涂料工业 ›› 2014, Vol. 44 ›› Issue (1): 52-56.

• 标准及检测 • 上一篇    下一篇

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   

  1. 上海出入境检验检疫局,上海 200135
  • 出版日期:2014-01-31 发布日期:2019-06-03
  • 作者简介:魏宇锋( 1981—) ,男,工程师,主要从事进出口石油及石化产品的检验鉴定工作。
  • 基金资助:
    国家质检总局科技计划项目(2013IK016)

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

Wei Yufeng, Wang wenqing, Qiu Feng, Fei Xudong, Zhang Jidong   

  1. Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China
  • Online:2014-01-31 Published:2019-06-03

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-质谱检测方法。 研究了丙酮、正己烷、四氢呋喃和乙酸乙酯 4 种溶剂对涂料中三氯苯 的提取以及分离效果。 配制三氯苯浓度分别为1 mg/L、5 mg/L、10 mg/L、20 mg/L、50 mg/L、100 mg/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 ~ 100 mg / 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 .3%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2 mg/kg、2 mg/kg、2 mg/kg。

关键词: 溶剂型涂料, 三氯苯, 气相色谱-质谱法, 检测

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 worksolutions with concentration of TCB of 1 mg/L, 5 mg/L, 10 mg/L, 20 mg/L, 50 mg/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 selected 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 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 obtained from detection of actural coating samples, and the method showed the advantage of good reproducibility, high sensitivity and simple operation.

Key words: solven-based coatings, trichlorobenzene, gas chromatography-mass spectrometry, detection