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氯代磺酚C测定铌已广泛应用在钢铁及非金属材料中。它是现有测铌方法中灵敏度较高的显色剂,能在酸度高范围宽的条件下显色,但用于炉渣中铌的测定文献报导很少。我们对试样的分解、钙的干扰做了实验;炉渣是由复杂的硅酸盐组成,碱熔融效果虽好,但时间长。稀盐酸溶解往往不完全,加入一定量氢氟酸溶解;同时铌与氟离子生成络合物,防止了铌的水解。溶后加高氯酸驱氟,加酒石酸络合铌,並能掩蔽微量的钒、钼、钛等元素。实验表明,在盐酸介质中EDTA存在下,Si(Ⅳ),Al(Ⅲ)、Mg(Ⅱ)、Ti(Ⅳ)、Cu(Ⅱ)、Mn(Ⅱ)、P(Ⅴ)无干扰,大量铁,100微克钼、钽以参比液抵消。200微克以上的钼使结果偏高。50微克V(Ⅴ),Cr(Ⅵ)使吸光度降低,加抗坏血酸溶液消除之。大量的Ca(Ⅱ)有干扰,在测铌的条
Determination of chlorosulfonamide niobium has been widely used in steel and non-metallic materials. It is the most sensitive reagent in the existing niobium test. It can develop color under a wide range of acidity, but there is little report about the determination of niobium in slag. We conducted an experiment on the decomposition of the sample and the interference of calcium. The slag is composed of complex silicates, and the alkali melting effect is good but it takes a long time. Dissolved dilute hydrochloric acid is often incomplete, adding a certain amount of hydrofluoric acid dissolved; the same time niobium and fluoride ions to form complexes to prevent niobium hydrolysis. Dissolved perchloric acid fluoride, tartaric acid complex niobium, and can mask a trace of vanadium, molybdenum, titanium and other elements. Experiments show that there is no interference between Si (Ⅳ), Al (Ⅲ), Mg (Ⅱ), Ti (Ⅳ), Cu (Ⅱ), Mn (Ⅱ) and P (Ⅴ) in the presence of EDTA in hydrochloric acid medium. , 100 micrograms of molybdenum, tantalum to reference solution offset. More than 200 micrograms of molybdenum makes the result high. 50 micrograms of V (V), Cr (VI) to reduce the absorbance, plus ascorbic acid solution to eliminate it. Large amounts of Ca (II) interfere with the measurement of niobium