| 研究生: |
陳駿 Chen, Chun |
|---|---|
| 論文名稱: |
環境水體中多氯戴奧辛及呋喃之高解析氣相層析儀/高解析質譜儀分析方法建立 Establishment of a HRGC/HRMS Method for the Analysis of Polychlorinated Dibenzo-p-Dioxins and Dibenzofurans in Environmental Water |
| 指導教授: |
黃福永
Huang, Fu-Yung 廖寶琦 Liao, Pao-Chi |
| 學位類別: |
碩士 Master |
| 系所名稱: |
理學院 - 化學系碩士在職專班 Department of Chemistry (on the job class) |
| 論文出版年: | 2008 |
| 畢業學年度: | 96 |
| 語文別: | 中文 |
| 論文頁數: | 124 |
| 中文關鍵詞: | 環境水體 、泡棉 、二聯苯呋喃 、多氯二聯苯戴奧辛 、偵測下限 |
| 外文關鍵詞: | PUF, detection limit, environmental water, PCDFs, PCDDs |
| 相關次數: | 點閱:142 下載:7 |
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由於戴奧辛是屬於疏水性化合物,其在環境水體中之濃度範圍僅介於10-12~10-15 g/L,導致分析環境水體中的多氯二聯苯戴奧辛及二聯苯呋喃極具挑戰性。本研究參考環檢所公告方法-NIEA M801.11B,利用固液萃取原理,將水體經用玻璃纖維濾紙過濾後,以每分鐘0.8~0.9 公升的流速將水體中戴奧辛吸附於泡棉(PUF)上,再經過索氏萃取、濃縮、淨化等程序,最後以高解析氣相層析儀及高解析質譜儀來分析水中超微量戴奧辛。本研究目的如下:(1)藉由添加已知濃度標準品方式來討論不同實驗階段標準品回收情形;(2)藉由樣本重複分析的再現性來探討本分析方法的精確度;(3)透過文獻比較方式來探討本分析方法的靈敏度、空白背景值、二重複分析精確度之優劣。測試結果在自來水的四重複分析實驗所得到的十七種多氯二聯苯戴奧辛及二聯苯呋喃精確度範圍為1~4%,其準確度在90%以上。而二次蒸餾水水中標準品添加回收率只在50~81%,經實驗證實是因為標準品無法有效溶解於水中而吸附於玻璃容器上,本研究參考文獻中的方法,將採樣管管件更改為不鏽鋼及高密度矽膠材質,同時以不透過容器而直接將水中多氯二聯苯戴奧辛及二聯苯呋喃濃縮於泡棉上,提升了10~21%的水中標準品添加回收率。在測試方法靈敏度的部份,經40公升採樣體積提升到600公升的結果,證實可有效提升方法靈敏度,如取600公升水體的分析得到的方法偵測下限為0.0001~0.0003pg/L,比美國環保署使用的吸附材質XAD-2低5~10倍,因為泡棉優勢在於通透性佳,所以可以用比XAD-2快1倍的速率濃縮大體積水體,同時泡棉有很低的空白背景值,分析低濃度水體較無干擾問題。本研究測得的自來水體十七種多氯二聯苯戴奧辛及二聯苯呋喃總毒性當量平均濃度為0.013pg /L(WHO-TEQ)(n=8),此結果相當接近環檢所發表的自來水體中十七種多氯二聯苯戴奧辛及二聯苯呋喃總毒性當量平均濃度0.012pg /L(WHO-TEQ),如將此結果依據美國環保署訂定可接受的上限潛在致癌因子(upper-limit carcinogenic potency factor for human)來估算國人飲用自來水體的致癌機率,求得其機率僅約為10-6。同時此濃度也遠低於政府將設立飲用水中氯二聯苯戴奧辛及二聯苯呋喃總毒性當量管制標準值12 pg /L(WHO-TEQ)有千倍之多。
Due to that the hydrophobic property, the concentration of PCDD/Fs solubility in environmental water is around 10-12~10-15 pg/L, which makes the analysis a tough challenge. In this study, we had developed a set up and method based on the principle of solid-liquid extraction setting by EPA(Environmental Protection Agency)-NIEA M801.11B for the analysis of water. The water was first filtered through a glass fiber membrane, followed by pumping through a column packed with PUF at a rate of 0.8~0.9L/min to absorb the PCDD/Fs. The PCDD/Fs absorbed on PUF were extracted by using Soxhlet extractor followed by concentration and purification, then subjected to HRGC/HRMS analysis.This study was aiming at: i) Assess the recovery yield by adding standard solution at various check points; ii) Assess the experimental precision by repeating the analysis; iii) Compare the results with the reported data to evaluate the feasibility and reliability of this set up and method.The results of this study were showed as below. The precision of four times analysis repetition was within 1~4% and the accuracy was over 90%. The recovery yield of the adding standard sample was low, attributing to the low solubility of sample in double distilled water as to be absorbed on the surface of glass container. To solve this problem the water specimen was collected directed and using PUF to absorb the Dioxin in the scene without using glass container and the pipes of the set up were replaced with stainless steel or high density silica gel material made pipes. This improved 10~20% increase in recovery yield. We also found that with the increase of sample volume, >600L , the sensitivity increased and the detection limit was 0.0001~0.0003pg/L, which was five to ten times lower than that reported by USEPA using XAD-2 as the adsorbent. Using PUF as the adsorbent, the sampling time was only half of that by using XAD-2 and there was low blank concentration when repeating use, indicating this method can be applied to analyze water with low concentration(ppt~ppq).The average concentration of PCDD/Fs detected with this method for water collected from different area in Taiwan was 0.013 pg /L (WHO-TEQ), which was similar to the value reported by EPA 0.012 pg /L(WHO-TEQ). This result also showed that the probability to cause cancer by drinking the tap water in Taiwan is about one of 106 based on the upper-limit carcinogenic potency factor for human setting by USEPA and this concentration is also much lower than the limit concentration of PCDD/Fs in drinking 12pg/L(WHO-TEQ)that will be published by Taiwan Government.
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