涂料工业 ›› 2017, Vol. 47 ›› Issue (3): 60-66.

• 标准及检测 • 上一篇    下一篇

气相色谱-质谱联用法测定防火涂料中的氯化石蜡及其分配规律

陈满英1 ,路风辉2 ,陆晓燕1 ,李 薇1   

  1. 1. 广东产品质量监督检验研究院,广州 510330; 2. 顺德职业技术学院,广东佛山 528300
  • 出版日期:2017-03-31 发布日期:2019-06-03
  • 作者简介:陈满英( 1974—) ,女,博士,高级工程师,从事化工和环保行业产品检测和科研标准化工作。
  • 基金资助:
    广东省自然科学基金项目(批准号 2015A030310165);国家质检总局科技计划项目(批准号 2013QK284)

Determination of Chlorinated Paraffin and Its Distribution Pattern in Fire Retardant Coatings by Gas Chromatography-Mass Spectrometry

Chen Manying, Lu renghui2 Lu Xiaoyan, Li Wei   

  1. 1. Guangdong Testing Institute of Product Quality Supervision, Guangzhou 510330,China; 2. Shunde Polytechnic, Foshan, Guangdong 528300,China
  • Online:2017-03-31 Published:2019-06-03

摘要: 建立了防火涂料的层析柱前处理法和气相色谱-质谱联用检测法,对 90 种防火涂料、10种电子电器产品防火涂料和 10 种已知含氯化石蜡( CPs) 配方涂料中的 24 种短链氯化石蜡( SCCPs) 和24 种中链氯化石蜡(MCCPs)进行定性定量分析。 方法的平均回收率为85%~112%,相对标准偏差(RSD,n=6)为3%~7.9%,检出限(LOD,S/N≥3)为0.000 1 mg/g。 结果表明防火涂料中,CPs 检出率为 30%,最大浓度为 95 83 mg / g,其中钢结构和电缆防火涂料中 CPs 浓度较大,在 90 个防火涂料产品中,有 6 个涂料 CPs 浓度超过 10 mg/ g。 电子/ 电器防火涂料中,CPs 浓度范围为 ND~10.803 mg/ g, 中位值为 0.205 mg / g。氯含量变动范围较小,集中在 65.6% ~ 66.4%。 钢结构防火涂料、电缆防火涂料 CPs 浓度水平最高,饰面防火涂料和木材防火涂料 CPs 浓度低,分布均匀。

关键词: 气相色谱-质谱, 层析柱法, CPs, 防火涂料, 分配规律

Abstract: The pretreatment and determination method have been established for the deter-mination of chlorinated paraffins (CPs) in fire-retardant coatings. The gas chromatographymass spectrometry method is used in the qualitative and quantitative analysis of the total 48kinds of the short-chain and medium-chain CPs in the coatings. The average recovery rate is8 5%~112% and RSD(n=6) is 3 %~7.9%. And the detection limit of this method is 0.000 1 mg/g. The results show that the detection rate of CPs is 30%. The highest concentra-tion is 95.83 mg/g, wherein the fire retardant coatings for steel structure and cable exhibit th higher concentration of CPs while the decorative and wood fire retardant coatings have the lower concentration of CPs with a uniform distribution of CPs. There are 6 samples among 90 fire retardant coatings showing their concentration of CPS more than 10 mg/g. The range of concentration of CPS in electronic appliances is ND~10803 mg/g, with a median of 0. 205mg/g. The range of chloride content concentrate is 65. 6%~66. 4% with a narrow change.

Key words: gas chromatography-mass spectrometry(gc-ms), chromatographic column, chlorinated paraffin ( CPS), fire-retardant coatings, distribution pattern