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目的建立了测定聚苯乙烯制品中苯乙烯单体残留量的气相色谱法,解决气相色谱法测定苯乙烯单体本底含量高的问题,同时建立GC-MS确证方法。方法聚苯乙烯制品用乙酸乙酯超声溶解,加入一定量对二乙苯作为内标物,经甲醇沉淀高聚化合物,采用GC法和GC-MS法测定。结果 GC法线性范围为0.1μg/ml~40.0μg/ml,GC-MS法线性范围为0.05μg/ml~20.0μg/ml,2个方法的线性r2≥0.999,平均加标回收率在94.2%~104.6%之间,相对标准偏差≤3%(n=6),GC法的定量限为5.0 mg/kg,GC-MS法的定量限为4.0 mg/kg。结论同溶液注入气相色谱法的国标方法相比,结果更准确,方法更简单、可靠。
OBJECTIVE To establish a gas chromatography method for the determination of styrene monomer residues in polystyrene products, and to solve the problem of high content of styrene monomer by gas chromatography. At the same time, GC-MS confirmation method was established. Methods Polystyrene products were dissolved in ethyl acetate by ultrasonic method. A certain amount of diethylbenzene was added as an internal standard, and the polymer was precipitated by methanol. The content of the compounds was determined by GC and GC-MS. Results The linear range of GC-MS was 0.1μg / ml ~ 40.0μg / ml. The linear range of GC-MS was 0.05μg / ml ~ 20.0μg / ml. The linearity of the two methods was r2≥0.999 with the average recovery of 94.2% ~ 104.6%, the relative standard deviation was less than 3% (n = 6), the limit of quantification was 5.0 mg / kg by GC method, and the limit of quantification was 4.0 mg / kg by GC-MS. Conclusion Compared with the GB method of GC injection, the result is more accurate and the method is simpler and more reliable.