提出了顶空-气相色谱-质谱法测定再生纤维素薄膜涂层中18种有机溶剂残留量的方法。选择顶空平衡温度和时间分别为150 ℃和45 min,选用HP-INNOWax毛细管色谱柱(0.25 mm×60 m,0.25 μm)分离,采用选择离子监测模式进行测定。18种溶剂在19 min内能完全分离。18种溶剂的质量均在0.4~8 μg范围内与峰面积呈线性关系,测定下限(10S/N)在0.005~0.02 mg·m-2之间。方法用于再生纤维素薄膜涂层样品分析,加标回收率在83.4%~106%之间,相对标准偏差(n=6)在3.5%~4.3%之间。

Eighteen residual organic solvents in coating of regenerated cellulose fiber film were determined by head-space-GC-MS. The temperature and time chosen for equilibration of the sample were 150 ℃ and 45 min respectively. Capillary chromatographic column of HP-INNOWax (0.25 mm×60 m, 0.25 μm) was used for the separation, and SIM mode was adopted in the determination. Under the optimum conditions, the 18 solvents were separated within 19 min. Linear relationships between values of peak area and mass of the 18 solvents were kept in the same range of 0.4-8 μg, with their lower limits of determination (10S/N) in the same range of 0.005-0.02 mg·m-2. The proposed method was applied to the analysis of samples of coating of regenerated cellulose fiber film, and values of recovery found by standard addition method were ranged from 83.4% to 106%, with RSD′s (n=6) in the range of 3.5%-4.3%.