摘要
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 the polymers was qualitatively and quantitatively analyzed by thermal gravimetric-infrared spectroscopy-gas chromatography/mass spectrometry（TG-IR-GC/MS） coupling technique. As for the unknown samples, their cracking gas would be qualitatively analyzed by online mode of TG-IR-GC/MS firstly, and the unknown samples and cracking temperature point could be identified by the cracking temperature in TG, real-time scanning IR spectrum and MS spectra in GC/MS. Based on the result of qualitative analysis, the samples were quantitatively analyzed by separation and analysis model of TG-IR-GC/MS. By scanning m/z（62, 93, 124） in the cracking gas of the specific temperature point, the red phosphorus in sample could be finally quantitative analyzed. The results show that the average content of red phosphorus in specific PA6 is 35 695 mg/kg, only 695 mg/kg higher than the reference value. The relative error and relative standard deviations（RSD） are 2.0% and 11.7% respectively, which shows that the technique has good accuracy and precision. It can be applied to analyze the red phosphorus in polymers or other materials.
出处
《塑料科技》
CAS
北大核心
2016年第11期82-85,共4页
Plastics Science and Technology
