历年来,纯金属中微量硅的测定,为了取得较高的灵敏度和降低试剂空白值,大都使用酸法溶样。但钽、铌和多数难熔金属一样,必须加入氢氟酸才能将试样分解;通常为了防止硅以氟化物的形态跑掉,往往使反应缓慢地进行,溶样时间延续几小时。Simons等人曾指出,硅以氟硅酸盐存在时具有相当的热稳定性,氟硅酸钠的热离解约在327℃才变得显著,而氟硅酸钾 Over the years, the determination of trace silicon in pure metal, in order to obtain higher sensitivity and reduce the reagent blank value, the majority of the use of acid sample solution. However, tantalum and niobium, like most refractory metals, require the addition of hydrofluoric acid to decompose the sample; usually, to prevent the silicon from running off in the form of fluoride, the reaction tends to proceed slowly and the dissolution time extends for several hours. Simons et al. Have pointed out that silicon possesses considerable thermal stability in the presence of fluorosilicate, the thermal dissociation of sodium fluorosilicate only becomes significant at about 327 ° C, and potassium fluorosilicate