摘要
采用气相色谱-质谱法对α-烯基磺酸盐(AOS)中磺内酯3对异构体进行定性分析,同时采用气相色谱外标法结合火焰离子化检测器进行α-烯基磺酸盐制备的中间过程(磺化、中和及水解)以及最终成品中磺内酯含量的测定。从4批AOS样品所得到的测定结果表明,当磺内酯质量浓度在20μg·mL^-1~200μg·mL^-1范围内时GC峰值与磺内酯质量浓度表现为良好的线性关系,相关系数为0.999 0,最低检出限为5μg/g。精密度测试所得标准偏差为1.1%~6.5%(n=6)。回收率达到90.00%~97.96%。
Three pairs of isomers of sultone in alpha olefin sulfonate(AOS) products were qualitatively identified by GC-MS method.Further,the content of sultones in the reaction mixture of intermediate steps(sulfonation,neutralization and hydrolysis) of the AOS preparation as well as in the finished AOS product was quantitatively determined by external standard method using GC in combination with flame ionization detector(GC-FID).Results obtained from samples of four batches of AOS product showed that within the mass concentration of the sultones of 20 μg·mL^-1~200 μg·mL^-1,the peak area vs.mass concentration of the sultones displays good linearity with correlation coefficient of 0.999 0 in the linear equation.The detection limit achieves 5 μg·g^-1.The relative standard deviation in the precision test achieves 1.1%~6.5%(n=6).The recovery achieves 90.00%~97.96%.
出处
《日用化学工业》
CAS
CSCD
北大核心
2010年第4期304-307,共4页
China Surfactant Detergent & Cosmetics