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在表面活性剂存在下,水杨基荧光酮,对羟基苯基荧光酮光度法等测定锆已有报道.邻氯苯基荧光酮(o-CPF)由于邻位强吸电子基氯的影响,与锆的反应灵敏度更高,可在更强的酸性介质中反应,选择性更好,实验证明:在0.4mol·L~(-1)盐酸介质中,锆与粼氯苯基荧光酮和溴化十六烷基三甲铵形成橙红色络合物,该络合物,络合物5分钟内显色完全,40分钟内基本不变,组成比在,0~12μg/25ml锆浓度范围内符合比尔定律。由于体系在较强的酸性介质中进行,大量的SO_4~(2-)、NO_3~-、Ca(Ⅱ)、Cu(Ⅱ)等不干扰测定,Fe(Ⅲ)及少量Ti(Ⅳ)、Mo(Ⅵ)干扰测定,可根据显色快慢消除Ti影响,用盐酸羟胺及抗坏血酸混用消除Fe(Ⅲ)及Mo(Ⅵ)影响。此法灵敏度高、选择性好,方法简单快速,可用于钢铁中微量锆的直接测定。
In the presence of surfactants, such as salicylfluorone and p-hydroxyphenylfluorone spectrophotometry have been reported. The o-chlorophenylfluorone (o-CPF) The reaction with zirconium is more sensitive and can react in more acidic medium with better selectivity. Experiments show that in the 0.4 mol·L -1 hydrochloric acid medium, zirconium and gliphenylfluorone and bromine The cetyltrimethylammonium formed an orange-red complex which developed completely within 5 minutes and remained essentially unchanged within 40 minutes with a compositional ratio within the range of 0-12 μg / 25 ml of zirconium Bill’s law. As the system was carried out in a strong acidic medium, a large amount of Fe (Ⅲ) and a small amount of Ti (Ⅳ), Mo (Ⅱ), Mo (Ⅵ), the effect of Ti can be eliminated according to the color developing speed and the effect of Fe (Ⅲ) and Mo (Ⅵ) can be eliminated by the mixture of hydroxylamine hydrochloride and ascorbic acid. This method has high sensitivity, good selectivity, simple and rapid method, can be used for direct determination of trace zirconium in steel.