大体积进样离子色谱-柱切换法测定环境水样中叠氮根  

Determination of Azide in Environment Water using Ion Chromatography with Large Volume Injection and Column-switching Technique

作　　者：李刚 陈燕 陈东 

机构地区：[1]绍兴市环境监测中心站,绍兴312000 [2]杭州萧山供水有限公司,杭州310002 [3]浙江龙盛集团股份有限公司,绍兴312000

出　　处：《现代科学仪器》2015年第5期109-111,共3页Modern Scientific Instruments

基　　金：本文系国家重大科学仪器设备开发专项（No.2012YQ09022903）;浙江省自然科学基金（Nos.Y4110532,LQl38050001,Z148070002）;浙江省公益性科技计划（分析测试）项目（No.2012C37038）,国家海洋局海洋-大气化学与全球变化重点实验室基金（Nos.GCMAC1208,GCMAC1109）,浙江省公益性技术应用研究计划项目（No.2013C37073）

摘　　要：建立了离子色谱一直接电导法测定环境水样中叠氮根的方法。环境水样经滤膜过滤后直接进样。将样品先通过一根高聚物反相柱进行在线预处理，除去水溶性有机杂质，采用阴离子富集柱TAC-ULPl收集叠氮根离子并进入分析系统分析。以IonPac AG18（4mm×50mm）＋IonPac ASl8（4m×250mm）色谱柱进行分离，采用氢氧化钾梯度淋洗，流速为1．0mL／min，柱温50℃，进样体积200μL，电导检测器检测。实验结果表明，叠氮根在0．01～2．0mg／L范围内线性关系良好（r=0．9994），检测限（LOD）为2．51μg／L（S／N=3）。该方法操作简单、灵敏度高、重现性好，可用于测定环境水体中的叠氮根。A method has been proposed for determination of azide in environment water by ion chromatography with large volume injection and column-switching techique. Samples were filtered through H column and 0.22μm filter membrane. A reversed-phase column was used as a pretreatment column to eliminate organics on-line. Azide was collected by TAC-ULP1 column and delivered to the analytical system to analyze. KOH gradient elution was selected as the eluent at a flow rate of 1.0mL/min. IonPac AG18（4 mm× 50 mm） and IonPac AS 18（4 mm×250 mm） were chosen for separation with suppressed conductivity detection. The results showed that azide has good linear in the range of 0.01-2.0mg/L（r=0.9994）. The detection limit（LOD） of the method is 2.51μg/L（S/N=3）, under the conditions of 200μL sample volume. The method has the advantage of simple operation, and can meet the quantitative analysis requirements of environment water.

关 键 词：离子色谱 叠氮根 大体积进样 环境水样 

分 类 号：O657.75[理学—分析化学]