气相色谱-负化学源质谱法测定电子电气产品聚合物材料中的卤代磷酸酯阻燃剂

发布时间：2019-05-05 11:50

【摘要】：采用丙酮作为萃取溶剂,对电子电气产品聚合物材料中的卤代磷酸酯阻燃剂超声萃取1.5h后,浓缩、定容、上机。为提高仪器分析方法的选择性,减少前处理流程,选取负化学电离(NCI)模式,在离子源温度210℃、甲烷气流量2.5mL/min条件下对目标分析物进行定性定量分析。结果表明,磷酸三(2-氯乙基)酯(TCEP)和磷酸三(1-氯-2丙基)酯(TCPP)在0.1~10mg/L浓度范围内,磷酸三(1,3-二氯异丙基)酯(TDCP)和磷酸三(2,3-二溴丙基)酯(TDBP)在0.010~10mg/L浓度范围内,均有良好的线性关系,相关系数(R2)大于0.999。TCEP和TCPP的检出限和定量限分别为0.010mg/kg(S/N=3)和0.10mg/kg(S/N=10);TDCP和TDBP的检出限和定量限分别为0.001mg/kg(S/N=3)和0.010mg/kg(S/N=10)。本方法对空白样品中目标分析物的加标回收率为85.6%~108.9%,相对标准偏差为8.5%。分析了30批次实际样品,包括丙烯腈-丁二烯-苯乙烯共聚物(ABS)、聚氯乙烯(PVC)、印刷电路板(环氧树脂为主要成分)和聚丙烯(PP)等电子电气产品聚合物材料,有2批次检出TCPP,其含量分别为367.5mg/kg、695.2mg/kg。可见,电子电气产品聚合物材料中存在一定的卤代磷酸酯阻燃剂污染风险。
[Abstract]:Ultrasonic extraction of halophosphate flame retardants from polymer materials of electrical and electronic products was carried out by ultrasonic extraction with acetone as extraction solvent for 1.5 h, then concentrated, constant volume and put on the machine. In order to improve the selectivity of instrumental analysis method and reduce the pretreatment process, a negative chemical ionization (NCI) model was selected to carry out qualitative and quantitative analysis of the target analyte under the condition of ion source temperature of 210C and methane gas flow rate of 2.5mL/min. The results showed that tris (2-chloroethyl) phosphate (TCEP) and tris (1-chloro-2-propyl) phosphate (TCPP) were in the range of 0.1~10mg/L concentration. Tris (1,3-dichloroisopropyl) phosphate (TDCP) and tris (2,3-dibromopropyl) phosphate (TDBP) showed good linear relationship in the concentration range of 0.010~10mg/L. The correlation coefficient (R2) was greater than the detection limit and quantitative limit of 0.999.TCEP and TCPP were 0.010mg/kg (S/N=3) and 0.10mg/kg (S/N=10), respectively. The detection limits and quantitative limits of TDCP and TDBP were 0.001mg/kg (S/N=3) and 0.010mg/kg (S/N=10), respectively. The recoveries of target analytes in blank samples were 85.6% ~ 108.9% and the relative standard deviation (RSD) was 8.5%. Thirty batches of practical samples, including acrylonitrile-butadiene-styrene copolymer (ABS), PVC (PVC), printed circuit board (epoxy resin as the main component) and polypropylene (PP) and other electronic and electrical products polymer materials, were analyzed. The content of TCPP, was 367.5 mg 路kg ~ (- 1) and 695.2 mg 路kg ~ (- 1) respectively in two batches. It can be seen that there is a certain risk of halogenated phosphate flame retardants pollution in the polymer materials of electronic and electrical products.
【作者单位】：深圳市计量质量检测研究院;
【基金】：广东省质量技术监督局科技项目基金(2014PJ03)资助
【分类号】：O657.63;TQ317

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