水相终止-溶剂萃取/气相色谱法分析氢氧化锆对VX的消毒率  

Determination of Degradation Rate of Zirconium Hydroxide on VX by Gas Chromatography Coupled with Aqueous Phase Termination-Solvent Extraction

作　　者：黄星绮 赵婷 严春晓 金彦任 张鸿鹏 胡晓春 武越 HUANG Xing-qi;ZHAO Ting;YAN Chun-xiao;JIN Yan-ren;ZHANG Hong-peng;HU Xiao-chun;WU Yue(Institute of NBC Defense,Chinese People's Liberation Army,Beijing 102205,China;Shanxi Xinhua Chemical Defense Equipment Research Institute Co.,Ltd.,Taiyuan 030000,China)

机构地区：[1]中国人民解放军陆军防化学院,北京102205 [2]山西新华防化装备研究院有限公司,山西太原030000

出　　处：《分析测试学报》2021年第10期1532-1537,共6页Journal of Instrumental Analysis

摘　　要：建立了水相终止-溶剂萃取/气相色谱/火焰光度检测法(GC/FPD)测定氢氧化锆粉末对维埃克斯(VX)消毒率的分析方法,以保留时间定性分析,内标法定量。对液-固消毒样品的前处理方法进行了优化,考察了萃取剂、萃取方式、终止剂和静置时间对氢氧化锆消毒VX回收率的影响,发现样品采用10 mL 0.05 mol/L硼砂水溶液终止、50 mL二氯甲烷萃取、振荡20 s、静置10 min的萃取效果最好,回收率为87.8%~90.3%,相对标准偏差(RSD)不高于1.2%。优化条件下,在9.7~388.0μg/mL线性范围内呈现良好的线性关系,相关系数(r^(2))为0.9969,方法检出限(LOD)为0.05μg/mL,定量下限(LOQ)为0.15μg/mL。VX的消毒率随反应时间的变化关系满足拟一级动力学过程,反应速率常数(k)为0.0192 min^(-1)。该方法前处理简单、快速、安全,灵敏度和准确度高,可为两性氢氧化物类物质水解消毒反应的评价提供方法参考。VX(O-Ethyl S-(2-diisopropylamino)ethyl methylphosphonothiolate)is one of nerve agents with high toxicity,which could easily penetrate into the skin.Once being poisoned,the nor⁃mal conduction function of the nervous system might be destroyed in a short time,causing breathing difficulties,severe convulsions,loss of consciousness and other symptoms.The most horrible thing is that only a few milligrams of VX could cause death.In 2017,Kim Jong Nam,the eldest brother of North Korea's top leader,died of this poison,which had attracted a great concern all over the world.Studies have shown that zirconium hydroxide could effectively hydrolyze VX through basic t-OH and acidic b-OH.In this study,an analytical method was established for the determination of the degradation rate of zirconium hydroxide powder on VX by gas chromatography with flame photo⁃metric detector coupled with aqueous phase termination-solvent extraction.Qualitative analysis and quantitative analysis were depended on retention time and internal standard method respectively.The pretreatment method for liquid-solid decontamination samples was optimized.The effects of ex⁃tractants,including n-hexane and dichloromethane,extraction methods,such as ultrasound and os⁃cillation,terminators,and standing time on the recovery of VX were investigated.Gas chromatogra⁃phy was used to detect the internal standard and VX,with the retention times of 11.603 min and 12.080 min,respectively.Generally,terminators are used in the degradation process to achieve the purpose of eliminating the activity of decontaminants.However,the most critical thing in this system is to select a terminator that could make the unreacted VX desorb from the adsorption sites of Zr(OH)4.Acidic substances may react with VX to form salt,increasing its solubility in water and making it difficult to extract it into the organic phase.Strong alkaline substances have a degradation reaction with VX.As a result,weak alkaline substances are suitable for termination.It was found that the borax buffer

关 键 词：氢氧化锆 维埃克斯 消毒率 气相色谱 

分 类 号：O657.71[理学—分析化学]