化学转化-气相色谱法测定氮化硅中的游离硅

建立了用化学转化－气相色谱法测定氮化硅中游离硅的分析方法。游离硅和氮化硅与熔融的氢化钠反应，排出氢，氨和少量二氧化碳和水蒸汽。吸收除去氨、二氧化碳和水蒸汽后，用热导检测器检测氢。方法简便，准确，平均回收率为９６％，相对标准偏差〈５％。

Determination of Free Silicon in Silicon Nitride by Chemical Conversion-Gas Chromatography

A chemical conversion-gas chromatography was studied for the determination of free silicon in silicon nitride. The method was based on the chemical conversion of fiee silicon and silicon nitride into hydrogen and ammonium, respectively. Free silicon and silicon nitride reacted with melten sodium hydroxide and released hydrogen ammonium small amount of carbon dioxide and water vapour. Hydrogen was then separated by absorbing NH3, CO2 and H2O and was measured by using a thermal conductivity detector, the mediod is simple, accurate. The average recovery is 96.1 % and the RSD of the results was less than 5% .