气相色谱法测定高纯三氯氢硅中的总碳含量

Determination of Total Carbon Contents in High Purity Trichlorosilane by Gas Chromatography

将高纯三氯氢硅中的含碳物质在氢气还原炉内转化成甲烷,利用配备氢火焰离子化检测器的气相色谱仪进行测定,最后换算成总碳的含量。结果发现,高纯三氯氢硅中的甲基二氯硅烷、甲基三氯硅烷、二甲基二氯硅烷等可能的含碳物质在转化炉内均具有良好的转化率,转化率大于85%。样品中含碳量的测定结果之间重复性好,精密度较高,相对标准偏差均小于10%。方法简单、快捷,准确度高,能很好地满足高纯三氯氢硅样品中对含碳物质的质量控制要求。

The carbon materials in the high purity trichlorosilane were firstly converted into methane in hydrogen reduction furnace, and then the methane content was determined by gas chromatography equipped with hydrogen flame ionization detector, which finally was converted into the content of total carbon. It was found that the possibly containing carbon materials such as methyl dichlorosilane, methyl trichlorosilane and dimethyl dichlorosilane had good conversion rates（〉85 ~）. The established method has good repeatability and high precision with the relative standard deviation （RSD） of less than 10~. It is simple, fast and high accurate, and could well meet the quality control requirements for analyzing carbon materials in the high purity trichlorosilane samples.