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研究生:翁慈伶
研究生(外文):Tzu-Ling Wong
論文名稱:環境空氣樣品中多環芳香烴及其衍生物之分析方法開發
論文名稱(外文):Determination of Polycyclic Aromatic Hydrocarbons and Their Derivatives in Ambient Air Sample
指導教授:徐永源徐永源引用關係俞仁渭
指導教授(外文):Youn-Yoen ShuJen-Wei Yu
學位類別:碩士
校院名稱:國立高雄師範大學
系所名稱:化學系
學門:自然科學學門
學類:化學學類
論文種類:學術論文
論文出版年:2009
畢業學年度:97
語文別:中文
論文頁數:111
中文關鍵詞:多環芳香烴化合物硝基多環芳香烴化合物周界空氣樣品
外文關鍵詞:Polycyclic Aromatic HydrocarbonsNitrated-Polycyclic Aromatic HydrocarbonsAmbient air sampleGC-MSGC-NICI-MS
相關次數:
  • 被引用被引用:1
  • 點閱點閱:310
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  • 下載下載:0
  • 收藏至我的研究室書目清單書目收藏:0
多環芳香烴碳氫化合物(PAHs)及其衍生物硝基多環芳香烴碳氫化合物(NPAHs)廣泛地存在於大氣環境當中,研究顯示PAHs和NPAHs為具有致突變性與致畸性之汙染物,並且這類物質容易累積於環境之中,因此對人類及生態環境有相當的危害性。
本研究著重於發展一分析方法能同時檢測環境空氣樣品中的12種NPAHs和19種PAHs。首先將樣品以二氯甲烷進行索式萃取16~20小時,再將萃取液經由固相萃取法(SPE)淨化分離得到PAHs與NPAHs兩部分沖提液。含NPAHs分析物之沖提液再以液相層析管柱(HPLC)進一步地淨化分離並收集其流析液。淨化後之PAHs與NPAHs萃取液皆以吹氮的方式濃縮至適當體積,並添加內標準品以GC/MS檢測。本研究中視分析物之靈敏度不同,NPAHs待測物使用GC/NICI-MS進行偵測;PAHs待測物則使用GC/EI-MS進行偵測。此分析程序之PAHs方法偵測極限(MDL)為1.56–11.97 pg/μL;NPAHs方法偵測極限為0.46–38.15 pg/μL。
此方法亦使用標準參考樣品(SRM1975,柴油引擎排放粒狀物萃取液)進行方法驗證,其結果顯示,回收率介於44%~129%之間,經由此方法之前處理程序以及搭配氣相層析質譜儀能夠成功地降低樣品基質對分析物之干擾,可做為於環境空氣樣品之檢測參考。
In the last decade, PAHs and nitro-PAHs are of special concern due to their toxicity (carcinogenicity, mutagenicity, estrogen disturbance) to human beings.
This study develops an analytical method for the quantification of 12 NPAHs and 19 PAHs in environmental samples. The procedure of the method is to extract samples by Soxhlet apparatus for a period of 16 to 20 hours with dichloromethane. The extract is cleaned up by solid phase extraction (SPE) technique and then is separated into two fractions each containing PAHs and NPAHs fraction, respectively. The NPAHs fraction is further separated and cleaned up by high performance liquid chromatography (HPLC) for group separation and cleanup. Qualitative/quantitative analysis for NPAHs and PAHs are performed with gas chromatography–mass spectrometry with negative ion chemical ionization (GC/NICI-MS) and using gas chromatography–mass spectrometry with electron impact ionization (GC/EI-MS) for the determination of PAHs fraction.
The method detection limits (MDL) for PAHs and NPAHs are in the range of 1.56–11.97 pg/μL and 0.46–38.15 pg/μL, respectively. The recovery rates were 44%~129%. This analytical method was also applied on standard reference material (SRM1975, Diesel particulate extract). The results show that using this method can decrease matrix interferences successfully and that it’s suitable for analyzing ambient air samples.
中文摘要 Ⅰ
英文摘要 II
目錄 III
表次 VI
圖次 VII

壹、緒論 1
1.1 引言 1
1.2 多環芳香烴碳氫化合物 (PAHs) 1
1.3 硝基多環芳香烴碳氫化合物(NPAHs) 5
1.4 PAHs與Nitro-PAHs對人類的影響 8
1.5 PAHs與Nitro-PAHs的檢測方法 10
1.6 固相萃取法 13
1.7 質譜原理 14
1.7.1 電子撞擊游離法 15
1.7.2 負離子化學游離法 16
1.7.3 四極柱質量分析器原理 16

