离子排斥色谱-脉冲安培法测定电镀液中的游离CN^-  

Determination of cyanide in electroplating wastewater by ion exclusion chromatography with pulsed amperometric detection

作　　者：韩静[1,2] 梁立娜[2] 蔡亚岐[2] ChengJun 牟世芬[2] 鲁毅强[1] 

机构地区：[1]北京科技大学化学系,北京100083 [2]中国科学院生态环境研究中心环境化学与生态毒理学国家重点实验室,北京100085 [3]Dionex Corporation, Sunnyvale, California 94088-3603, USA

出　　处：《分析试验室》2008年第10期59-62,共4页Chinese Journal of Analysis Laboratory

基　　金：国家重点基础研究计划(973项目)(2003CB415001);中国科学院重要方向性(KZCX3-SW-432)项目资助

摘　　要：建立了离子排斥色谱-脉冲安培法测定游离CN-的检测方法。方法使用IonPac ICE-AS1离子排斥柱为分析柱,以120 mmol/L HClO4为淋洗液,安培法检测（工作电极为Pt电极）。CN-的检出限为0.42μg/L（50μL进样,三倍基线噪音）;在1-1000μg/L范围内具有良好的线性（r=0.9996）。0.01 mg/L和0.1mg/LCN-分别连续进样9次,峰面积相对标准偏差（RSD）分别为4.0%和3.0%。用该方法检出了电镀液样品中大量的游离CN^-。对实际样品进行加标,其回收率在83%-117%之间。A new method was developed for the determination of CN^- in electroplating wastewater by ion exclusion chromatography with pulsed amperometric detection. The separation of the CN^- was achieved on an IonPac ICE-AS1 column with 120 mmol/L HClO4 as isocratic eluent and the detection was performed with amperometric detector on a Pt working electrode. The detection limit of cyanide was 0.42 μg/L （50μL injection, signal-to-noise ratio of 3） and the linear range of the calibration curve of peak area vs analyte concentration was from 1.0 to 1000 μg/L. Relative standard deviations （RSD） of the peak area for 0.01 mg/L and 0.1 mg/L CN^- were 4.0% and 3.0%, respectively （ n = 9）. The established method had been applied to analysis of CN^- contents in electroplating wastewater. The spiked recoveries of three real samples were 83% - 117%.

关 键 词：游离氰根 离子排斥色谱 积分脉冲安培 电镀液 

分 类 号：O657.7[理学—分析化学]