PVC塑料中己二酸酯类增塑剂的快速筛查和半定量分析

Rapid screening and semi-quantitative analysis of adipate plasticizers in PVC plastics

利用裂解器的热解吸功能,采用固体样品直接进样技术,通过加热将PVC塑料中的己二酸酯类增塑剂释放出来,在线利用气质联用仪进行定性和半定量分析,外标法定量,从而建立了一种能快速筛查和半定量测定PVC塑料中8种己二酸酯类增塑剂含量的气质联用分析方法,并对热解吸温度、热解吸时间、附件初始温度、裂解头升温速率等裂解器热解吸工作条件和仪器分析条件进行了优化,对方法的线性关系和精密度进行了研究。在3倍信噪比(S/N=3)的条件下,方法检出限为0.1〜1.0 mg/kg。方法精密度试验相对标准偏差为3.74%〜11.42%。该方法不需使用任何有机溶剂进行样品前处理,绿色环保,对环境友好,简单快速、灵敏度高,定性可靠,检出限低。

A solid sample was introduced directly and was heated in a pyrolysis instrument.Adipate plasticizers in PVC plastics were released.Then qualitative and semi-quantitative analysis were carried out online by gas chromatography/mass spectrometry(GC/MS)technique.The concentration of each adipate plasticizer were calibrated by external standard method.Therefore,a GC/MS method was established for the rapid screening and semi-quantitative analysis of eight adipate plasticizers in PVC plastics.The working conditions of thermal desorption such as thermal desorption temperature,thermal desorption time,initial temperature of accessory,and heating rate of the pyrolysis instrument,were optimized.The chromatographic separation conditions were also optimized.The linear relationship and precision of the proposed method were studied.At the condition that ratio of signal to noise(S/N)was three,the limits of detection(LODs)varied from 0.1 mg/kg to 1.0 mg/kg.The relative standard deviation(RSD)of the precision experiments changed from 3.74%to 11.42%.The sampling method adopted in the proposed method was direct sampling of solid samples,did not need organic solvents for the pretreatment of the samples.Therefore,the proposed method was environmentally friendly,simple and rapid and had high sensitivity,reliable qualitativeness and low detection limit.