气相色谱-质谱法测定固体废渣中二苯氰胂

摘要

提出了气相色谱-质谱法测定固体废渣中二苯氰胂的方法。样品经甲醇提取，所得提取液用1-丁硫醇试剂衍生。在气相色谱分离中用DB-5MS毛细管柱为固定相，在质谱分析中采用选择离子监测模式。二苯氰胂的峰面积与质量浓度在0．5～10mg·L^-1范围内呈线性关系，检出限（3s）为0．04mg·L^-1。在3个浓度水平上做加标回收试验，测得回收率在91．6％～101％之间。相对标准偏差（n=5）在3．3％～4．5％之间。%A method of GC-MS for determination of diphenyIcyanoarsine in solid waste was proposed. Sample was extracted with methanol and derivatized with [ butyl thiol. DB-SMS capillary column was used for GC separation and selected ion monitoring mode was adopted in MS determination- Linear relationship between values of peak area and mass concentration of diphenylcyanoarsine was obtained in the range of 0. 5 - 10 mg·L^-1with detection limit (3s) 0. 04 mg·L^-1. Tests for recovery were performed by addition of standard at 3 concentration levels, results of recovery found were in the range of 91.6%-101% with RSD's (n=5) in the range of 3. 3%-4.5%.