本研究旨在調查典寶溪底泥中6種鄰苯二甲酸酯類、18種抗生素藥物類及10種非抗生素藥物類之殘留濃度，並嘗試利用奈米級施威特曼石 (nano-SHM) 催化過氧化氫氧化程序結合電動力法整治鄰苯二甲酸酯類及藥物類污染底泥，期盼未來建立一本土化可行的現地整治技術，以作為後續實場應用。於典寶溪底泥中鄰苯二甲酸酯類及藥物類之殘留濃度調查工作方面，已針對選定之5個採樣點位進行7梯次採集底泥樣品，綜合調查結果發現，於底泥中可檢出6種鄰苯二甲酸酯類、4種抗生素藥物類及4種非抗生素藥物類之化合物，於角宿支流角宿橋處檢出mg/kg (ppm) 濃度等級之鄰苯二甲酸二 (2-乙基己基) 酯 (DEHP) 殘留量，其最高濃度 (5,939 µg/kg) 約為「底泥品質指標之分類管理及用途限制辦法」下限值的3倍。於新穎組合式整治技術試驗方面，利用實驗室規模之新穎組合式整治技術─利用電動力法輔助nano-SHM/H2O2氧化去除鄰苯二甲酸酯類及藥物類污染底泥，於陽極槽液及底泥反應器注入孔添加nano-SHM/H2O2氧化劑，並施加定電壓 (1.5 V/cm) 進行為期 14日及28日期程之6組電動力試驗。試驗結果顯示：(1) nano-SHM藉由電泳移向陰極端，而H2O2則藉由電滲透流移向陰極端，同時藉由反應產生OH‧強氧化劑，可將底泥中鄰苯二甲酸酯類及藥物類予以降解，去除率分別為70-99%及100%；(2) 由於電極極性轉換之緣由，經過28日反應時間後，底泥酸鹼梯度現象並不顯著；(3) 利用電動力法輔助nano-SHM/H2O2氧化去除鄰苯二甲酸酯類及藥物類污染底泥試驗，可將標的污染物主要礦化成CO2及H2O且無二次污染之虞。本工法除具有上述之技術可行性外，其粗估整治費用 (6,639元/噸) 相較其他實驗室規模整治技術較為低廉，亦具經濟可行性。雖然現階段仍屬於實驗室規模之試驗，但未來若能應用於現地整治，不僅具有現階段試驗之優勢外，尚可節省龐大之開挖工程費用，實具有相當大的應用潛勢。

The objectives of this study are two-fold: (1) to investigate the residual concentrations of six phthalate esters (PAEs) and 28 pharmaceuticals in sediment samples collected from the Dianbao River; and (2) to develop and establish a localized, feasible in situ remediation technology coupling nano- schwertmannite (nano-SHM)/H2O2 process and electrokinetic process for the removal of PAEs and pharmaceuticals in sediments of the Dianbao River. To meet the first objective, seven batches of sediment sampling were conducted at five sampling sites along the Dianbao River. After analysis of sediment samples, six PAEs and eight pharmaceuticals were detected. The order of parts per million (ppm) of residual di(2-ethylhexyl) phthalate (DEHP) was detected at the sampling site under the Jiaosu Bridge. The highest concentration of DEHP (5,939 µg/kg) is about 3 times greater than the “Regulations for Systematic Management of Quality Indices of Sediments and Their Use Restrictions” promulgated by Taiwan EPA. To meet the second objective, six tests with a remediation time of 14 days or 28 days were carried out using the electrokinetic-assisted nano-SHM/H2O2 process under an electric field of 1.5 V/cm. Test results for the removal of PAEs and pharmaceuticals in the sediment samples collected at the sampling site under the Shengxing Bridge of the Dianbao River are given as follows: (1) injection of nano-SHM and H2O2 into the anode reservoir and the sediment compartment would yield OH• that would be transported by the electrophoresis and electroosmotic flow from the anode end toward the cathode to degrade PAEs and pharmaceuticals if any; (2) as a result of the electrode polarity reversal, the pH gradient of sediment is not significant after 28 days; and (3) 70-100% of the PAEs and pharmaceuticals would be removed, and no secondary pollution would be generated in the sediment compartment. Accordingly, the novel remediation process employed in this study could be considered as a viable remediation technology for the removal of PAEs and pharmaceuticals from sediments. An operating cost analysis has also showed the economic feasibility of the present remediation technology. In summary, the coupling of nano-SHM/H2O2 process and electrokinetic process would be a very competitive process for the treatment of PAEs and pharmaceuticals-contaminated sediment in terms of remediation time and cost.

