液相色谱柱前衍生法检测水中无机一氯胺研究  

Research of inorganic monochloramine detection by HPLC-pre-column derivatization method

作　　者：钱玮玲 王正萍[1] 赵晓蕾[2] 张跃军[2] 

机构地区：[1]南京理工大学环境与生物工程学院,南京210094 [2]南京理工大学化工学院,南京210094

出　　处：《安全与环境学报》2017年第2期735-739,共5页Journal of Safety and Environment

基　　金：国家自然科学基金面上项目(21377054)

摘　　要：采用高效液相色谱柱前衍生法建立了水中无机一氯胺(NH2Cl)的检测方法,该方法可以有效区分水中的无机氯胺和有机氯胺。以2-巯基苯并噻唑(2-MBTZ)作为衍生剂,以乙腈和水作为淋洗液,选取Sun FireTMC18分析柱,发现无机一氯胺的衍生产物(2-MBTZNH2)得到了良好的分离。结果表明,在优化衍生反应时间、衍生剂投加量和衍生反应温度条件下,无机一氯胺质量浓度与衍生产物峰面积在0.10~10.00 mg/L的范围内具有良好的线性关系(R2=0.999)。采用液相色谱柱前衍生法测定无机一氯胺的精密度为2.5%~3.4%,检出限为0.013 mg/L,在已知无机一氯胺质量浓度(0.26 mg/L)水样中的加标回收率为93.5%~113.4%,在实际水样中的加标回收率92.6%~106.0%。研究表明,该液相色谱柱前衍生法操作简单方便,测定的无机一氯胺浓度与衍生产物峰面积具有良好的线性关系,同时具有较好的精密度和加标回收率,可用于水中无机一氯胺的分析和检测。The paper is inclined to introduce a so-called HPLCpre-column derivatization method we have developed to identify and determine the inorganic monochloramine（NH2Cl） in treating micro-polluted water samples with ammonia nitrogen through experiments.The method we have developed known as the HPLCpre-column derivatization method can be used to characterize the organic and inorganic chloramines effectively,and detect the colored samples through comparison with the spectrophotometric method,whereas the inorganic monochoramine standard solution can be prepared through the reaction of ammonium chloride and sodium hypochlorite.At the same time,we have also worked out the concentration of the standard solution through N,N-diethyl-1,4-phenylenediamine（DPD） spectrophotometric method.Furthermore,we have adopted 2-mercaptobenzothiazole（2-MBTZ） as the derivative agent,with 70% of acetonitrile and 30% of water being used as the mobile phases.And,next,we have successfully isolated and determined the derivatives of NH2Cl（2-MBTZNH2） through Sun FireTMC18 column and the ultraviolet detector.In proceeding with the given study,we have conducted a series of comparative experiments to optimize the derivative reaction conditions,so as to maximize the concentration of the derivatives in the experimental condition when the reaction time length can be set up for 110 min,and 0.6 m L 1 g/L of the derivatization agent is enough for the reaction with the concentration of the inorganic monochloramine below 8.00 mg/L.However,the reaction temperature turns out not to have much effect on the concentration of the derivative,so the room temperature of 20 ℃ could be chosen.And,simultaneously,we have also found that it is possible to find a perfect linear relationship（R^2= 0.999） of NH2 Cl within the concentration range from 0.10 mg/L to 10.00 mg/L in the optimized derivative reaction conditions.The results of the aforementioned experiments have shown that the detection limit（MDL） of NH2 Cl in the water should be 0.013 mg/L wit

关 键 词：环境工程学 无机一氯胺 液相色谱柱前衍生法 

分 类 号：X830.2[环境科学与工程—环境工程]