目前报导微量锆的极谱测定法的文献尚不多见。文献[1—3]报导过锆的极谱测定法。文献[1]报导的方法灵敏度较低,文献[2]报导的方法在应用中需经过有机溶剂萃取分离干扰元素。对于锆这种电活性特殊的元素,寻找一些灵敏度及选择性都较好的极谱测定法,这在理论上及实际应用上都是很有意义的。 文献[4]曾提出,含胂羧基的偶氮化合物与锆形成的络合物,能产生较灵敏的导数示波极谱波,无肿羧基的偶氮化合物则无此特性。我们发现,在一定浓度的硝酸介质中,在安替比林存在下,许多不含胂羧基的偶氮化合物,例如硝基磺酚M、硝基磺酚C、硝基磺酚K、氯代磺酚C、偶氮硝羧、偶氮氯膦Ⅲ、偶氮氯膦mk等与锆形成的络合物,也能产生较灵敏的导数示波极谱波,而且波 At present, the literature about polarographic determination of trace zirconium is still rare. Literature [1-3] reported zirconium polarography. The method reported in [1] has low sensitivity. The methods reported in [2] need to be separated by organic solvent extraction in the application. For zirconium, the special element of electro-activity, looking for some of the better sensitivity and selectivity of the polarographic determination method, which in theory and practical applications are of great significance. It has been proposed in [4] that azo complex containing arsine and zirconium complex can produce more sensitive derivative oscillopolarographic waveforms, while the azo compound without any carboxyl group has no such characteristic. We have found that in a certain concentration of nitric acid medium, many azo compounds not containing arsine carboxyl groups, such as nitrosulphol M, nitrethulol C, nitrosulphol K, chlorinated Sulfonamide C, azocarboxylate, chlorophosphonazo III, chlorophosphonazo mk and zirconium complexes formed, but also can produce more sensitive derivative oscillopolarographic polarographic wave, and the wave