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Journal of the Korean Chemical Society (JKCS)

ISSN 1017-2548(Print)
ISSN 2234-8530(Online)
Volume 8, Number 4
August 20, 1964 

A New Gas-Chromatographic Method of Organic Elemental Analysis

가스크로마토그래피에 의한 미량원소분석
You Sun Kim, Youn Soo Son, Q. Won Choi

김유선, 손연수, 최규원
미량원소분석용 연소로 내에서 내부산화제(산화은과 이산화 망간의 혼합물)와 함께 유기시료를 헤륨 기류하에서 연소시키고 발생한 물은 칼슘카바이드관에 통하여 아세틸렌으로 변환시킨다. 이산환탄소와 아세틸렌을 molecular sieve 5A 관에 실온에서 흡착시킨 후 340℃까지 온도·프로그램법으로 탈착시켜 실리카겔겔관을 통하여 분별유출시키고 열전도식 검지기로 CO2와 C2H2를 정량하는 방법을 발전시켰다. 벤조산을 표준물질로 하여 작성한 검양선을 사용하여 각종 유기시료중의 탄소 및 수소함량을 분석한 평균오차가 탄소의 경우 ±0.33%이었다.

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℃ and the released gases were passed through a silica gel column. The adsorption of CO2 and C2H2 in the molecular sieve 5A trapping column were found to be quantitative and the silica gel column showed an excellent resolution of CO2 and C2H2 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 ±0.5% and ±0.33% for carbon and hydrogen, respectively.

188 - 191
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