气相色谱-质谱法分析水中1,4-二噻烷  

Determination the Concentration of 1,4-Dithiane in Water by Gas Chromatography-Mass Spectrometry

作　　者：赵华 韩世同 ZHAO Hua;HAN Shitong(State Key Laboratory of NBC Protection for Civilian,Beijing 102205,China)

机构地区：[1]国民核生化灾害防护国家重点实验室,北京102205

出　　处：《防化研究》2023年第4期25-33,共9页CBRN DEFENSE

摘　　要：1,4-二噻烷(1,4-dithiane)是一种具有中等毒性的芥子气降解产物,稳定性高、持久性强,可以被氧化成亚砜与砜类物质。因此,检测水体中1,4-二噻烷的浓度,对于控制污染物扩散和保护人员健康具有重要意义。本研究建立了液液萃取-气相色谱-质谱法,用于直接测定水中1,4-二噻烷。结果表明,该方法在2~100μg·L^(-1)范围内线性关系良好,方法检出限(MDL)为0.47μg·L^(-1),具有较高的检测灵敏度;在不同pH、腐殖酸(Humic Acid)浓度、阳离子和阴离子条件下,具有较强的抗干扰能力;在实际地表水和地下水检测中,对于1,4-二噻烷的高、中、低3个添加水平的加标溶液回收率为96.46%~116.13%,相对标准偏差(RSD)为4.01%~9.66%(n=6)。该分析方法高效、准确,可为日本遗弃在华化学武器中芥子气在水体中的分解产物检测提供帮助。1,4-dithiane is a moderately toxic degradation product of mustard with high stability and persistence,which can be oxidized to sulfoxides and sulfones,so it is important to detect the concentration of 1,4-dithiane in water in order to control the spread of pollution and protect the health of personnel.In this study,a method of liquid-liquid extraction with gas chromatography-mass spectrometry was demonstrated to analyze 1,4-dithiane in water.The results show that the method has good linearity in the range of 2~100μg·L^(-1),and the method detection limit(MDL)is 0.47μg·L^(-1)with good precision and accuracy;it has strong anti-interference capability under different pH,humic acid concentration,cation and anion conditions;and for the detection of surface water and groundwater,the spiked recoveries for high,medium,and low levels of 1,4-dithiane are 96.46%~116.13%,and the relative standard deviation(RSD)is 4.01%~9.66%(n=6).This analytical method is efficient and accurate,and can be useful for the detection of decomposition products of mustard contaminated water caused by chemical weapons abandoned in China by Japanese.

关 键 词：气相色谱-质谱法 芥子气 1 4-二噻烷 地表水 地下水 

分 类 号：X8[环境科学与工程—环境工程]