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作 者:郭会时[1] 肖鹏峰[1] 聂立波[1] 李益恒[2] 何农跃[1]
机构地区:[1]东南大学吴健雄实验室,南京210096 [2]湘潭大学化学系,湘潭411105
出 处:《Journal of Southeast University(English Edition)》2004年第2期221-225,共5页东南大学学报(英文版)
基 金:TheNationalNaturalScienceFoundationofChina(No .60 12 110 1) ,Trans CenturyTrainingProgrammeFoundationfortheTalentsbytheStateEducationCommission ,ChinaPostdoctoralScienceFoundation
摘 要:A sensitive method is described for the determination of trace antimony based on the antimony-bromopyrogallol red (BPR) adsorption at a carbon paste electrode (CPE). Three steps were involved in the overall analysis: preconcentration,reduction and stripping. Optimal conditions were found to be an electrode containing 25% paraffin oil and 75% high purity graphite powder as working electrode;a 0.10 mol/L HCl solution containing 40 μmol/L BPR as accumulation medium;a 0.20 mol/L HCl solution as reduction and stripping electrolyte;accumulation time,150 s;reduction potential and time,-0.50 V,60 s;scan range from -0.50 to 0.20 V. Interferences by other ions were studied as well. The detection limit was found to be 0.5 nmol/L for 150 s preconcentration. The linear range was from 1.0 nmol/L to 0.50 μmol/L. Application of the proposed method to the determination of antimony in water and human hair samples gave good results.根据锑与溴邻苯三酚红 (BPR)生成的络合物在碳糊电极上的吸附特性 ,建立了测定痕量锑的吸附伏安法 .整个分析过程分 3个步骤 :吸附富集、还原和溶出 .用单因素变化法得出最佳试验条件为 :以含 4 0 μmol/LBPR的 0 .10mol/LHCl为富集底液 ;富集时间 15 0s ;还原和溶出介质为 0 .2 0mol/LHCl;还原电位为 - 0 .5 0V ;还原时间为 6 0s ;扫描范围为 - 0 .5~ 0 .2 0V .考察了共存离子的影响 .二次导数溶出峰电流与锑 (Ⅲ )浓度在 1.0nmol/L~ 0 .5 0 μmol/L范围内呈良好的线性关系 ,检出限达 0 .5nmol/L .该方法已成功应用于人发和水样中锑的测定 .
关 键 词:ANTIMONY bromopyrogallol red carbon paste electrode adsorptive voltammetry
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