离子色谱阀切换快速测定六氟磷酸根及多种阴离子  

Fast Determination of Hexafluorophosphate,Fluorid,Chloride, Nitrate and Sulfate Inorganic Anions by Ion Chromatography with Valve Switching

作　　者：朱作艺[1] 许锦钢[1] 钟乃飞[2] 张培敏[1] 朱岩[1] 

机构地区：[1]浙江大学西溪校区化学系,杭州310028 [2]桂林理工大学化学与生物工程学院,桂林541004

出　　处：《分析化学》2011年第11期1738-1742,共5页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(Nos.20775070;J0830413);浙江省自然科学基金(Nos.R4080124;Y4090104;Y4090268)资助项目

摘　　要：建立了快速测定离子液体中六氟磷酸根（PF6^-）及其它常规阴离子（F^-，CI^-，NO3^-，SO4^2-的离子色谱阀切换方法。通过保护柱与分离柱的简单切换，使强保留离子PF6^-仅通过保护柱，缩短其流通路径，在较短时间内出峰，其它离子既通过保护柱又通过分离柱，从而达到快速同时分离的目的。样品经稀释溶解后直接进样，淋洗液选用KOH，流速为1．0mL／min，采用抑制型电导检测，外标法定量。PF6，F，C1，N03和SO4^2-的线性范围分别为1-200mg／L，0．1～25mg／L，0．1-5mg／L，0．1～5mg／L和0．1～5mg／L，线性相关系数均大于0．9995；加标回收率在86．5％～112．2％之间；相对标准偏差在1．4％～4．1％之间，检出限分别为8．9，0．41，0．44，1．2和1-2μg／L。本方法适用于一系列强弱保留离子同时分析的问题。A new method has been proposed for fast determination of hexafluorophosphate （PF6-） and some inorganic anions （F^- , C1^- , NO3^- , SO4^2- ）. It was accomplished by valve switching between anion exchange guard column and separation column connected in series. With strong retentive ion （PF6 ） only through guard column and the inorganic anions through both guard column and separation column, the separation was completed within a much shorter time. Under the optimum conditions, the linear ranges of the method for PF6^-, F , CI-, NO3 and SO4^2- were 1-200 mg/L （r=0. 9997）, 0.1-25 mg/L （r=0. 9995）, 0.1-5 mg/L（r=0. 9997）, 0.1-5 mg/L（r=0. 9997） and 0.1-5 mg/L（r=0. 9999）, whereas detection limits calculated at S/N=3 were 8.90, 0.41, 0.44, 1.23 and 1.20 gg/L, respectively. The recoveries were in the range of 86. 5%- 112.2% with the relative standard deviations of 1.4%-4.1%. The method could be applied to determine strong retentive and weak retentive ions simultaneously.

关 键 词：离子色谱 阀切换 离子液体 六氟磷酸根 阴离子 

分 类 号：O657.75[理学—分析化学]