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阐述了一种采用高氯酸脱水重量法测定氮化硅铁中硅的方法。以氢氧化钠作为熔剂,于镍坩埚内熔融分解试料,采用高氯酸冒烟使硅酸脱水凝聚,以硫酸-氢氟酸加热处理沉淀,使硅成四氟化硅挥发,根据前后质量差求得硅的含量,滤液中的硅采用电感耦合等离子体原子发射光谱法(ICP-AES)测定,两者之和即为试料中的硅含量。通过试验考察了熔剂选择、熔剂加入量、试样称取量、熔融温度、熔融时间、高氯酸脱水以及ICP-AES测定条件等因素。结果表明,该方法具有较好的准确度及精密度,能满足生产检验的要求。
A method for determination of silicon in ferrosilicon nitride by perchlorate dehydration gravimetry is described. Using sodium hydroxide as a flux, the sample is melted and decomposed in a nickel crucible, the silicic acid is dehydrated and condensed by smoking with perchloric acid, the precipitate is heated and treated with sulfuric acid-hydrofluoric acid to volatilize silicon into silicon tetrafluoride, The difference of silicon content was determined. The content of silicon in the filtrate was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The sum of the two was the silicon content in the sample. The parameters of flux selection, flux addition, sample weight, melting temperature, melting time, dehydration of perchlorate and the determination conditions of ICP-AES were investigated. The results show that the method has good accuracy and precision, which can meet the requirements of production inspection.