論文審定書 i
聲明切結書 ii
誌謝 iii
摘要 iv
Abstract vi
目錄 viii
圖目錄 xii
表目錄 xviii
第一章 緒論 1
1.1 研究緣起 1
1.2 研究目的 5
1.3 研究項目 5
第二章 文獻回顧 9
2.1 底泥中鄰苯二甲酸酯類及藥物類之流布調查 9
2.1.1 鄰苯二甲酸酯類 9
2.1.2 藥物類 12
2.2 底泥中鄰苯二甲酸酯類及藥物類之整治技術 14
2.2.1 Fenton法 16
2.2.2 類Fenton法 18
2.2.3 新穎的類Fenton法 19
2.2.4 電動力法 21
第三章 材料與方法 29
3.1 化學藥品 29
3.1.1 鄰苯二甲酸酯類之標準品 29
3.1.2 鄰苯二甲酸酯類之內標準品 34
3.1.3 抗生素藥物類之標準品 34
3.1.4 非抗生素藥物類之標準品 34
3.1.5 其他相關藥品 35
3.2 典寶溪底泥調查 35
3.2.1 樣品採集 35
3.2.2 樣品前處理 36
3.2.3 樣品分析 38
3.3 新穎組合式整治技術 52
3.3.1 整治試驗用河川底泥來源及其基本性質 52
3.3.2 奈米級施威特曼石及其懸浮液製備 54
3.3.3 整治試驗用河川底泥與nano-SHM/H2O2反應之瓶杯試驗 56
3.3.4 新穎整治系統建置及其試驗方法 58
3.4 鄰苯二甲酸酯類及藥物類污染去除反應機制探討 64
3.5 組合式整治技術評估 65
第四章 結果與討論 66
4.1 典寶溪底泥調查 66
4.1.1 空間分布調查 66
4.1.2 時間分布調查 68
4.1.3 鄰苯二甲酸酯類及藥物類殘留濃度與其他地區底泥之比較 71
4.1.4 水體環境影響評估 74
4.2 新穎組合式整治技術 77
4.2.1奈米級施威特曼石合成 77
4.2.2 奈米級施威特曼石懸浮液製備 81
4.2.3 整治試驗底泥之nano-SHM/H2O2瓶杯試驗 83
4.2.4 電動力法輔助nano-SHM/H2O2之組合式整治試驗 89
4.2.5 鄰苯二甲酸酯類及藥物類污染去除反應機制探討 124
4.3 標的污染物殘留質量分率及中間產物之評估 131
4.3.1標的污染物殘留質量分率 131
4.3.2 標的污染物降解反應中間產物 136
4.4 操作成本粗估 138
4.5 未來工程應用構想 142
第五章 結論與建議 146
5.1 結論 146
5.2 建議 148
參考文獻 150
附錄 就學期間發表之學術論文 176
圖1-1 研究架構流程圖 6
圖2-1 電動力整治技術原理示意圖 23
圖3-1 河川底泥樣品前處理程序之流程圖 30
圖3-2 典寶溪底泥採樣位置圖 37
圖3-3 實驗室規模新穎組合式整治系統示意圖 59
圖4-1 鄰苯二甲酸酯類殘留濃度與其他地區底泥之比較 72
圖4-2 藥物類殘留濃度與其他國家河川底泥之比較 73
圖4-3 化學合成奈米級施威特曼石之ESEM影像圖 77
圖4-4 化學合成奈米級施威特曼石之TEM影像圖 78
圖4-5 化學合成奈米級施威特曼石之XRD分析圖譜 79
圖4-6 化學合成奈米級施威特曼石之ESEM-EDS圖譜 79
圖4-7 化學合成奈米級施威特曼石在不同pH值水溶液中之界達電位檢測值 80
圖4-8 Nano-SHM/H2O2 瓶杯試驗組別–反應後底泥中標的污染物之殘留濃度：(a) 鄰苯二甲酸酯類；及 (b) 藥物類 84
圖4-9 化學合成奈米級施威特曼石及其重複使用12次之XRD分析圖譜 85
圖4-10 試驗用河川底泥與nano-SHM/H2O2反應之瓶杯試驗，其不同反應時間之底泥ESEM影像圖 (50X)：(a) 0日；(b) 0.5日；(c) 1日；(d) 2日；(e) 3日；(f) 4日；及 (g) 5日 87
圖4-11 試驗用河川底泥與nano-SHM/H2O2反應之瓶杯試驗，其不同反應時間之底泥ESEM影像圖 (5000X)：(a) 0日；(b) 0.5日；(c) 1日；(d) 2日；(e) 3日；(f) 4日；
及 (g) 5日 88
圖4-12 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第1組試驗組別 (空白試驗)—陰、陽極槽液pH值之變化 90
圖4-13 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第1組試驗組別 (空白試驗)—累積電滲透流流量之變化 91
圖4-14 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第1組試驗組別 (空白試驗)—反應後底泥pH值之分布 92
圖4-15 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第1組試驗組別 (空白試驗)—反應後底泥中標的污染物之殘留濃度：(a) 鄰苯二甲酸酯類；及 (b) 藥物類之殘留濃度 93
圖4-16 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第2組試驗組別—陰、陽極槽液pH值之變化 95
圖4-17 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第2組試驗組別—累積電滲透流流量之變化 96
圖4-18 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第2組試驗組別—反應後底泥pH值之分布 97
圖4-19 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第2組試驗組別—反應後底泥中標的污染物之殘留濃度：(a) 鄰苯二甲酸酯類；及 (b) 藥物類之殘留濃度 98
圖4-20 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第3組試驗組別—陰、陽極槽液pH值之變化 100
