热裂解气相色谱质谱法分析聚合物中红磷

采用单击热裂解(PY)模式和逸出气体分析(EGA)程序升温两种热裂解模式对红磷样品进行定性分析,利用气相色谱分离技术对红磷进行分离,根据红磷的特征质谱31,62,93,124及特征丰度比,质谱法分析不同材料中的红磷含量。单击热裂解模式下,材质和添加剂有可能对红磷造成干扰,改进后的EGA热裂解模式能排除红磷检测中材质和添加剂的干扰,并采用改进后的EGA裂解程序测定自制阳性样品中红磷的含量。结果表明:通过优化裂解温度和气相色谱条件可以有效改善红磷的分析结果,红磷质量浓度在100~500 mg/kg范围内具有良好线性,加标回收率在90.7%~97.7%,相对标准偏差(RSD)为1.6%~2.3%,定量限为81.27 mg/kg。

Analysis of red phosphorus in polymers by pyrolysis gas chromatography-mass spectrometry

Two pyrolysis modes including single-shot cracking mode and evolved gas analysis(EGA)temperature programmed cracking mode were used to analyze red phosphorus.The red phosphorus was separated quickly and efficiently by gas chromatography.According to the mass spectra peaks of 31,62,93,124 and the abundance ratio of red,the content of red phosphorus in different materials was analyzed using mass spectrometry.Additives could cause interference to the analysis of red phosphorus,the improved EGA pyrolysis mode could eliminate the interference of materials and additives in red phosphorus detection,The improved EGA pyrolysis program was used to determine the content of red phosphorus in the self-made positive samples.The results showed that the optimized pyrolysis temperature and gas chromatographic conditions could effectively improve the analytical results of red phosphorus.The mass concentration of red phosphorus had good linearity in the range of 100-500 mg/kg.The recoveries of red phosphorus were between 90.7%and 97.7%with the relative standard deviations(RSDs)of 1.6%to 2.3%,and the quantitative limit of 81.27 mg/kg.