Abe Kodai, Shimohira Koki, Miki Yusuke, Hirose Yasuo, Ohira Shin-Ichi, Toda Kei
Department of Chemistry, Kumamoto University, 2-39-1 Kurokami, Kumamoto 860-8555, Japan.
Tsukuba Laboratory, Taiyo Nippon Sanso Co., 10 Okubo, Tsukuba, Ibaraki 300-2611, Japan.
ACS Omega. 2020 Sep 30;5(40):25704-25711. doi: 10.1021/acsomega.0c02985. eCollection 2020 Oct 13.
A portable chemical analysis system for monitoring ambient carbonyl sulfide (COS) was investigated for the first time. COS is paid attention to from the perspectives of photosynthesis tracer, breath diagnosis marker, and new process-use in the manufacture of semiconductors. Recently, the threshold level value of COS was settled at 5 ppm in volume ratio (ppmv) for workplace safety management. In this work, COS was converted to HS by a small column packed with alumina catalyzer at 65 °C. Then, the HS produced was collected in a small channel scrubber to react with fluorescein mercuric acetate (FMA), and the resulting fluorescence quenching was monitored using an LED/photodiode-based miniature detector. The miniature channel scrubber was re-examined to determine its robustness and easy fabrication, and conditions of the catalyzer were optimized. When the FMA concentration used was 1 μM, the limit of detection and dynamic range, which were both proportional to the FMA concentration, were 0.07 and 25 ppbv, respectively. Ambient COS in the background level and even contaminated COS in the nitrogen gas cylinder could be detected. If necessary, HS was removed selectively by reproducible adsorbent columns. COS concentrations of engine exhaust were measured by the proposed method and by cryo-trap-gas chromatography-flame photometric detection, and the results obtained (0.5-5.9 ppbv) by the two methods agreed well ( = 0.945, = 19). COS in ambient air and exhaust gases was successfully measured without any batchwise pretreatment.
首次对一种用于监测环境中羰基硫(COS)的便携式化学分析系统进行了研究。COS从光合作用示踪剂、呼吸诊断标志物以及半导体制造新工艺用途等角度受到关注。最近,为了工作场所安全管理,COS的阈值水平设定为体积比5 ppm(ppmv)。在这项工作中,COS在65°C下通过填充有氧化铝催化剂的小柱转化为HS。然后,产生的HS在一个小通道洗涤器中收集,与荧光素汞乙酸酯(FMA)反应,并使用基于LED/光电二极管的微型探测器监测产生的荧光猝灭。对微型通道洗涤器进行了重新评估,以确定其耐用性和易于制造的特点,并对催化剂的条件进行了优化。当使用的FMA浓度为1 μM时,与FMA浓度成正比的检测限和动态范围分别为0.07和25 ppbv。可以检测到背景水平的环境COS,甚至氮气瓶中受污染的COS。如有必要,可通过可再生吸附柱选择性去除HS。用所提出的方法和低温捕集-气相色谱-火焰光度检测法测量了发动机尾气中的COS浓度,两种方法得到的结果(0.5 - 5.9 ppbv)吻合良好( = 0.945, = 19)。成功测量了环境空气和废气中的COS,无需任何分批预处理。