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铜的荧光法测定已有不少报道。有利用催化荧光法,而直接荧光法测定铜的报道不多。我们将绕丹宁与重氮盐偶联,合成新的荧光试剂5-(4-氯-2-羧基苯偶氮)绕丹宁(CCPAR)与CU(Ⅱ)反应,Cu(Ⅱ)与试剂在pH 5.0～5.4的邻苯二甲酸氢钾-氢氧化钠缓冲介质中形成配合物,用于测定铜元素。目前国内未见报道,该方法的特点是干扰少,灵敏度高,可测至0.5ng·ml~(-1)的Cu,不经分离,直接测定某些样品如茶叶中的铜,结果令人满意。 1 试验部分1.1 试剂与仪器铜标准溶液:1mg·ml~(-1),称取纯铜粉1.000g置于小烧杯中。加入浓硝酸3ml溶解,溶解完全后转入1000ml量瓶中,以水稀释至刻度。用时稀释至浓度为1μg·ml~(-1) CCPAR:由本实验室合成。经硅胶柱层析提纯,通过元素分析红外光谱,核磁共振谱和质谱鉴定,证明其
There have been many reports on the determination of copper by fluorescence method. The use of catalytic fluorescence method, and direct fluorescence method for the determination of copper is not reported. We synthesized a new fluorogenic reagent 5- (4-chloro-2-carboxyphenylazo) rhodanine (CCPAR) with CU (Ⅱ) by coupling tannin with diazonium salt. The reaction of Cu Complexes were formed in a potassium hydrogen phthalate-sodium hydroxide buffer at pH 5.0-5.4 for the determination of copper. At present, there is no report in our country. The method is characterized by less interference and high sensitivity. Cu can be measured to 0.5 ng · ml -1. Without any separation, the direct determination of Cu satisfaction. 1 Experimental 1.1 Reagents and Instruments Copper standard solution: 1mg · ml -1, weighed 1.000g of pure copper powder placed in a small beaker. Add concentrated nitric acid 3ml dissolved, dissolved completely transferred to 1000ml volumetric flask, diluted with water to the mark. Diluted with time to a concentration of 1μg · ml -1 CCPAR: synthesized by the laboratory. Purification by silica gel column chromatography, by elemental analysis of infrared spectroscopy, nuclear magnetic resonance and mass spectrometry identification, to prove that