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研究生:洪晟瀚
研究生(外文):Cheng-Han Hung
論文名稱:吹氣輔助頂空固相微萃取結合氣相層析質譜術於水中硝基多環芳香烴之研究
論文名稱(外文):Purge Assisted Headspace Solid Phase Microextraction Combined with Gas Chromatography/Mass Spectrometry for Determination of Nitrated Polycyclic Aromatic Hydrocarbons in Aqueous Solution
指導教授:李茂榮李茂榮引用關係
指導教授(外文):Maw-Rong Lee
學位類別:碩士
校院名稱:國立中興大學
系所名稱:化學系所
學門:自然科學學門
學類:化學學類
論文種類:學術論文
畢業學年度:96
語文別:中文
論文頁數:127
中文關鍵詞:吹氣輔助頂空固相微萃取氣相層析質譜術硝基多環芳香烴環境分析
外文關鍵詞:Purge Assisted Headspace Solid Phase MicroextractionGas Chromatography/Mass SpectrometryNitrated Polycyclic Aromatic HydrocarbonsEnvironmental analysis
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  • 被引用被引用:4
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本實驗是以實驗室自行開發的吹氣輔助頂空固相微萃取技術結合氣相層析質譜術,以負離子化學游離化法選擇離子偵測模式,進行水中微量硝基多環芳香烴化合物之研究,並探討不同離子化方式、纖維塗覆物質、萃取時間、萃取溫度、水溶液酸鹼值、添加鹽類、氮氣流速對於萃取效率之影響,並討論此技術之線性範圍、相關係數、偵測極限與再現性等,更進一步的應用此技術於真實河川樣品之偵測。
實驗結果顯示以吹氣輔助頂空固相微萃取結合氣相層析質譜術,以負離子化學游離化法選擇離子偵測模式,進行水中微量硝基多環芳香烴化合物之研究,於10 mL水樣品中,添加pH值為4.5的緩衝溶液與25 %的NaCl,於氮氣流速30 mL/min下,以100 μm PDMS固相微萃取塗覆纖維於90 °C水浴下,萃取45分鐘,再於氣相層析儀的程序升溫注射口下脫附7.5分鐘,所測得水中硝基多環芳香烴的線性範圍為5 – 5000 pg/mL,其線性相關係數介於0.996至0.999,偵測極限則介於0.01 - 0.11 pg/mL之間。此方法也應用於真實河川樣品之分析。結果顯示以吹氣輔助頂空固相微萃取結合氣相層析質譜儀可大幅提升低揮發性物質之靈敏度與選擇性,可做為水樣品中微量硝基多環芳香烴化合物檢測之參考。
This study was evaluated to determine trace seven nitrated polycyclic aromatic hydrocarbons (NPAHs) in aqueous solution by using purge assisted headspace solid phase microextraction (PA-HS-SPME) combined with gas chromatography/mass spectrometry in negative ion chemical ionization (GC/NICI-MS). The proposed method was based on continuous purging gas through the sample to carry analytes to headspace in which a SPME fiber was used as sorptive device. The parameters affecting the extract efficiency such as SPME fiber, extraction temperature, extraction time, agitation rate, salt effect, pH, hollow fiber length, and nitrogen flow rate were systematically studied. Compared to HS-SPME, PA-HS-SPME provides a significantly improved sensitivity for the extraction of NPAHs, especially for less-volatile NPAHs which could not be detected by HS-SPME. The linear range was 5 - 5000 pg/mL with correlation coefficients above 0.996. Limits of detection (LOD) of seven NPAHs were in the range of 0.01 to 0.10 pg/mL. The application of the methods to the determination of NPAHs in real samples was tested by analyzing aqueous samples from rivers in Taichung city.
