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用次甲基蓝比色测定某些含铌钽钢中微量硼时,常常遇到如下困难:铌钽的严重干扰;王水分解试样时氯化硼的挥发损失;某些硼化物如碳化硼、氮化硼以及铌钽的金属间硼化物等不易被王水和硫酸所分解等。为了解决这些问题,本文研究了用焦硫酸钾熔融试样,以水解方式分离铌钽,方法简单,效果较好,避免了卤化硼的挥发损失,并解决了难溶硼化物的溶样问题。本法适用于含铌钽的镍基、铁基和部分钴基合金中微量硼的测定。
The determination of trace amounts of boron in niobium-tantalum steels with methylene blue colorimetric often involves the following difficulties: severe interference with niobium-tantalum; volatilization of boron chloride during decomposition of the aqua regia; loss of certain borides such as carbonization Boron, boron nitride and niobium tantalum intermetallic boride are not easily broken by aqua regia and sulfuric acid. In order to solve these problems, this paper studied the dissolution of niobium tantalum by hydrolysis with potassium pyrosulphate. The method is simple, the effect is better, the volatilization loss of boron halide is avoided, and the problem of solute boricum is solved. This method is applicable to the determination of trace boron in nickel base, iron base and some cobalt base alloys containing niobium tantalum.