气相色谱-质谱法测定溶剂型涂料中三氯苯的含量  

Determination of Trichlorobenzene Content in Solvent-Based Coatings by Gas Chromatography-Mass Spectrometry

作　　者：魏宇锋[1] 王文青[1] 邱丰[1] 费旭东 张继东[1] 

机构地区：[1]上海出入境检验检疫局,上海200135

出　　处：《涂料工业》2014年第1期52-56,共5页Paint & Coatings Industry

基　　金：国家质检总局科技计划项目(2013IK016)

摘　　要：建立了溶剂型涂料中三氯苯3种同分异构体（1，3，5-三氯苯、1，2，4-三氯苯、1，2，3-三氯苯）的气相色谱一质谱检测方法。研究了丙酮、正己烷、四氢呋喃和乙酸乙酯4种溶剂对涂料中二氯苯的提取以及分离效果。配制三氯苯浓度分别为1mg／L、5mg／L、10mg／L、20mg／L、50mg／L、100rag／L的标准溶液，以选择离子（SIM）模式进行定性及定量分析。以三氯苯提取m／z=180．0离子峰面积为横坐标，以对应的三氯苯浓度（mg／L）为纵坐标，绘制标准曲线。3种同分异构体对应曲线的相关系数均大于0．999，在1-100mg／L浓度范围内线性良好；样品平均回收率为95．9％-107．6％；相对标准偏差（RSD，n=6）在1．44％-4．33％之间。样品中1，3，5-三氯苯、1，2，4-三氯苯、1．2，3-三氯苯检出限（LOD，S／N=3）分别为2mg／kg、2rag／kg、2rag／kg。Abstract：A simultaneous determination method was developed for the quantification and confirmation of three isomers of trichlorobenzene （ TCB ） including 1,3,5-TCB, 1,2,4-TCB, and 1,2,3-TCB in solvent-based coatings by gas chromatography-mass spectrometry （GC- MS）. The extraction and separation efficiencies of target compounds were investigated by using organic solvents of acetone, n-hexane, tetrahydrofuran and ethyl acetate. The standard work- solutions with concentration of TCB of I mg/L, 5 mg/L, 10 rag/L, 20 rag/I., 50 rag/L, 100 mg/L respectiely were prepared, and the solutions were qualitatively and quantitatively analyzed by selected ion monitoring （SIM） mode. Calibration curves were prepared using se- lected nWz = 180.0 peak area of TCB as abscissa and corresponding concentration （rag/L） of TCB as ordinate. The three correlation coefficients were all higher than 0. 999 with good linear relation in the range of 1 mg/L - 100 mg/L. The average sample recoveries were 95.9% 107.6% and the relative standard deviations （RSD, n= 6） were 1.44% -4.33%. The detec- tion limits （LOD, S/N = 3） of 1,3,5-TCB, 1,2,4-TCB and 1,2,3-TCB in coating samples were 2 mg/kg, 2 mg/kg and 2 mg/kg, respectively. Reliable results were obtainedEom detection of actural coating samples, and the method showed the advantage of good repro- ducibility, high sensitivity and simple operation.

关 键 词：溶剂型涂料 三氯苯 气相色谱-质谱法 检测 

分 类 号：TQ630.72[化学工程—精细化工]