圖4-21 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第3組試驗組別—累積電滲透流流量之變化 101
圖4-22 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第3組試驗組別—反應後底泥pH值之分布 102
圖4-23 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第3組試驗組別—反應後底泥中標的污染物之殘留濃度：(a) 鄰苯二甲酸酯類；及 (b) 藥物類之殘留濃度 103
圖4-24 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第4組試驗組別—陰、陽極槽液pH值之變化 105
圖4-25 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第4組試驗組別—累積電滲透流流量之變化 106
圖4-26 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第4組試驗組別—反應後底泥pH值之分布 107
圖4-27 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第4組試驗組別—反應後底泥中標的污染物之殘留濃度：(a) 鄰苯二甲酸酯類；及 (b) 藥物類之殘留濃度 108
圖4-28 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第5組試驗組別—陰、陽極槽液pH值之變化 110
圖4-29 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第5組試驗組別—累積電滲透流流量之變化 111
圖4-30 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第5組試驗組別—反應後底泥pH值之分布 112
圖4-31 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第5組試驗組別—反應後底泥中標的污染物之殘留濃度：(a) 鄰苯二甲酸酯類；及 (b) 藥物類之殘留濃度 113
圖4-32 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第6組試驗組別—陰、陽極槽液pH值之變化 115
圖4-33 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第6組試驗組別—累積電滲透流流量之變化 116
圖4-34 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第6組試驗組別—反應後底泥pH值之分布 117
圖4-35 電動力整治鄰苯二甲酸酯類及藥物類污染典寶溪底泥第6組試驗組別—反應後底泥中標的污染物之殘留濃度：(a) 鄰苯二甲酸酯類；及 (b) 藥物類之殘留濃度 118
圖4-36 河川底泥與nano-SHM/H2O2反應在不同反應系統及反應時間/條件下之ESEM影像圖 (50X)：[I] 瓶杯試驗：(a) 0日；及 (b) 3日；與 [II] 電動力試驗組別：
(c) 第1組；(d) 第2組；(e) 第3組；(f) 第4組；(g) 第5組；及 (h) 第6組 122
圖4-37 河川底泥與nano-SHM/H2O2反應在不同反應系統及反應時間/條件下之ESEM影像圖 (5000X)：[I] 瓶杯試驗：(a) 0日；及 (b) 3日；與 [II] 電動力試驗組別：(c) 第1組；(d) 第2組；(e) 第3組；(f) 第4組；(g) 第5組；及 (h) 第6組 123
圖4-38 Nano-SHM及H2O2在本研究電動力整治系統之傳輸現象示意圖 125
圖4-39 Nano-SHM於不同pH環境之變化：(a) 化學反應；及 (b) 顆粒表面電荷性 126
圖4-40 Nano-SHM/H2O2氧化鄰苯二甲酸酯類及藥物類化合物之反應機制示意圖 129
圖4-41 電動力輔助nano-SHM/H2O2氧化程序現地整治遭受鄰苯二甲酸酯類及藥物類污染底泥之技術原理示意圖 130
圖4-42 電動力整治鄰苯二甲酸酯類及藥物類污染底泥在負模式掃描下之離子層析質譜圖 (m/z 50-1000)：(a) 整治前；及 (b) 整治後 (第6組試驗組別) 137
圖4-43 組合式整治技術工程應用示意圖：(a) 第1階段俯視圖；(b) 第2階段俯視圖；及 (c) 第1階段剖面圖 143
表3-1 鄰苯二甲酸酯類及藥物類化合物資本資料 31
表3-2 河川底泥中鄰苯二甲酸酯類及藥物類經前處理程序之回收率測試 39
表3-3 鄰苯二甲酸酯類及藥物類於超高效液相層析儀之分析條件 41
表3-4 鄰苯二甲酸酯類及藥物類於三重串聯四極桿質譜儀MRM模式之分析條件 42
表3-5 鄰苯二甲酸酯類及藥物類之LC–ESI-MS/MS定性及定量偵測極限 48
表3-6 典寶溪底泥基本性質分析結果 53
表3-7 過氧化氫於整治試驗底泥中反應1日後之殘留濃度 57
表3-8 利用電動力法輔助nano-SHM/H2O2試驗之參數及條件一覽表 61
表4-1 典寶溪底泥中鄰苯二甲酸酯類及藥物類殘留濃度之調查結果 67
表4-2 典寶溪底泥中鄰苯二甲酸酯類及藥物類殘留濃度於豐水期及枯水期之比較 69
表4-3 可見光 (900 nm) 分光光度計量測nano-SHM懸浮液之結果 82
表4-4 電動力試驗組別之鄰苯二甲酸酯類化合物殘留質量分率分析結果一覽表 132
表4-5 電動力試驗組別之藥物類化合物殘留質量分率分析結果一覽表 134
表4-6 電動力試驗之操作費用估算 (分析級及試藥級藥劑) 一覽表 139
表4-7 電動力試驗之操作費用估算 (工業級藥劑) 一覽表 140
表4-8 有機物污染土壤及底泥整治費用之比較 141

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