貮、研究方法 21
2.1 分析流程 21
2.2 藥品、實驗器材和儀器設備 22
2.2.1 試劑與溶劑 ..22
2.2.2 標準品 22
2.2.3 內標準品 23
2.2.4 擬似標準品 24
2.2.5 標準參考樣品 24
2.2.6 藥品配製 24
2.2.7 實驗儀器設備與器材 25
2.2.8 試劑與器材之準備 27
2.3 分析步驟 28
2.3.1索式萃取 28
2.3.2 減壓濃縮與置換溶劑 29
2.3.3固相萃取分離淨化程序 29
2.3.4液相層析分離淨化程序 29
2.4 分析儀器 31
2.4.1 GC/EI-MS 檢測方法 31
2.4.2 GC/NICI-MS 檢測方法 33
2.5 前處理步驟與回收率試驗 35
2.5.1 固相萃取條件之探討 35
2.5.2 液相層析條件之探討 35
2.6 真實樣品-標準參考物質SRM1975分析 35
2.6.1重複分析試驗 36
2.6.2標準添加回收率試驗 36
2.7 數據處理 36
2.7.1 定量方法 36
2.7.2標準參考物質回收率 38
2.7.3重複分析 39
2.7.4標準添加回收率 39
2.8方法偵測極限 39

參、結果與討論 42
3.1 PAHs氣相層析質譜儀之檢測結果 42
3.1.1 多環芳香烴碳氫化合物氣相層析分析結果 42
3.1.2 多環芳香烴碳氫化合物檢量線與偵測極限 45
3.2 Nitro-PAHs氣相層析質譜儀之檢測結果 51
3.2.1 硝基多環芳香烴碳氫化合物氣相層析分析結果 51
3.2.2 硝基多環芳香烴碳氫化合物檢量線與偵測極限 53
3.3 固相萃取管柱分離淨化條件 57
3.3.1 沖提溶劑比例對萃取效果影響 57
3.3.1.1沖提溶劑比例對Nitro-PAHs萃取效果影響 57
3.3.1.2沖提溶劑比例對PAHs萃取效果影響 59
3.3.2 沖提溶劑體積對萃取效果影響 63
3.3.2.1沖提溶劑體積對Nitro-PAHs萃取效果影響 63
3.3.2.2沖提溶劑體積對PAHs萃取效果影響 63
3.3.3 固相萃取步驟回收率 65
3.4 高效能液相層析法(HPLC)淨化分離條件 68
3.4.1 高效能液相層析結果 68
3.4.2 高效能液相層析步驟回收率 68
3.5 真實樣品-標準參考物質SRM1975分析結果 71
3.5.1 重複分析試驗 71
3.5.2 標準添加試驗 71
3.6 方法偵測極限 85
肆、結論 91
伍、參考文獻 92
附錄 101

表 次

表1-1、16種USEPA列管之多環芳香烴碳氫化合物的基本物化性質 3
表1-2、加拿大全國空氣污染監測網NAPS監測之31種PAHs. 4
表1-3、加拿大全國空氣污染監測網NAPS監測之24種NPAHs. 6
表1-4、12種硝基多環芳香烴化合物的物理性質 7
表1-5、NPAHs與Benzo[a]Pyrene之致突變性之比較 9
表1-6、硝基多環芳香烴碳氫化合物之分析方法 12
表1-7、本實驗所分析的PAHs與NPAHs化合物及其氘化物 18
表2-1、PAHs於質譜圖中之對應離子 32
表2-2、NPAHs於質譜圖中之對應離子 34
表3-1、19種PAHs、擬似標準品與內標準品之縮寫與滯留時間 32
表3-2、 PAHs標準品於GC/ MS檢量範圍、線性相關係數及儀器偵測極限 45
表3-3、12種NPAHs、擬似標準品與內標準品之縮寫與滯留時間 51
表3-4、NPAHs標準品於GC/NCI-MS檢量範圍、線性相關係數及儀器偵測極限 53
表3-5、固相萃取PAHs以各種不同沖提溶劑比例沖提下之累計回收率列表 62
表3-6、NPAHs固相萃取沖提體積回收率測試 64
表3-7、不同沖提條件對PAHs與NPAHs固相萃取效果影響 66
表3-8、19種PAHs與12種NPAHs於固相萃取步驟之回收率列表 67
表3-9、 NPAHs 於液相層析管柱中滯留時間 69
表3-10、NPAHs及其surrogates 於HPLC步驟回收率試測結果 70
表3-11、標準參考樣品SRM 1975 重覆分析與回收率試測結果(PAHs部分) 81
表3-11、(續)標準參考樣品SRM 1975 重覆分析與回收率試測結果
(NPAHs部分) 82
表3-12、標準參考樣品SRM1975添加分析結果(NPAHs部分) 83
表3-12、(續) 標準參考樣品SRM 1975 添加分析結果(PAHs部分) 84
表3-13、方法偵測極限(PAHs第一次添加) 86
表3-14、方法偵測極限(PAHs第二次添加) 87
表3-15、方法偵測極限(PAHs第一、二次添加測試)之擬似標準品回收率列表 88
表3-16、方法偵測極限(NPAHs第一次添加) 89
表3-17、方法偵測極限(NPAHs第二次添加) 90

