顶空-气相色谱法测定苄基化季铵盐中氯化苄的含量  

Determination of Benzyl Chloride in Benzylated Quaternary Ammonium Salts by Headspace-Gas Chromatography

作　　者：刘向凯 李晓婷 严方 姚晨之 LIU Xiangkai;LI Xiaoting;YAN Fang;YAO Chenzhi(China Research Institute of Daily Chemical Co.,Ltd.,Taiyuan 030001,China;Sinalight Daily Chemical Inspection&Certification Co.,Ltd.,Taiyuan 030001,China)

机构地区：[1]中国日用化学研究院有限公司,太原030001 [2]中轻日用化学检验认证有限公司,太原030001

出　　处：《理化检验（化学分册）》2024年第11期1163-1166,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：通过正交试验优化平衡温度、平衡时间以及进样体积等顶空条件,提出了题示方法。苄基化季铵盐样品被乙醇稀释成300 g·L^(-1)样品溶液,分取4 m L置于顶空瓶中,于90℃平衡20 min,气体进入气相色谱仪,在DB-WAX UI毛细管色谱柱上以程序升温条件分离氯化苄,外标法定量。结果显示:氯化苄的质量浓度在10~110 mg·L^(-1)内和峰面积呈线性关系,检出限(3s/k)为3.73 mg·L^(-1);对十二烷基二甲基苄基氯化铵(1227)样品重复测定6次,测定值的相对标准偏差为1.3%;对1227样品进行3个加标浓度水平的回收试验,氯化苄的回收率为104%~107%。方法用于3种1227样品和1种十八烷基二甲基苄基氯化铵(1827)样品的分析,在1种1227样品中检出了氯化苄,检出量为177 mg·kg^(-1)。The method mentioned by the title was proposed after optimizing headspace conditions of the equilibrium temperature,equilibrium time,and sampling volume by orthogonal experiments.The sample of benzylated quaternary ammonium salts was diluted with ethanol to a 300 g·L^(−1) sample solution,and an aliquot(4 mL)was taken and placed into a headspace bottle.The mixed solution was equilibrated at 90℃for 20 min,and the gas obtained was introduced into a gas chromatograph.Benzyl chloride was separated on a DB-WAX UI capillary column under programmed temperature conditions,with external standard method for quantification.It was shown that linear relationship between values of the mass concentration and peak area of benzyl chloride was kept in the range of 10−110 mg·L^(−1),with the detection limit(3s/k)of 3.73 mg·L^(−1).RSD of the determined values was 1.3%from 6 repeated tests on the sample of dodecyldimethylbenzylammonium chloride(1227).Test for recovery was conducted at the 3 spiked concentration levels on the 1227 sample,and recoveries of benzyl chloride ranged from 104%to 107%.The proposed method was used for three 1227 samples and one octadecyldimethylbenzylammonium chloride(1827)sample.Benzyl chloride was detected in one 1227 sample,with the detection amount of 177 mg·kg−1.

关 键 词：顶空-气相色谱法 正交试验 苄基化季铵盐 氯化苄 

分 类 号：O657.7[理学—分析化学]