取经剪碎的聚碳酸酯制品(0.5 g)溶于二氯甲烷(10 mL)中,边搅拌边滴加甲醇40 mL至试样溶液中,使样品聚合物基体沉淀析出,样品中残留的碳酸二苯酯存留于溶液中,过滤后,将滤液氮吹浓缩至5 mL,供气相色谱分析。色谱分离中采用HPINNOWAX毛细管柱,测定中采用火焰离子化检测器。碳酸二苯酯的质量浓度在5.0~80.0 mg·L-1范围内与相应的峰面积呈线性关系,方法的检出限(3S/N)为20 mg·kg-1。应用此方法分析了6件聚碳酸酯制品试样,并以其中一件样品作基体,用标准加入法在3个浓度水平上进行回收试验,测得回收率在94.2%~98.2%范围内,测定值的相对标准偏差(n=6)均小于3%。

Sheared pieces of products of polycarbonate (0.5 g) were dissolved in CH2Cl2 (10 mL) and 40 mL of CH3OH were added dropwise into the sample solution with constant stirring to precipitate the matrix polymer leaving diphenyl carbonate in solution. After filtration, the filtrate was concentrated to 5 mL by N2blowing, and the concentrate was used for GC analysis. HPINNOWAX capillary column was used for separation and FID was adopted in the determination. Linear relationship between values of peak area and mass concentration of diphenyl carbonate was kept in the range of 5.0 to 80.0 mg·L-1, with detection limit (3S/N) of 20 mg·kg-1. The proposed method was used for analysis of 6 samples of polycarbonatewares, and test for recovery was made standard addition method at 3 concentration levels using one of the sample as matrix, values of recovery found were in the range of 94.2%-98.2% with RSD′s (n=6) less than 3%.