摘要
建立快速、准确的检测水中三氯甲烷和四氯化碳含量的检测方法。采用自动进样顶空-气相色谱法,电子捕获检测器,顶空加热箱60℃,平衡30 min,毛细色谱柱为Agilent HP-5(30 m×320μm×0.05μm)。三氯甲烷在2~100μg/L范围内与峰面积呈现良好的线性关系,线性方程为Y_(1)=84.495X_(1)+48.287,相关系数R^(2)为0.9992,回收率在100.0%~108.8%范围内,重复测定8次的相对标准偏差为0.9%~3.4%;四氯化碳在0.2~10μg/L范围内与峰面积呈现良好的线性关系,线性方程为Y_(2)=1452.9X_(2)+64.375,相关系数R^(2)为0.9998,回收率为98.5%~111.0%,重复测定8次的相对标准偏差为3.2%~6.6%;三氯甲烷和四氯化碳的检出限分别为0.05μg/L和0.005μg/L。与国标方法相比,本方法符合国标要求且检出限低于国标要求,能快速准确地检测水中三氯甲烷和四氯化碳的含量,可极大满足实际用水需求。
We established a rapid and accurate determination method for trichloromethane and carbon tetrachloride in water.Automat-ic sampling headspace gas chromatography was performed on Agilent HP-5(30 m×320μm×0.05μm)column with electron capture detector(μ-ECD)at 60℃for 30 min.The linear relationship of trichloromethane was good within the concentration range of 2μg/L to 100μg/L;the linear equation was Y_(1)=84.495X_(1)+48.287,and the correlation coefficient(R^(2))was 0.9992;the recoveries were in the range of 100.0%to 108.8%,and the relative standard deviations were between 0.9%and 3.4%.The linear relationship of carbon tetrachloride was good within the concentration range of 0.2 to 10μg/L;the linear equation was Y_(2)=1452.9X_(2)+64.375,and the corre-lation coefficient(R^(2))was 0.9998;the recoveries were in the range of 98.5%to 111.0%,and the relative standard deviations were be-tween 3.2%and 6.6%.The limit of detection was 0.05μg/L for trichloromethane and 0.005μg/L for carbon tetrachloride.Com-pared with the method in the national standard,this method has lower limit of detection,and can quickly and accurately detect the content of trichloromethane and carbon tetrachloride in water.
作者
冯小兵
程平言
杨军林
陈明学
蒋力力
FENG Xiaobing;CHENG Pingyan;YANG Junlin;CHEN Mingxue;JIANG Lili(Xijiu Co.Ltd.of Maotai Distillery Group,Xishui,Guizhou 564622,China)
出处
《酿酒科技》
2022年第2期117-120,共4页
Liquor-Making Science & Technology
基金
遵市科合(2018)29号
遵市科合R&D(2019)4号
遵优青科[2019]1号
黔科合成果[2020]2Y042
黔财工[2019]226号贵州省十大千亿级工业(优质烟酒)专项资金项目-酱香型白酒品质提升关键技术集成研究与应用
黔财建[2019]303号-贵州省纯粮固态酿造技术工程研究中心建设。
关键词
三氯甲烷
四氯化碳
顶空气相色谱
水
trichloromethane
carbon tetrachloride
headspace gas chromatography
water