摘要

本研究探討自行合成之奈米級零價鐵懸浮液使其形成類-Fenton法，並針對去離子水及含腐植酸的模擬地下水進行As(III)氧化為As(V)之反應進行討論，更進一步藉由奈米級零價鐵懸浮液的注入結合電動力法產生類-Fenton作用氧化土壤中As(III)。
在奈米級零價鐵製備方面，發現利用獨具網狀空間的結構的特性，使其形成空間位阻的概念，在添加3 wt%可溶性澱粉情況下，成功地達到分散效果，後續以XRD、FE-SEM、ESEM-EDS及EDS-Mapping觀察其物種及型態分佈，上述儀器觀察結果發現，本研究所合成之奈米級零價鐵係屬非結晶型態之鐵物種。
在水體試驗中，比較去離子水與含腐植酸之模擬地下水在未增加溶氧且注入奈米級零價鐵懸浮液的情況下As(III)氧化為As(V)之效果，發現在未增加溶氧情況下，模擬地下水的試驗組別中奈米級零價鐵產生之OH•屬非選擇性氧化劑，因此降低了As(V)的產率。而在增加溶氧的情況下，水中溶氧可以幫助氧化模擬地下水中的有機物，使得OH•能進一步氧化As(III)，以致於在增加溶氧的模擬地下水中有較多的As(V)生成率。最後以未增加溶氧時，利用模擬地下水試驗組別之最佳參數條件下，以實際地下水進行試驗，由試驗結果得知As(V)產量約為17.18 μg/L，而在模擬地下水之As(V)產量約為4.63 μg/L。
本研究進一步利用奈米級零價鐵懸浮液注入結合電動力技術進行整治土壤管柱中含低濃度(初始濃度為100 mg/kg)及高濃度(初始濃度為500 mg/kg)之As(III)，在低濃度試驗組別中僅施加電動力法的組別Test E-1，試驗終了後土體As(V)殘餘濃度為24 mg/kg，而在Test E-2(奈米級零價鐵懸浮液注入陽極槽)及Test E-3(奈米級零價鐵懸浮液注入陰極槽)土體As(V)殘餘濃度分別為2.3 mg/kg和3.4 mg/kg。在高濃度試驗組別中Test E-4(僅施加電動力法)、Test E-5(奈米級零價鐵懸浮液注入陽極槽)及Test E-6(奈米級零價鐵懸浮液注入陰極槽)僅在正規化土壤區段(Normalized Distance from Anode Reservoir)為0.2及0.4處符合土壤污染管制標準，在其餘正規化土壤區段為0.6、0.8及1.0處則高出法規標準許多。而在正規化土壤區段為1.0處，Test E-6土壤之As(V)殘餘濃度低於Test E-5，約116.6 mg/kg，原因可能為Test E-6為陰極槽注入奈米級零價鐵在高pH值環境下不發生鐵腐蝕作用進而轉換為吸附作用為主，導致帶負電之As(V)物種只有濃度約183.5 mg/kg隨離子遷移作用至正規化土壤區塊1.0處。

Abstract

The object of this study was to investigate the synthesis of a nanoscale zero-valent iron slurry (NZVIS) for use in Fenton-like reactions, and to evaluate its efficiency for As(III) oxidation to As(V) in spiked deionized water and simulated groundwater containing humic acid. Furthermore, this study used injection of the nanoiron slurry combined with electrokinetic processes to remediate As(III) in soil.
NZVI was prepared by a chemical reduction process. The efficiency of using 3 wt% soluble starch (SS) to stabilize NZVI was also studied. It was found that the SS could keep the nanoparticles dispersed for over one day. The NZVI was characterized by XRD, FE-SEM, ESEM-EDS, and EDS-mapping, to observe its morphology and crystal structure. In this research the iron species observed took non-crystalline forms.
In water batch tests, studies in deionized water were compared with those in simulated groundwater with humic acid, and dissolved oxygen content was adjusted. Injection of NZVIS oxidized As(III) to As(V) in all cases. In both deionized water and simulated groundwater, it was found that when the dissolved oxygen(DO) content was not increased, the NZVIS generated non-selective oxidant OH•, thus reducing the As(V) production rate. When dissolved oxygen content was increased, the DO oxidized organic matter present in the simulated groundwater, allowing the OH• to react further with As(III) and increasing the As(V) production rate. Finally, a test was performed in actual groundwater under optimal reaction conditions, without increasing the dissolved oxygen content, for comparison of As(V) yield. The concentration of As(V) was found to be higher in this test (As(V) Conc. = 17.55 μg/L) than when using simulated groundwater (As(V) Conc. = 4.63 μg/L).
This study further examined NZVIS injection combined with electrokinetic (EK) technology for the remediation of soil columns containing a low concentration (initial conc. = 100 mg/kg) and a high concentration (initial conc. = 500 mg/kg) of As(III). EK alone without injection of NZVIS (Test E-1) resulted in a residual soil As(V) concentration of 24 mg/kg in the low-concentration test group. In Test E-2, where NZVIS was injected into the anode reservoir, and Test E-3, where NZVIS was injected into the cathode reservoir, residual soil As(V) concentrations were 2.3 mg/kg and 3.4 mg/kg, respectively.
The high-concentration test group was comprised of Test E-4 (EK alone without injection of NZVIS), Test E-5 (NZVIS injected into anode reservoir), and Test E-6 (NZVIS injected into cathode reservoir). In these tests, only soil sections 0.2 and 0.4 (normalized distance from anode reservoir) met soil regulation standards. Residual As(V) concentrations in soil sections 0.6, 0.8, and 1.0 are much higher than the regulatory standard. In soil section 1.0, the residual As(V) concentration was less in Test E-6 than in Test E-5 (116.6 mg/kg and 183.5 mg/kg, respectively). This may be because at high pH values, the iron surface does not corrode, instead arsenic adsorption prevails. Only a fraction of negatively charged As(V) species will migrate towards the anode resulting in a relatively low soil As(V) concentration near the cathode.

