标准及检测
第44卷第1期 2014年1月
涂料工业
PAINT&COATINGS INDUSTRY
Vol.44No.1 Jan.2014
气相色谱-质谱法测定溶剂型涂料中三氯苯的含量魏宇锋，王文青，邱丰，费旭东，张继东（上海出入境检验检疫局，上海200135）摘要：建立了溶剂型涂料中三氧苯3种同分异构体（1.3.5-三氧苯、1.2.4-三氯苯、1.2.3-三氟苯）的气相色谱-质谱检测方法。研究了丙酮、正己烷、四氢呋嘴和乙酸乙酯4种溶剂对涂料中三氟苯的提取以及分离效果。配制三氟苯浓度分别为1mg/L、5mg/L、10mg/L、20mg/L、50mg/L、100mg/L 的标准溶液，以选择离子（SIM）模式进行定性及定量分析。以三氟苯提取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1~100m/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1.3.5-三氟苯、1.2.4-三氟苯、1.2.3-三氟苯检出限(LOD，S/N=3）分别为2mg/kg、2mg/kg、2mg/kg。
关键词：溶剂型涂料：三氯苯：气相色谱-质谱法：检测
文章编号：0253-4312（2014)01-0052-05
中图分类号：TQ630.7*2
文献标识码：A
Determination of Trichlorobenzene Content in Solvent-Based
CoatingsbyGasChromatography-MassSpectrometry Wei YufengWang Wenqing,QiuFeng,FeiXudong,Zhang,Jidong(Shanghai EntryExit Inspection and QuarantineBureau,Shanghai 200135.China)
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 1,2,3TCB in solventbased coatings by gas chromatographymass 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-solutionswithconcentrationofTCBof1mg/L,5mg/L,10mg/L,20mg/L,50mg/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 m/z = 180. 0 peak area of TCB as abscissa and corresponding concentration (mg/L) of TCB as ordinate. The three correlation coefficients were all higher than O0. 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 obtained
【基金项目】国家质检总局科技计划项目（2013IK016）
作者简介：姚宇锋（1981一），男，工程师，主要从事进出口石油及石化产品的检验基定工作。 52