摘要
提出了离子色谱法同时测定工作场所空气中二乙胺、三乙胺和乙二胺含量的方法。使用碱性硅胶管采集工作场所空气样品,以10.0 mL 0.01 mol·L^(-1)硫酸溶液超声解吸20 min,经0.22μm水相针式过滤器过滤,滤液注入离子色谱仪。以IonPac CS17阳离子分析柱为固定相,以10 mmol·L^(-1)甲磺酸溶液为淋洗液分离3种目标物,采用电导检测器测定,外标法定量。结果表明:二乙胺、三乙胺和乙二胺的质量浓度分别在19.1~114.4 mg·L^(-1),15.8~94.6 mg·L^(-1)和2.7~16.3 mg·L^(-1)内与对应的峰面积呈线性关系,检出限(3 s)分别为0.012,0.018,0.017 mg·L^(-1);按照标准加入法对空白碱性硅胶管进行回收试验,回收率为88.4%~102%,测定值的相对标准偏差(n=6)均小于4.0%;方法用于某化工企业的5份空气样品分析,其中二乙胺、三乙胺均未检出,乙二胺的质量浓度为0.47~1.78 mg·m^(-3)。
A method for the simultaneous determination of diethylamine,triethylamine and ethyldiamine in air of workplace by ion chromatography was proposed.The workplace air sample was collected by alkaline silicone tube,and desorbed with 10.0 mL of 0.01 mol·L^(-1)sulfuric acid solution by ultrasonic for 20 min.After filtration through a 0.22μm water phase needle filter,the filtrate was injected into an ion chromatograph.The IonPac CS17 cationic analysis column was used as the stationary phase,and 10 mmol·L^(-1)methanesulfonic acid solution was used as the rinsing solvent to separate the 3 targets,with determination by conductivity detector and quantitation by external standard method.As shown by the results,linear relationships between mass concentrations of diethylamine,triethylamine and ethyldiamine and corresponding peak areas were kept in the ranges of 19.1-114.4 mg·L^(-1),15.8-94.6 mg·L^(-1)and 2.7-16.3 mg·L^(-1),with detection limits(3 s)of 0.012,0.018,0.017 mg·L^(-1),respectively.Test for recovery was made on the blank alkaline silicone tubes according to the standard addition method,giving results in the range of 88.4%-102%,with RSDs(n=6)of the determined values less than 4.0%.The method was used to analyze 5 air samples from a chemical enterprise,in which diethylamine and triethylamine were not detected,and the mass concentration of ethyldiamine was in the range of 0.47-1.78 mg·m^(-3).
作者
刘晙玭
杨莉
王敏
江金凤
LIU Junpin;YANG Li;WANG Min;JIANG Jinfeng(Wuhan Prevention and Treatment Center for Occupational Diseases,Wuhan 430015,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2024年第4期414-417,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
湖北省重点实验室开放基金项目(OHIC2018G07)
武汉市临床医学科研项目(WG20C02)。
关键词
离子色谱法
二乙胺
三乙胺
乙二胺
工作场所
空气
ion chromatography
diethylamine
triethylamine
ethyldiamine
workplace
air
作者简介
刘晙玭,硕士,主要从事职业卫生理化检验工作;通信联系人:江金凤。422644897@qq.com。
