본 연구에서는 GC/PFPD와 AS/TD를 연계한 저온농축 열탈착 시스템을 이용하여, 시료의 주입부피 증감에 따른 열탈착 회수율의 경향성을 파악하고자 하였다. 이를 위하여, 주요 악취물질에 속하는 환원황(reduced sulfur compounds: RSC) 성분들을 대상으로 비교실험을 진행하였다. 4가지 농도대로 준비한 RSC 표준시료(10, 20, 50, 100 ppb)를 각각 6개의 주입 부피(40, 80, 200, 400, 800, 1200 mL)로 조절하면서 검량자료를 확보하였다. 황화합물의 회수율 측정은 이론적 주입량과 실제 열탈착 회수 후 절대량을 비교하여 산출하였다. 본 연구의 결과, 시료의 주입 시간이 짧아서 정확한 주입 부피의 변화를 파악하기 어려운 영역과 주업부피가 50 ng 대를 넘어갈 때 cold trap의 파과에 따른 검출의 제한 영역이 동시에 존재하는 것을 파악할 수 있다. 따라서 TD분석은 최적화 조건의 설정이 무엇보다 중요하다는 것을 알 수 있다.
본 연구에서는 GC/PFPD와 AS/TD를 연계한 저온농축 열탈착 시스템을 이용하여, 시료의 주입부피 증감에 따른 열탈착 회수율의 경향성을 파악하고자 하였다. 이를 위하여, 주요 악취물질에 속하는 환원황(reduced sulfur compounds: RSC) 성분들을 대상으로 비교실험을 진행하였다. 4가지 농도대로 준비한 RSC 표준시료(10, 20, 50, 100 ppb)를 각각 6개의 주입 부피(40, 80, 200, 400, 800, 1200 mL)로 조절하면서 검량자료를 확보하였다. 황화합물의 회수율 측정은 이론적 주입량과 실제 열탈착 회수 후 절대량을 비교하여 산출하였다. 본 연구의 결과, 시료의 주입 시간이 짧아서 정확한 주입 부피의 변화를 파악하기 어려운 영역과 주업부피가 50 ng 대를 넘어갈 때 cold trap의 파과에 따른 검출의 제한 영역이 동시에 존재하는 것을 파악할 수 있다. 따라서 TD분석은 최적화 조건의 설정이 무엇보다 중요하다는 것을 알 수 있다.
In this study, the recovery rate of thermal desorbing (TD) method was investigated in relation to sample concentration and loading volume of reduced sulfur compounds (RSC). All the analysis of RSC was made by gas chromatography/pulsed flame photometric detector (GC/PFPD) combined with air server/the...
In this study, the recovery rate of thermal desorbing (TD) method was investigated in relation to sample concentration and loading volume of reduced sulfur compounds (RSC). All the analysis of RSC was made by gas chromatography/pulsed flame photometric detector (GC/PFPD) combined with air server/thermal desorber (AS/TD). The RSC measurement data were obtained by loading gaseous RSC standards prepared at 4 concentrations (10, 20, 50, 100 ppb) at 6 injection volumes (40, 80, 200, 400, 800, and 1200 mL). The recovery rates of each RSC were computed in terms of relationship between expected vs. measured values. According to our analysis, the following conclusions can be drawn. First, the results were less stable at short loading time (1 and 2 min at 40 mL/min) with reduced recovery rate, especially with light RSCs (H₂S and CH₃SH). On the other hand, at sufficiently high loading volume, their quantification was limited by off-scale peaks (at a near 50 ng) due to the breakthrough of cold trap in TD. Thus, the optimization of TD-based analysis may be considered as a prerequisite for analyzing the RSC in a reliable manner.
In this study, the recovery rate of thermal desorbing (TD) method was investigated in relation to sample concentration and loading volume of reduced sulfur compounds (RSC). All the analysis of RSC was made by gas chromatography/pulsed flame photometric detector (GC/PFPD) combined with air server/thermal desorber (AS/TD). The RSC measurement data were obtained by loading gaseous RSC standards prepared at 4 concentrations (10, 20, 50, 100 ppb) at 6 injection volumes (40, 80, 200, 400, 800, and 1200 mL). The recovery rates of each RSC were computed in terms of relationship between expected vs. measured values. According to our analysis, the following conclusions can be drawn. First, the results were less stable at short loading time (1 and 2 min at 40 mL/min) with reduced recovery rate, especially with light RSCs (H₂S and CH₃SH). On the other hand, at sufficiently high loading volume, their quantification was limited by off-scale peaks (at a near 50 ng) due to the breakthrough of cold trap in TD. Thus, the optimization of TD-based analysis may be considered as a prerequisite for analyzing the RSC in a reliable manner.
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