对安替比林偶氮苯甲酸固相萃取分光光度法测定钯的研究  

Study on solid phase extraction and spectrophotometric determination of palladium with p-antipyrinylazo benzoic acid

作　　者：黄章杰[1] 黄锋[2] 谢琦莹[2] 

机构地区：[1]昆明理工大学材料与冶金工程学院,云南昆明650093 [2]云南大学化学系,云南昆明650091

出　　处：《冶金分析》2007年第11期17-20,共4页Metallurgical Analysis

基　　金：云南省自然科学基金(2005E0003Z);云南省教育厅科学研究基金(5Z0103A)

摘　　要：合成了新试剂对安替比林偶氮苯甲酸（AABA），根据其与钯的显色反应及C18固相萃取小柱对显色络合物的固相萃取，建立了一种测定痕量钯的新方法。在pH3．5～5．5的乙酸一乙酸钠缓冲介质中，有乳化剂OP存在下，钯与AABA发生反应形成1：2的稳定络合物，该络合物可用C18固相萃取小柱富集，小柱上富集的络合物用乙醇洗脱后用分光光度法测定。在富集后的测定液中，络合物最大吸收波长为452nm，表观摩尔吸光系数ε=1．22×10^5L·mol^-1·cm^-1，Pd^2＋含量在0．1～1．5μg／mL内符合比尔定律，方法用于测定催化剂中钯的含量，结果与原子吸收光谱法相一致。A new reagent p-antipyrinylazo benzoic acid（AABA）was synthesized. Based on its color reaction with palladium（Ⅱ）and the solid phase extraction of its colored complex with C18 cartridge,a new method for the determination of palladium was studied. In the presence of OP and in HAc-NaAc buffer solution（pH3.5-5.5）medium, AABA reacts with palladium（Ⅱ）to form a stable 2 ： 1 complex. The colored complex extracted by C18 cartridge can be eluted with ethanol and is determined by spectrophotometry at 452 nm. Beer＇s law is obeyed in the range of 0. 1-1. 5 μg/mL for palladium and ε=1.22×10^5L·mol^-1·cm^-1. The method was applied to determine the trace palladium in the Pt/Pd catalysts and the results found were agreement with those of AAS method.

关 键 词：对安替比林偶氮苯甲酸 固相萃取 钯 

分 类 号：O657.3[理学—分析化学]