謝誌 I
中文摘要 II
英文摘要 III
目錄 IV
表目錄 IX
圖目錄 X

壹、緒論 1
1.1、前言 5
1.2 硝基多環芳香烴類化合物之偵測方法 10
1.3 固相微萃取法 12
1.4 氣相層析法 20
1.5 質譜術原理 23
1.5.1 離子源部分 24
1.5.2 質量分析器 28
貳、實驗部分 35
2.1 藥品、實驗器材與儀器設備 35
2.1.1 藥品 35
2.1.2 實驗器材與儀器設備 36
2.2 藥品配製 37
2.2.1 硝基多環芳香烴化合物標準儲存溶液之配製 37
2.2.2 硝基多環芳香烴化合物標準儲存溶液100 μg/mL之配製
38
2.2.3 硝基多環芳香烴化合物不同濃度混合標準溶液之配製 38
2.2.4 不同濃度內標準溶液之配製 39
2.2.5 不同濃度標準水溶液之配製 39
2.2.6 緩衝溶液之配製 39
2.3 玻璃器具之矽烷化 40
2.4 儀器操作參數 41
2.4.1 氣相層析儀部分 41
2.4.2 質譜儀部分 42
2.5 固相微萃取纖維之活化 42
2.6 氣相層析質譜儀參數之探討 43
2.6.1 電子游離法與負離子化學游離法之比較 43
2.6.2 負離子化學游離法最佳化 43
2.7 吹氣輔助頂空固相微萃取方法之探討 44
2.7.1 吹氣輔助頂空固相微萃取裝置 44
2.7.2 頂空固相微萃取與吹氣輔助頂空固相微萃取方法之比較 44
2.7.3 萃取纖維之比較 44
2.7.4 萃取纖維膜厚之比較 46
2.7.5 萃取溫度最佳化 46
2.7.6 萃取時間最佳化 47
2.7.7 添加氯化鈉於萃取效率之影響 47
2.7.8 水溶液酸鹼值最佳化 47
2.7.9 添加氯化鈉與緩衝溶液於萃取效率之影響 48
2.7.10 中空纖維管長度最佳化 48
2.7.11 氮氣流速最佳化 49
2.7.12 攪拌速率最佳化 49
2.7.13 使用正交設計表探討中空纖維管長度、氮氣流速與攪拌速率 50
2.7.14 恆溫注射口與程序升溫注射口之比較 50
2.7.15 使用正交設計表探討注射口初始溫度、升溫速率與脫附時間 50
2.8 吹氣輔助頂空固相微萃取法分析水中硝基多環芳香烴化合物之線性關係及偵測極限 51
2.9 吹氣輔助頂空固相微萃取法分析水中硝基多環芳香烴化合物之精密度分析 52
2.10 真實河川樣品中硝基多環芳香烴化合物之分析 52
参、結果與討論 53
3.1 硝基多環芳香烴類化合物於氣相層析質譜儀之分析 53
3.1.1 硝基多環芳香烴以電子游離法之分析 54
3.1.2硝基多環芳香烴以負離子化學游離法之分析 54
3.1.3 電子游離法與負離子化學游離法游離化效果之比較 66
3.1.4 負離子化學游離法最佳化 66
3.2 吹氣輔助頂空固相微萃取方法之探討 71
3.2.1 頂空固相微萃取與吹氣輔助頂空固相微萃取方法之比較 71
3.2.2 萃取纖維之比較 73
3.2.3萃取纖維膜厚之比較 77
3.2.4 萃取溫度最佳化 77
3.2.5 萃取時間最佳化 81
3.2.6 添加氯化鈉於萃取效率之影響 83
3.2.7 水溶液酸鹼值最佳化 85
3.2.8 添加氯化鈉與緩衝溶液於萃取效率之影響 87
3.2.9 中空纖維管長度最佳化 87
3.2.10 氮氣流速最佳化 89
3.2.11 攪拌速率最佳化 91
3.2.12 使用正交設計表探討中空纖維管長度、氮氣流速與攪拌速率 93
3.2.13 恆溫注射口與程序升溫注射口之比較 101
3.2.14 使用正交設計表探討注射口初始溫度、升溫速率與脫附時間 103
3.3 吹氣輔助頂空固相微萃取法分析水中硝基多環芳香烴化合物之線性關係及偵測極限 108
3.4 吹氣輔助頂空固相微萃取法分析水中硝基多環芳香烴化合物之精密度分析 108
3.5 真實河川樣品中硝基多環芳香烴化合物之分析 111
肆、結論 115
伍、參考文獻 116
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