论文部分内容阅读
针对纺织品中联苯胺测定时样品前处理存在的问题,对纺织品中联苯胺检测方法中的样品前处理条件进行了研究探讨。采用气相色谱-质谱(GC/MS)分析技术,DB-5 MS石英毛细管柱,选择离子检测(SIM)模式,选择特征碎片离子(m/z)184对联苯胺含量进行检测。对前处理条件中检测结果有明显影响的因素:提取溶剂的选择,还原剂连二亚硫酸钠溶液的配制时间,放置时间和光照等条件进行了考察。解决了由于前处理操作差别带来的联苯胺回收率偏低的问题,提高了检测的准确度和效率。联苯胺质量浓度在0.1~30 mg/L范围内线性关系良好,线性相关系数为r2=0.9993,检出限为1.0 mg/kg,回收率在85%~108%之间。
Aiming at the problems in sample pretreatment of benzidine in textiles, the pretreatment conditions of benzidine in textiles were studied. The benzidine content was determined by gas chromatography-mass spectrometry (GC / MS) analysis, DB-5 MS quartz capillary column, selective ion detection (SIM) mode and selective fragment ion (m / z) Factors that significantly affect the test results in the pretreatment conditions: the choice of extraction solvent, the preparation time of the sodium dithionite solution, the placement time and the light conditions were investigated. Solve the problem of low benzidine recovery due to the difference of pre-treatment operation, and improve the accuracy and efficiency of the detection. The linear range of benzidine was 0.1 ~ 30 mg / L with a linear correlation coefficient of r2 = 0.9993. The detection limit was 1.0 mg / kg. The recoveries ranged from 85% to 108%.