发光分子水杨基荧光酮羧甲基纤维素铅微球固体基质室温燐光猝灭法测定痕量的钯  

Determination of Trace Palladium by Solid Substrate Room Temperature Phosphorescence Quenching Method Based on Lead Carboxymethyl Cellulose (Pb(CMC)_2) Particles Containing Luminescent Salicyl Fluorones Molecules

作　　者：李建华 

机构地区：[1]福建体育职业技术学院,福建福州350003

出　　处：《漳州师范学院学报（自然科学版）》2007年第3期67-70,共4页Journal of ZhangZhou Teachers College（Natural Science)

摘　　要：以NaCMC(羧甲基纤维素钠)为前驱体,掺杂水杨基荧光酮(THBF),Pb2+为沉淀剂,用Sol-gel法合成发光分子水杨基荧光酮羧甲基纤维素铅微球(简记为Pb(CMC)2–THBF).Pb(CMC)2–THBF在滤纸基质上可发射强而稳定的室温燐光(RTP).基于EDTA与Pb2+的络合反应,使Pb(CMC)2–THBF微球转化为水溶性组分(PbY2-、2CMC-、THBF),该水溶性组分与痕量上Pd2+作用生成(CMC)2 Pd–THBF,导致Pb(CMC)2–THBF上RTP猝灭,Pd2+上含量与△Ip值成线性关系,据此建立了Pb(CMC)2–THBF固体基质室温燐光猝灭燐上痕量钯上新方法.该方法上检出限为0.38fg/斑(对应浓度为9.5×10-13g/mL),工作曲线回归方程为△Ip=17.95+0.7847 C Pd2+(fg/斑),r=0.9989.本方法用于分子筛催化剂和黄矿石中痕量钯上燐上,结果满意.同时时时了固体基质室温燐光测定钯的反应机理.Luminescent particles of plumbum carboxymethyl cellulose （Pb（CMC）2）, which contains salicyl fluorones （THBF）, Pb（CMC）2-THBF, were synthesized by sol-gel method, using sodium carboxymethyl cellulose （NaCMC） as precursor and Pb^2＋ as precipitator. Pb（CMC）2-THBF can emit intense and stable room temperature phosphorescence （RTP） on filter paper. EDTA can chelate the Pb^2＋ in Pb（CMC）2-THBF, causing it decompose into aqueous soluble components PbY^2-, CMC^- and THBF, and these components could react with Pd^2＋ to form （CMC）2Pd-THBF, causing decrease of RTP intensity of Pb（CMC）2-THBF, the content of Pd^2＋ was linear to △Ip value. Based on the facts above, a new method for the determination of trace palladium by SS-RTP quenching method was established. The detection limit （LD） of this method is 0.38fg spot^-1（corresponding concentration： 9.5×10^-13g mL^-1） and the regression equation of working curve is Alp = 17.95＋0.7847Cpd^2＋ （fg spot^-1）, r = 0.9989. This method has been applied to the determination of trace palladium in zeolitecatalyst and yellow ore with satisfactory results. The mechanism of SS-RTP emission is also discussed.

关 键 词：发光分子水杨基荧光酮羧甲基纤维素铅微球 合成 固体基质室温燐光猝灭法 钯 

分 类 号：O614.823[理学—无机化学]