微乳液介质-氯酚偶氮罗丹宁分光光度法测定微量钯  

Spectrophotometric determination of micro palladium with chlorophenolazo rhodanine in microemulsion medium

作　　者：陈文宾[1] 马卫兴[1] 许兴友[1] 徐国想[1] 

机构地区：[1]淮海工学院化学工程系,江苏连云港222005

出　　处：《冶金分析》2007年第9期73-76,共4页Metallurgical Analysis

基　　金：淮海工学院海洋生物技术重点建设实验室基金项目(2005HS010;2005HS001);江苏省科技厅自然科学基金(BK2005045);淮海工学院自然科学基金(Z2006)

摘　　要：研究了在自制的十六烷基三甲基溴化铵、正丁醇、正庚烷和水微乳溶液存在下,氯酚偶氮罗丹宁与Pd(的显色反应,建立了分光光度法测定微量PdⅡ的新方法。结果表明,在pH5.3的HAc-NaAc缓冲溶液中,Pd(与试剂形成1∶2的暗红色络合物,络合物的最大吸收峰在500nm波长处,表观摩尔吸光系数ε为1.79×105L.mol-1.cm-1。在10mL显色液中,Pd(量在0.01～12μg范围内符合比尔定律,检出限为0.0003μg/mL。本法可用于碳钯催化剂和含钯分子筛中微量钯的测定,回收率在98.1%～98.6%之间,RSD在1.17%～2.34%(n=6)范围内。The color reaction of the reagent chlorophenolazo rhodanine with Pd（Ⅱ） was studied in the presence of microemulsion consisting of CTMAB, n -C4 H9 OH, C7 H14 , H20. A new spectrophotometry for the determination of trace Pd（Ⅱ） has been proposed. Results show that the new color reagent reacts with Pd（Ⅱ） to form a stable red complex（1 ： 2） in the medium of HAc--NaAc buffer solution at pH 5.3. The maximum absorption wavelength and apparent molar absorptivity are 500 nm and 1.79 × 105 L · mol^-1· cm^-1 ,respectively. Beer＇s law is obeyed in the range of 0.01-12 μg for Pd（Ⅱ） in 10 mL of color solution. The detection limit is 0. 000 3 μg/mL. The method has been applied to the determination of trace Pd （Ⅱ） in palladium catalyst and molecular sieve with the RSDs of 1.17%--2.34% （n =6）and recoveries of 98. 1%--98.6%.

关 键 词：氯酚偶氮罗丹宁 分光光度法 钯 微乳液 

分 类 号：O657.3[理学—分析化学]