难熔金属中痕量硅的测定主要是空白值问题,而决定空白值的关键在于溶样方法。现行的碱熔分离法、氢氟酸、氢氟酸-硝酸溶样法不仅灵敏度较低(n×10~(-8)％),而且重现性也不太好。Stoburt所提出的蒸馏法,由于仍使用氢氟酸-硝酸溶样,方法的灵敏度也只能达到～5×10~(-4)％。由于这些方法使用氢 The determination of trace amounts of silicon in refractory metals is primarily a matter of blank value, and the key to determining the blank value lies in the sample-dissolving method. Current alkali fusion method, hydrofluoric acid, hydrofluoric acid - nitric acid solution method not only low sensitivity (n × 10 -8%)), but also not very good reproducibility. Stoburt’s proposed distillation method, due to the still hydrofluoric acid-nitric acid sample, the sensitivity of the method can only reach ~ 5 × 10 ~ (-4)%. Because these methods use hydrogen