氧弹燃烧-离子色谱法测定4种再生醇溶剂中总氯、氮和硫的含量  

Contents Determining Total Chlorine,Nitrogen,and Sulfur in Four Regenerated Alcohol Solvents by Oxygen Bomb Combustion-Ion Chromatography

作　　者：郑杰 吴雅鹏 张娟娟 侯宇庭 ZHENG Jie;WU Yapeng;ZHANG Juanjuan;HOU Yuting(Zhejiang Jiajing Environmental Protection Technology Co.,Ltd.,Ningbo,Zhejiang 315000,China)

机构地区：[1]浙江佳境环保科技有限公司,浙江宁波315000

出　　处：《浙江化工》2024年第6期50-54,共5页Zhejiang Chemical Industry

摘　　要：建立并优化了甲醇、乙醇、异丙醇与正丁醇等4种再生一元醇中总氯、总氮与总硫含量的测定方法。采用氧弹燃烧的样品前处理方法,以25 mmol/L的氢氧化钠溶液为氧弹内吸收液,目标物转化为相应的离子化合物,使用离子色谱法进行定量。结果表明,方法中总氯、总氮与总硫拟合的标准曲线,其线性相关系数均大于0.999;样品取样量为1.5 g时,总氯、总氮与总硫的检出限分别为4.79 mg/kg、15.0 mg/kg与6.33 mg/kg,测定下限分别为19.2 mg/kg、60.0 mg/kg与25.3 mg/kg,RSD在2.58%~3.05%之间,加标回收率在70.6%~119%之间。该方法操作简单、准确度较高,实现了甲醇、乙醇、异丙醇与正丁醇等4种再生产品中总氯、总氮与总硫含量的同步快速测定。Methods for the determination of total chlorine,total nitrogen and total sulfur in four regen erated monoalcohols,including methanol,ethanol,isopropanol and n-butanol,were established and optimized.The sample pretreatment method of oxygen bomb combustion was used,and 25 mmol/L sodium hydroxide solution was used as the absorption liquid in the oxygen bomb,and the target was converted into corresponding ionic compounds,which were quantified by ion chromatography.The results showed that the linear correlation coefficients of the standard curves of total chlorine,total nitrogen and total sulfur were all greater than 0.999,and the detection limits of total chlorine,total nitrogen and total sulfur were 4.79 mg/kg,15.0 mg/kg and 6.33 mg/kg,respectively.When the sample sampling amount was 1.5 g,the lower limits of determination were 19.2 mg/kg,60.0 mg/kg and 25.3 mg/kg,respectively.RSD was between 2.58%~3.05%.The recovery rate of spike was between 70.6%~119%.The method is simple to operate and has high accuracy,and realizes the simultaneous and rapid determination of total chlorine,total nitrogen and total sulfur content in four recycled products,including methanol,ethanol,isopropanol and n-butanol.

关 键 词：溶剂 回收 醇 氧弹燃烧 离子色谱法 

分 类 号：TQ413[化学工程] O657.7[理学—分析化学]