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新荧光试剂3-对甲苯基-5-(2’-羧基苯偶氮)绕丹宁的合成及荧光光度法测定蚕丝制品中痕量铜的研究
Synthesis and Analytical Application ofa New Fluorescent Reagent 3-p-Tolyl-5-(21-Carboxyphenylazo)Rhodanine
【摘要】 本文报道了新荧光试剂3-对甲苯基-5-(2’-羧基苯偶氨)绕丹宁(PM-PRACP)的合成。用元素分析、红外光谱、核磁共振氢谱和质谱确证了其结构,研究了其荧光性质。在pH5.6时,该试剂与Cu ̄(2+)形成稳定的荧光螯合物,且在λ_(ex)/λ_(em)=305nm/405nm产生强烈荧光。其荧光强度与Cu ̄(2+)的浓度在0~1.6μg/25mL范围内呈线性关系,检测限为5×10 ̄(-4)μg/g。已用于痕量铜(Ⅱ)的荧光分光光度法测定。测定了蚕茧、蚕丝和丝绸中的痕量铜,结果满意。
【Abstract】 This paper reports the synthesis of 3-p-tolyl-5-(2’-carboxyphenylazo)rhodanine(PMPRACP ).5.6g o-aminobenzoic acidwas made into diazonium salt , then coupledwith 5. 6g 3-p-methylrhodanine in ammoniawater,giving yellow needle crystals,m,p.164~166℃,The product has been con-firmed by elemental analysis , IR , HNMRand MS.A fluorescence analytical methodfor Cu(Ⅱ)was developed with this reagent.Toa 25 mL volumetric flaskwese added 1mL1.0μg/mL Cu(Ⅱ) working solution,0. 5mL1×10 ̄(-4)mol.L ̄(-1)PMPRACP solution and2mL pH5.66 buffer solution,the mixtusewas thenheated for 30 min to form the fluo-rescent chelate, and measured at λex/λem=305nm/405nm, There is a linear relationshipbetween the fluorescence intensity and con-centration of Cu ̄(2+) in the range of 0-1.6μg/25mL, The detection limit is 5 × 1 0 ̄(-4) μg/g.The reagent has been used in fluorimetricdetermination of trace Cu in cocoon, naturalsilk and silk cloth with satisfactory results.
【Key words】 p-tolyl-5-(2’-car-boxyphenylazo)rhodanine; synthesis,fluo-rescence analysis,fluorescence reagent;
- 【文献出处】 分析试验室 ,ANALYTICAL LABORATORY , 编辑部邮箱 ,1995年06期
- 【分类号】O657.3
- 【被引频次】11
- 【下载频次】75