目錄

聲明切結書 i
謝誌 ii
摘要 iii
Abstract v
圖目錄 x
表目錄 xiv
照片目錄 xv
第一章 前言 1
1-1 研究緣起 1
1-2 研究目的 4
1-3 研究架構與內容 4
第二章 文獻回顧 6
2-1 重金屬砷 6
2-1-1 砷物種於自然界中分布及其物化特性 6
2-1-2 砷對人體健康危害特性 8
2-1-3 世界上高濃度砷之分佈及管制標準 9
2-2 Fenton法及類-Fenton法相關理論介紹 14
2-1-1 Fenton法之相關理論 14
2-1-2 類-Fenton法之相關理論 16
2-1-3 影響類-Fenton法之相關因子 17
2-3 奈米級零價鐵之發展與污染物的反應機制 20
2-3-1 氧化或還原反應機制原理 20
2-3-2 吸附反應機制 25
2-4 電動力整治技術 27
2-4-1 電動力技術之基本反應原理 27
2-4-2 影響電動力法處理孔隙間污染物的相關因子 31
2-4-3 利用電動力技術整治土壤污染相關之研究 34
第三章 實驗材料與方法 36
3-1 研究材料與試劑 36
3-2 研究設備 38
3-3 研究方法 41
3-3-1 奈米級零價鐵的製備與基本特性分析 41
3-3-1-1 可溶性澱粉添加奈米級零價鐵於水溶液中穩定探討 42
3-3-1-2 奈米級零價鐵物種鑑定 44
3-3-1-3 奈米級零價鐵之顆粒形貌及粒徑觀測 45
3-3-1-4 環境掃描式電子顯微鏡X-光能譜分析儀(ESEM-EDS)與元素能量 分佈面描分析(EDS-Mapping)之分布形 45
3-3-2 模擬地下水配製及實際地下水離子濃度檢測 46
3-3-3 奈米級零價鐵於水溶液中氧化As(III) 47
3-3-3-1 高錳酸鉀滴定法(雙氧水檢測法) 48
3-3-3-2 醋酸鹽型態強鹼型陰離子交換樹脂的製備 48
3-3-3-3 水溶液中分離As(III)及As(V)之試驗 49
3-3-3-4 pH值及溶氧量對氧化不同水溶液中As(III)之影響 51
3-3-4 奈米級零價鐵懸浮液結合電動力技術整治飽和土體中As(III)試驗 53
3-3-4-1 As(III)於土體中吸附試驗 56
3-3-4-2 人工污染土樣製備及土壤管柱的填充 57
3-3-4-3 每日反應過程分析 57
3-3-4-4 試驗前後之土壤分析 58
第四章 結果與討論 64
4-1 奈米級零價鐵基本特性分析 64
4-1-1 X-光繞射(X-Ray Diffraction, XRD)物種成分分析 64
4-1-2 場發射型掃瞄式電子顯微鏡FE-SEM (Field Emission Scanning Electron Microscope) 66
4-1-3 環境掃描式電子顯微鏡-X-光能譜分析儀(ESEM-EDS)與能量分佈面描分析(EDS-Mapping) 67
4-2 奈米鐵懸浮液之穩定性探討 69
4-3 利用高錳酸鉀檢測水溶液中過氧化氫 74
4-4 As(III)及As(V)之分離 75
4-5 去離子水、模擬地下水及實際地下水中改變pH值對As(III)氧化成 As(V)的影響 77
4-6 去離子水和模擬地下水中改變溶氧對As(III)氧化成As(V)的影響 83
4-7 土壤樣品基本特性分析 87
4-8 去離子水中改變奈米級零價鐵劑量對As(III)氧化成As(V)的影響 88
4-9 泥漿試驗 91
4-10 奈米級零價鐵懸浮液注入結合電動力整治技術處理土壤中As(III) 試驗 93
4-11 奈米級零價鐵結合電動力技術經濟效益評估 113
4-12 高濃度As(III)試驗組別之長期整治試驗 116
第五章 結論與建議 124
5-1 結論 124
5-2 建議 127
參考文獻 128
附錄 142

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