吹扫捕集气相色谱质谱法测定黄原酸的关键问题探究  

The key problems in determination of xanthic acid by purge and trap gas chromatography-mass spectrometry

作　　者：朱红霞[1] 谭丽[1] 陈烨[1] 齐炜红 ZHU Hongxia;TAN Li;CHEN Ye;QI Weihong(State Environmental Protection Key Laboratory of Quality Control in Environmental Monitoring,Beijing,100012,China;Handan Environmental Monitoring Station,Handan,056000,China)

机构地区：[1]中国环境监测总站,北京100012 [2]邯郸市环境监测中心站,邯郸056000

出　　处：《环境化学》2019年第11期2449-2456,共8页Environmental Chemistry

基　　金：国家环境保护标准制修订项目(2014-43)资助~~

摘　　要：通常状况下,黄原酸一般以黄原酸盐的状态存在,主要作为捕收剂广泛应用于矿产浮选.本研究采用吹扫捕集/气相色谱-质谱法测定黄原酸总量,对测定涉及的关键操作环节及重点技术问题进行了深入研究.研究了黄原酸种类、酸加入时间、pH、酸加入量和酸种类等样品前处理步骤中的影响因素,讨论了重金属、含盐量、氧化物以及化学性质相同的共存物质等方法干扰问题.其中水样中氧化物对测定的干扰问题较为突出,可通过加入5-20 mg硫代硫酸钠去除.此外,硫代硫酸钠的加入还可将样品保存时间由1 d延长到2周.Under normal circumstances,xanthic acid generally exists in the state of xanthate, and is used as a collector in mineral flotation mainly. In this research, the total amount of xanthic acid was determined by purge and trap/gas chromatography-mass spectrometry. The key operational steps and technical issues were further studied, including the influence factors of xanthogen type, acid addition time, pH, acid addition amount, acid type, et al in the sample preparation step. The problems of method interference were discussed, such as heavy metals, salinity, oxides and coexisting substances with same chemical nature. The interference of oxides in the water sample was more prominent, which could be removed by adding 5-20 mg sodium thiosulfate. Besides, sample storage time was extended from one day to two weeks by using sodium thiosulfate.

关 键 词：黄原酸 吹扫捕集 气相色谱质谱法 二硫化碳 磷酸 硫代硫酸钠 

分 类 号：O65[理学—分析化学]