Jiaming Liu, Wenqi Li, Xuelin Li, Hailing Chen, Qiaomei Lu, Longdi Li, Zhimin Li, Guohui Zhu, Cuilian Chen
Department of Chemistry, Zhangzhou Normal College, Zhangzhou 363000, PR China.
Spectrochim Acta A Mol Biomol Spectrosc. 2005 Oct;61(13-14):3077-81. doi: 10.1016/j.saa.2004.11.033. Epub 2005 Jan 26.
Luminescent particles of lead carboxymethyl cellulose (Pb(CMC)2) containing salicyl fluorones (THBF), Pb(CMC)2-THBF were synthesized by the sol-gel method, using sodium carboxymethyl cellulose (NaCMC) as precursor and Pb2+ as precipitant. Pb(CMC)2-THBF can emit the intense and stable solid substrate room temperature phosphorescence (SS-RTP) on filter paper. And EDTA can chelate Pb2+ in Pb(CMC)2-THBF, causing it to decompose into aqueous soluble components PbY2-, CMC- and THBF, which can react with Ag+ to form Ag(CMC)2-THBF, causing the decrease of phosphorescence intensity. Based on the facts above, a new method for the determination of trace silver by SS-RTP quenching method was established. The linear range of this method is 8.0-40.0 fg spot(-1) (20.0-100.0 pg ml(-1)), with a detection limit (LD) of 2.2 fg spot(-1) (corresponding to a concentration range of 5.5 x 10(-13) g ml(-1)), and the regression equation of working curve is DeltaI(p) = 12.56 + 0.5527C(Ag+) (fg spot(-1), 0.4 microl spot(-1)), n = 8, r = 0.9992. This method has been applied to the determination of trace silver in human hair and tea sample with satisfactory results. The mechanism of SS-RTP emission is also discussed.
以羧甲基纤维素钠(NaCMC)为前驱体、Pb²⁺为沉淀剂,采用溶胶 - 凝胶法合成了含水杨基荧光酮(THBF)的羧甲基纤维素铅(Pb(CMC)₂)发光颗粒,即Pb(CMC)₂ - THBF。Pb(CMC)₂ - THBF能在滤纸上发射强烈且稳定的固体基质室温磷光(SS - RTP)。而EDTA能螯合Pb(CMC)₂ - THBF中的Pb²⁺,使其分解为水溶性成分PbY²⁻、CMC⁻和THBF,它们能与Ag⁺反应形成Ag(CMC)₂ - THBF,导致磷光强度降低。基于上述事实,建立了一种用SS - RTP猝灭法测定痕量银的新方法。该方法的线性范围为8.0 - 40.0 fg spot⁻¹(20.0 - 100.0 pg ml⁻¹),检测限(LD)为2.2 fg spot⁻¹(对应浓度范围为5.5×10⁻¹³ g ml⁻¹),工作曲线的回归方程为ΔI(p)=12.56 + 0.5527C(Ag⁺)(fg spot⁻¹,0.4 μl spot⁻¹), n = 8, r = 0.9992。该方法已应用于人体头发和茶叶样品中痕量银的测定,结果令人满意。还讨论了SS - RTP发射的机理。