离子色谱法检测硫酸镍中痕量氯离子  

Determination of trace chloride in nickel sulfate by ion chromatography

作　　者：刘肖[1] 汪琼[2] 施超欧[2] 叶明立[3] 蔡亚岐[1] 牟世芬[1] 

机构地区：[1]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 [2]上海华东理工大学测试中心,上海200237 [3]浙江大学化学系,浙江杭州310028

出　　处：《化学试剂》2006年第8期471-474,477,共5页Chemical Reagents

基　　金：国家重点基础研究计划(973项目);国家自然科学基金(20577058);中国科学院优秀博士论文科研基金资助

摘　　要：介绍并比较了离子色谱法检测硫酸镍中痕量氯离子的两种方法。选择的色谱条件分别为：（1）高容量氢氧化物选择性的IonPac AS11-HC阴离子交换柱，淋洗液自动发生装置在线产生KOH淋洗液等度淋洗，抑制型电导检测；（2）高容量碳酸盐选择性的IonPac AS9-HC阴离子交换柱，Na2CO3淋洗液等度淋洗，抑制型电导检测。在进样前需对固体样品进行溶解，NaOH沉淀，离心和过滤等简单前处理。这两种方法皆具备选择性好，灵敏度高，操作简单，节省时间，对环境友好等特点。实际样品检测结果显示，方法（1）的检出限为60ng／g（以固体样品实际浓度计）或0．3μg／L（以溶液浓度计），r=0．9999，连续7次进样所得RSD为1．43％，回收率为96．6％-101．2％；方法（2）的检出限为170ng／g（以固体样品实际浓度计）或1．7μg／L（以溶液浓度计），r=0．9994，连续7次进样所得RSD为1．65％，回收率为97．4％-103．9％，所得结果均令人满意。The present paper introduced and compared two methods in which pretreated solid samples by dissolving, precipitating, centrifuging and filtrating followed by separating analytes by different high capacity ion chromatography columns and detecting chloride in nickel sulfate by suppressed conductivity detector.The separation and determination of chloride were obtained by （1） high capacity hydroxyl selectivity lonPac ASll-HC column together with KOH isocratic eluent obtained by Eluent Generator and suppressed conductivity detector and （2） high capacity carbonate selectivity IonPac AS9-HC column together with manual prepared Na2CO3 isocratic eluent and suppressed conductivity detector. In Method （1）, the method detection limit was 60 ng/g （calculated by the concentrations in solid samples） or 0.3 μg/L （calculated by the concentration in solutions）, linear coefficient was 0.9999, BSD was 1.43 % and recoveries were between 96.6% - 101.2%.In Method （2）, the method detection limit was 170 ng/g （calculated by the concentrations in solid samples） or 1.7μg/L （calculated by the concentration in solutions）, linear coefficient was 0.9994, RSD was 1.65 % and recoveries are between 97.4% - 103.9% . Both of above methods possessed the advantages of good selectivity, high sensitivity, distinguished flexibility, easily operation, time-saving and friendly to the environment.

关 键 词：离子色谱 氯离子 硫酸镍 高容量色谱柱 前处理 

分 类 号：O613.42[理学—无机化学]