Abstract
A new gas-chromatographic method for determining carbon and hydrogen in organic compounds has been developed. After sample combustion was performed in a regular analytical combustion tube with an internal oxidant (a mixture of silver oxide and manganese dioxide) under a helium flow, the water produced was converted to acetylene by passing through a calcium carbide tube. The carbon dioxide and acetylene were trapped by a molecular sieve 5A column at room temperature. The trapped gases were released under programmed temperature raise up to $340^{\circ}C$ and the released gases were passed through a silica gel column. The adsorption of $CO_2$ and $C_2H_2$ in the molecular sieve 5A trapping column were found to be quantitative and the silica gel column showed an excellent resolution of $CO_2$ and $C_2H_2$ for analytical purpose. The analytical results for various known compounds based on the out-put of the thermal conductivity cell calibrated for the amounts of carbon and hydrogen contents in benzoic acid, showed average errors ${\pm}0.5%$ and ${\pm}0.33%$ for carbon and hydrogen, respectively.
微量元素分析用 燃燒爐 內에서 內部酸化劑(酸化銀과 二酸化 망간의 混合物)와 함께 有機試料를 헤륨 氣流下에서 燃燒시키고 發生한 물은 칼슘카바이드管에 通하여 아세틸렌으로 變換시킨다. 二酸化炭素와 아세틸렌을 molecular sieve 5A 管에 室溫에서 吸着시킨 후 $340^{\circ}C$까지 溫度${\cdot}$프로그탬法으로 脫着시켜 실리카켈管을 通하여 分別流出시키고 熱傳導式 檢知器로 $CO_2$와 $C_2H_2$를 定量하는 方法을 發展시켰다. 벤조酸을 標準物質로 하여 作成한 檢量線을 使用하여 各種 有機試料中의 炭素 및 水素含量을 分析한 結果 平均誤差가 炭素의 경우 ${\pm}0.5%$, 水素인 경우${\pm}0.33%$ 이었다.