方法表明,采用多种氧同位素标准的线性校正优于采用单一高氯酸盐氧同位素标准的校正,特别是在样品与标准的氧同位素组成差别较大时,单一标准的校正会产生较大的误差。基于A530E型双官能团阴离子交换树脂的富集与提取ClO-4的预处理方法,可实现高氯酸盐环境样品的氧同位素测定,测试精度优于0.3‰。High temperature convertion online measurement of oxygen isotopic composition of perchlorate can provide important clues to recognize the origin of perchlorate,trace the subsequent migration and transformation processes of perchlorate,and prevent the pollution of perchlorate.The accurate research on the effects of reaction temperature,sample size and sample type on analytical precision,and the research on preparation and purification procedures of field perchlorate samples are important to expand the application of this method.The results indicate that the reaction temperature has a significant effect on analytical precision,so the reaction temperature must be controlled at 1325℃.The sample size has a slight effect on analytical precision,with the least sample size of 0.25μmol ClO-4.This method can be applied to different types of perchlorate,with a good analytical precision of 0.5‰.Both the method corrected by USGS37,the international standard of perchlorate,and linearity correction of multiple international standards of oxygen isotope are used to correct the test results of field perchlorate samples.The method corrected by USGS37 will result in a major inaccuracy,especially when oxygen isotopic composition of samples have significant differences with the standard.Based on the pretreatment method of ClO-4concentrated and extracted by the bifunctional ion-exchange resin A530 E,the test results of field perchlorate samples are within a good analytical precision of 0.3‰.

关 键 词：高氯酸盐 高温裂解 阴离子交换 氧同位素 多标准校正 

分 类 号：X830[环境科学与工程—环境工程]