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利用热重-红外-气相色谱/质谱(TG-IR-GC/MS)联用技术对聚合物中红磷阻燃剂实现快速定性、定量分析。对于未知样品先用TG-IR-GC/MS联用在线分析模式实时对裂解气体进行分析,根据TG裂解温度点、IR实时扫描红外谱图及GC/MS质谱图对样品进行初步定性;结合定性分析的温度点对样品采用TG-IR-GC/MS联用分离分析模式,抽取该温度点裂解气进入GC/MS扫描红磷系列离子质荷比(m/z)分别为62、93、124,提取m/z为124的离子对样品进行定量分析。结果表明:PA6样品中红磷含量的平均值为35 695 mg/kg,仅比参考值高695 mg/kg,相对误差为2.0%,相对标准偏差(RSD)为11.7%,说明该技术具有较好的准确度和精确度,能很好地应用于测试聚合物中甚至其他形态下的红磷。
The red phosphorus flame retardant in polymer was rapidly qualitatively and quantitatively analyzed by TG-IR-GC / MS. For the unknown samples, the pyrolysis gas was analyzed in real time using TG-IR-GC / MS in-line analysis mode, and the samples were initially characterized according to TG pyrolysis temperature, IR real-time scanning infrared spectra and GC / MS spectra; The samples were analyzed by TG-IR-GC / MS with separated analysis mode at the temperature point of the analysis. The ion mass to charge ratio (m / z) of the pyrolysis gas entering the GC / MS scans at this temperature point were 62, 93 and 124 , Extracted m / z ions of 124 samples for quantitative analysis. The results showed that the average content of red phosphorus in PA6 samples was 35 695 mg / kg, which was only 695 mg / kg higher than the reference value, the relative error was 2.0% and the relative standard deviation (RSD) was 11.7% Good accuracy and accuracy make it well suited for testing red phosphorus in polymers and even in other forms.