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目的:建立D-101型树脂中苯、甲苯、苯乙烯3种低沸点残留有机溶剂直接固体树脂顶空进样GC含量测定方法。方法:顶空条件为平衡温度120℃,加压时间0.5 min,平衡时间30 min,定量环填充时间0.5 min,进样时间1 min。色谱条件:FID检测器,DM-1气相柱,柱温60℃保持10 min,5℃.min-1升至200℃,分流比2∶1,流速0.4 mL.min-1,N2-Ai-H2(30∶300∶30)。结果:各成分线性关系均良好,回收率>90%,精密度、重复性良好,各有机残留溶剂最低检测限均<3 ppm。结论:直接固体树脂顶空进样较溶剂提取进样法,检测结果更接近真值,且操作简单,适用于D-101树脂中苯等低沸点有机溶剂残留的含量测定。
OBJECTIVE: To establish a method for determining the GC content of direct solid resin headspace sampling by three kinds of low-boiling residual organic solvents such as benzene, toluene and styrene in D-101 resin. Methods: The headspace conditions were equilibrium temperature of 120 ℃, pressurization time of 0.5 min, equilibration time of 30 min, loop filling time of 0.5 min and injection time of 1 min. Chromatographic conditions: FID detector, DM-1 gas phase column, column temperature 60 ℃ for 10 min, 5 ℃ .min-1 rose to 200 ℃, split ratio 2: 1, flow rate 0.4 mL.min- H2 (30: 300: 30). Results: The linear relationship between the ingredients was good, the recovery rate was> 90%, and the precision and repeatability were good. The detection limits of all organic solvents were all <3 ppm. Conclusion: The direct solid resin headspace sampling is better than the solvent extraction sampling method, the detection results are closer to the true value, and the operation is simple. It is suitable for the determination of benzene and other low boiling point organic solvents in D-101 resin.