摘要
建立了用硅胶整体柱和直接电导检测的离子对色谱快速分析碘离子的方法。采用Chromolith Speed ROD RP-18e色谱柱,以氢氧化四丁铵(离子对试剂)-邻苯二甲酸+乙腈(有机改进剂)为淋洗液,讨论了离子对试剂浓度、有机改进剂浓度、pH、流速和色谱柱温度对碘离子保留的影响。确定最佳色谱条件为:0.25 mmol/L氢氧化四丁铵-0.18 mmol/L邻苯二甲酸+体积分数7%乙腈(pH5.5)作为淋洗液,流速6.0 mL/min,色谱柱温30℃。在此条件下,碘离子的保留时间在0.5 min之内,其它常见阴离子(Cl-、NO3-、SO42-)及SCN-、ClO4-不干扰测定。方法的检出限为0.86 mg/L,标准曲线的线性范围为1.6～85.0 mg/L,峰面积的相对标准偏差为2.3%。将方法应用于测定地下水和果汁中的碘离子,加标回收率为98.5%～104.2%。
An ion-pair chromatographic method for the fast analysis of iodide has been developed using a silica-based monolithic column and direct conductivity detection.Chromatographic separation was performed on a Chromolith Speed ROD RP-18e column with tetrabutylammonium hydroxide（TBAH）-phthalic acid＋acetonitrile as eluent.The effects of eluent concentration,eluent pH,column temperature and flow rate on retention time of iodide were investigated.The optimized chromatographic conditions for the determination of iodide were as follows： using 0.25 mmol/L TBAH-0.18 mmol/L phthalic acid＋7% acetonitrile（pH 5.5） as the eluents, column temperature 30 ℃ and a flow rate of 6.0 mL/min.Retention time of iodide is less than 0.5 min under the optimal conditions.Common anions（Cl-,NO3-,SO42-） and SCN-,ClO4-do not interfere with the determination of iodide.Detection limit（S/N=3） for iodide was 0.86 mg/L.Calibration graph of peak area was linear in the range of 1.6～85.0 mg/L.Relative standard deviation of chromatographic peak area was 2.3%（n=5）.The method has been applied to the determination of iodide in groundwater and juices.Recoveries of iodide after spiking were 98.5%～104.2%.
出处
《分析试验室》
CAS
CSCD
北大核心
2010年第3期85-88,共4页
Chinese Journal of Analysis Laboratory
基金
黑龙江省自然科学基金(B200909)
哈尔滨师范大学科技发展预研(08XYG-15)项目资助
关键词
整体柱
离子对色谱
碘离子
电导检测
Monolithic column
Ion-pair chromatography
Iodide
Conductivity detection