圖 次

圖1-1、NPAHs代謝及轉化機制 9
圖1-2、A. 只經由SPE淨化程序之SRM1649a萃取液分析結果層析圖B. 經由SPE續以HPLC淨化前處理之SRM1649a萃取液分析結果層析圖 11
圖1-3、固相萃取法程序圖 14
圖1-4、電子撞擊游離法裝置圖 15
圖1-5、四極柱質量分析器裝置示意圖 17
圖1-6、19種PAHs分子結構 19
圖1-7、12種NPAHs分子結構 20
圖2-1、分析方法流程圖 21
圖3-1、PAHs 標準品與內標準品GC/EI-MS層析圖譜 44
圖3-2、 19種PAHs標準品之檢量線 46
圖3-3、 12種NPAHs 標準品與內標準品GC/NCI-MS層析圖譜 52
圖3-4、 12種Nitro-PAHs標準品之檢量線 54
圖3-5、 Nitro-PAH固相萃取沖提溶劑比例對萃取效果影響 58
圖3-6、 PAHs固相萃取沖提溶劑比例對萃取效果影響(A) 60
圖3-7、 PAHs固相萃取沖提溶劑比例對萃取效果影響(B) 61
圖3-8、 PAHs固相萃取沖提溶劑體積對萃取效果影響 64
圖3-9、 12種 Nitro-PAHs標準品液相層析圖 69
圖3-10、SRM1975樣品分析所得之離子質譜層析圖(NPAHs部分) 72
圖3-10、(續) SRM1975樣品分析所得之離子質譜層析圖(NPAHs部分) 73
圖3-11、SRM1975樣品分析所得之離子質譜層析圖(PAHs部分) ... 74
圖3-11、(續) SRM1975樣品分析所得之離子質譜層析圖(PAHs部分) 75
圖3-12、SRM1975標準添加樣品分析所得之離子質譜層析圖(NPAHs部分) 76
圖3-12、(續) SRM1975標準添加樣品分析所得之離子質譜層析圖(NPAHs部分) 77
圖3-13、SRM1975標準添加樣品分析所得之離子質譜層析圖(PAHs部分) 78
圖3-13、(續) SRM1975標準添加樣品分析所得之離子質譜層析圖(PAHs部分) 79
圖3-13、(續) SRM1975標準添加樣品分析所得之離子質譜層析圖(PAHs部分) 80
圖4-1、naphthalene於EI-MS所得之質譜圖 101
圖4-2、2-methylnaphthalene於EI-MS所得之質譜圖 101
圖4-3、acenaphthylene於EI-MS所得之質譜圖 101
圖4-4、acenaphthene於EI-MS所得之質譜圖 102
圖4-5、flourene於EI-MS所得之質譜圖 102
圖4-6、phenanthrene於EI-MS所得之質譜圖 102
圖4-7、anthracene於EI-MS所得之質譜圖 103
圖4-8、flouranthene於EI-MS所得之質譜圖 103
圖4-9、pyrene於EI-MS所得之質譜圖 103
圖4-10、benz(a)anthracene於EI-MS所得之質譜圖 104
圖4-11、chrysene於EI-MS所得之質譜圖 104
圖4-12、benzo(b)fluoranthene於EI-MS所得之質譜圖 104
圖4-13、benzo(k)fluoranthene於EI-MS所得之質譜圖 105
圖4-14、benzo(e)pyrene於EI-MS所得之質譜圖 105
圖4-15、benzo(a)pyrene於EI-MS所得之質譜圖 105
圖4-16、perylene於EI-MS所得之質譜圖 106
圖4-17、dibenz(a,h)anthracene於EI-MS所得之質譜圖 106
圖4-18、indeno(1,2,3-cd)pyrene於EI-MS所得之質譜圖 106
圖4-19、benzo(g,h,i)perylene於EI-MS所得之質譜圖 107
圖5-1、2-Nitrofluorene於NCI-MS所得之質譜圖 108
圖5-2、9-Nitroanthracene於NCI-MS所得之質譜圖 108
圖5-3、9-Nitrophenanthrene於NCI-MS所得之質譜圖 108
圖5-4、2-Nitrofluoranthene於NCI-MS所得之質譜圖 109
圖5-5、3-Nitrofluoranthene於NCI-MS所得之質譜圖 109
圖5-6、1-Nitropyrene於NCI-MS所得之質譜圖 109
圖5-7、7-Nitrobenz[a]anthracene於NCI-MS所得之質譜圖 110
圖5-8、6-Nitrochrysene於NCI-MS所得之質譜圖 110
圖5-9、1,3-Dinitropyrene於NCI-MS所得之質譜圖 110
圖5-10、1,6-Dinitropyrene於NCI-MS所得之質譜圖 111
圖5-11、1,8-Dinitropyrene於NCI-MS所得之質譜圖 111
圖5-12、6-Nitrobenzo[a]pyrene於NCI-MS所得之質譜圖 111
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