固相微萃取-脉冲火焰光度法测定大气及水中的路易氏剂  

Determination of Lewisite in Ambient Air and Water by Solid Phase Microextraction-Pulsed Flame Photometric Detector

作　　者：王红英[1] 王延东[1] 王秀凤[1] 郝焕明[1] 

机构地区：[1]北京防化研究院,北京102205

出　　处：《分析化学》2005年第10期1479-1482,共4页Chinese Journal of Analytical Chemistry

摘　　要：建立了固相微萃取(SPME)与气相色谱/脉冲火焰光度检测器(GC/PFPD)联用测定大气和水中路易氏剂及其水解产物的方法.探讨了影响SPME萃取效率的萃取头类型、萃取时间、解吸时间等因素.优化了PFPD的条件参数、衍生化试剂及衍生条件.在优化的条件下,路易氏剂衍生产物的响应值与浓度有良好的线性关系.本方法对水中路易氏剂及其水解产物的检出限为0.1 μg/L;气体中路易氏剂的检出限为10 ng/m3;水样的加标回收率为96.7%～102.1%;气体样品的加标回收率为94.9%～103.0%;RSD为2.06%.A novel method for the determination of Lewisite and its hydrolysates in ambient air and water by solid phase microextraction（SPME） coupled with gas chromatography and pulsed flame photometric detector （GC/PFPD） was developed. Some optimum conditions of SPME such as extraction fibres（ 100μm polydimethylsiloxane）, absorption time （ 15 min ） and desorption time （ 3 min ） were chosen by experiments. The operating conditions of GC/PFPD and the derivating reagents were also investigated. The results indicated that detection limits of Lewisite and its hydrolysates of this method were 0.1 μg/L in water, 1 × 10^-5 mg/m3 in air. The recoveries of aqueous samples were 96.7% - 102. 11% and gas samples were 94.9% - 103.0%. The linear range of this method was from 0. 053 to 6. 640μg/L. The relative standard deviations were less than 2. 1%. The proposed method has the advantages of solvent-free sample preparation, simplicity of the procedure, high selectivity and sensitivity.

关 键 词：路易氏剂及其水解产物 固相微萃取 气相色谱 脉冲火焰光度检测器 衍生化 水解产物 路易氏剂 光度法测定 大气 加标回收率 

分 类 号：O657.31[理学—分析化学]