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在pH 1.3～2.4的酸性介质中,亚硝酸盐与间苯二酚发生亚硝化反应,亚硝基产物再与氧锆基离子形成一种淡黄色的螯合物。据此作者拟定了一个分光光度微量测定水中亚硝酸盐的方法,为亚硝酸盐测定提供了一个新途径。此法简单、快速,选择性和重现性均好,有色产物稳定;仅磷酸盐和铁(Ⅲ)离子浓度超过亚硝酸盐离子八倍时产生较严重的干扰;但于试剂中加入适量的硫酸可防止磷酸盐的干扰,铁(Ⅲ)离子可用阳离子交换树脂处理除去。若有银离子存在时,须用硝酸氧锆代替氧氯化锆。[试剂] 溶液甲:溶解1 g间苯二酚和1 g氧氯化锆(ZrOCl_2·8 H_2O)于含有7.5 ml浓盐酸的重蒸馏水中,并稀释至500 ml。溶液乙:溶解1 g硫酸钠和1.5 g
In an acidic medium at pH 1.3 to 2.4, nitrite reacts with resorcinol and the nitroso product forms a light yellow chelate with the zirconyl radical. Accordingly, the authors developed a method for spectrophotometric determination of nitrite in water, which provided a new way for the determination of nitrite. This method is simple, rapid, selectivity and reproducibility are good, the colored product is stable; only phosphate and iron (III) ion concentration exceeds the nitrite ion eight times more serious interference; but in the reagent by adding appropriate amount of Sulfuric acid can prevent the interference of phosphate, and the iron (III) ions can be removed by cation exchange resin treatment. In the presence of silver ions, zirconyl nitrate should be replaced by zirconium oxychloride. [Reagent] Solution A: Dissolve 1 g resorcinol and 1 g zirconium oxychloride (ZrOCl 2 .8 H 2 O) in double distilled water containing 7.5 ml concentrated hydrochloric acid and dilute to 500 ml. Solution B: Dissolve 1 g of sodium sulfate and 1.5 g