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研究生: 劉勇村
論文名稱: 建立水中揮發性有機化合物之現場自動化即時連續監測吹氣捕捉/氣象層析分析系統
Construction of In-situ Automatic Continual Monitoring of VOCs In Water by Purge and Trap/Gas Chromatography System
指導教授: 羅俊光
吳劍侯
口試委員:
學位類別: 碩士
Master
系所名稱: 原子科學院 - 生醫工程與環境科學系
Department of Biomedical Engineering and Environmental Sciences
論文出版年: 2004
畢業學年度: 92
語文別: 中文
論文頁數: 123
中文關鍵詞: 吹氣捕捉揮發性有機化合物即時監測
外文關鍵詞: VOCs, purge and trap, wastewater, in-situ monitoring
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  • 本研究使用PSM連續式自動進樣器搭配矽烷化不□鋼管作為進樣裝置,以吹氣捕捉裝置為前濃縮方法,再利用氣相層析/火焰游離偵檢器做為分析儀器,並設置一套自動化管路清洗系統,完全由商業化的自動吹氣捕捉裝置控制,如此建立一套可用於分析現場的現場自動化即時連續監測分析系統,可同時分析水中17種高科技產業常見的揮發性有機化合物,包括丙酮(Acetone)、三氯甲烷(Chloroform)、苯(Benzene)、甲苯(Toluene)及萘(Naphthalene)等有機化合物,本方法的各物種校正曲線R-Square值均高於0.993,方法偵測極限丙酮(Acetone)為9.07ppb,其他物種介於0.32~2.39pbb,精確度在15%之內,準確度介於0.27%~23.54%,適合用於長時間即時連續監測。
    本研究並在5月26日凌晨至28日下午五時及6月15日晚間九時至17日中午12時於污水廠放流口進行現場連續分析,由結果可看出監測期間內所測得物種的總濃度分佈趨勢,也可了解各別物種濃度對時間的關係,由所得數據可知丙酮(Acetone)在分析物種總濃度佔有很高比例,其他例如三氯甲烷(Chloroform)、三氯乙烯(Trichloroethylene)、甲苯(Toluene)、二氯苯(1,4-Dichlorobenzene)、三氯苯(1,2,4-Trichlorobenzene)以及萘(Naphthalene)等化合物也在本次的現場即時監測中被偵測出。


    ABSTRACT
    For real-time monitoring of VOCs in wastewater discharged from high-tech industries, an automatic sampling device, process sampling module (PSM) connected with PT-GC-FID system was developed. The system was designed to simultaneously monitor 17 compounds, including one polar compound, acetone, and 16 non-polar compounds, such as benzene, toluene, chloroform, etc. The trapping tube designed is 20 cm in length and 1/8” in O.D, and was packed with two adsorbents, carbopackB and carbosieve III, to trap the target compounds. For the purpose of in-situ monitoring, the flush of sampling tube composed of two two-way valves and one time controller to prevent the absorption interference of the residual. The optimum condition for the analytical system was 12min of purge time at 60℃ (purge temperature) and 4min of desorption time at 260℃ (desorption temperature). Good chromatograms were obtained with the developed analytical system even if cryogenic device and de-mist process were not used. The precision was high (RSD 1.99%~13.35%) and the accuracy was achieved at the level between 0.27% to 23.54%. The method detection limits ranged from 0.32 to 2.39 ppb. Variations of the VOCs concentration in wastewater discharged from high-tech industries were obtained and recorded from two times three day sampling campaign during 2004/05/26 to 2004/05/28 and 2004/06/15 to 2004/06/17.

    總目錄 摘要 i 英文摘要(Abstract) ii 總目錄 iii 圖目錄 vi 表目錄 x 謝誌 xiii 第一章 緒論 1 1.1 研究緣起 1 1.2 研究目的 2 1.3 研究方法 3 第二章 文獻回顧 5 2.1 環境樣品前處理技術 5 2.2 吹氣捕捉(Purge & Trap, P&T)方法說明 5 2.2.1 吹氣捕捉方法之原理 6 2.2.2 影響P&T之操作參數 9 2.2.3 捕集管內固體吸附劑的選擇 12 2.2.4 實驗分析中潛在之干擾 13 2.2.5 自動化吹氣捕捉技術之發展與應用 14 2.3偵測極限定義 16 第三章 研究方法 27 3.1 自動化即時連續監測吹氣捕捉/氣相層析系統說明 28 3.1.1 PSM自動進樣系統 29 3.1.2 分析儀器與設備 30 3.1.3 進樣管路與清洗系統 31 3.2 配置儲備標準溶液 32 3.3 捕集管的製備 34 3.4 品保品管項目(QA/QC) 35 3.5 自動化連續監測P&T/GC/FID系統參數探討與測試 37 3.6 真實樣品採樣規劃 42 3.7 污水處理廠現場自動化連續監測規劃 43 第四章 結果與討論 55 4.1 現場自動化即時連續監測吹氣捕捉/氣相層析系統 55 4.1.1 PSM連續式自動進樣管路測試 55 4.1.1.1 PSM自動進樣裝置訊號評估測試 55 4.1.1.2 PSM進樣管路過濾裝置測試 56 4.1.1.3 進樣前管路沖洗(rinse)時間測試 56 4.1.1.4 清洗系統建立 57 4.1.2 吹氣捕捉/氣相層析/火焰游離偵檢器系統結果與討論 58 4.1.2.1 OV-624升溫條件測試 59 4.1.2.2 吹氣捕捉/氣相層析系統最佳化參數結果與討論 59 4.1.3 自動化即時連續監測吹氣捕捉/氣相層析系統之品保與品管項 目 64 4.2 真實樣品分析 66 4.2.1 現場自動化及時連續監測吹氣捕捉/氣相層析系統整體系統評 估 66 4.2.2 現場自動化即時連續監測吹氣捕捉/氣相層析系統現場實測結 果與討論 66 第五章 結論 121 參考文獻 xiv 附錄 xviii

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