高效阴离子交换色谱-脉冲安培检测器测定工业醋酸中痕量碘离子的方法  

High performance anion exchange chromatography hyphenated with pulsed amprometric detector for determination of trace iodide in industrial acetic acid

作　　者：梁立娜[1] 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

出　　处：《分析试验室》2005年第11期66-69,共4页Chinese Journal of Analysis Laboratory

基　　金：国家重点基础研究计划(973项目)资助课题(2003CB415001)

摘　　要：用一次性银电极高效阴离子交换色谱-脉冲安培检测器(HPAEC-PAD)研究了36%HAc中痕量碘离子的测定方法。用5 mL分析纯HAc(36%,不含碘离子)配制碘离子的标准工作溶液,然后加入一定体积的质量分数为25%NaOH溶液中和HAc,待溶液冷却至室温后用Milli-Q水定容至10 mL,最后用高效阴离子交换色谱-脉冲安培检测器分离测定,得到碘离子的标准工作曲线。工业醋酸样品经同样处理步骤。方法的检出限为0.06μg/L(3倍基线噪音),定量限为0.2μg/L(10倍基线噪音)。10μg/L碘离子的加标回收率为105%,5次连续测定的相对标准偏差为3.4%。A method using disposable silver working electrode high performance anion exchange chromatography（HPAEC） hyphenated with pulsed amprometric detector for the determination of trace iodide in acetic acid （36 % ） was proposed. Different concentrations of iodide standard solutions were prepared in 5 mL of acetic acid （36%, analytical grade）. Then 25% （w/w） NaOH was added to neutralize acetic acid. After the solution was cooled to room temperature, Milli-Q water was added to 10 mL. And this final solution was injected to HPAEC-PAD equipment to get the working curve. The industrial acetic acid samples were processed at the same way as the standards. The detection limit and quantitative limit of this method were 0.06 μg/L （three times of the noise） and 0.2μg/L （ten times of the noise）, respectively. No iodide was detected in industrial acetic acid samples. The spiking recovery of 10μg/L iodide was 105% and the RSD was 3.4% （n=5）.

关 键 词：HAC 碘离子 一次性银电极 离子色谱 脉冲安培检测 

分 类 号：O658.1[理学—分析化学]