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研究生：	潘毅峰 Pan, Yi-Fong
論文名稱：	三種鐵氧化物對水中砷之吸附平衡與動力特性研究 Adsorption Equilibrium and Kinetics of Arsenic onto Three Iron Oxide Based Adsorbents
指導教授：	林財富 Lin, Tsair-Fuh
共同指導教授:	邱成財 Chiou, Cary-T.
學位類別：	博士 Doctor
系所名稱：	工學院 - 環境工程學系 Department of Environmental Engineering
論文出版年：	2013
畢業學年度：	101
語文別：	英文
論文頁數：	113
中文關鍵詞：	三價砷、五價砷、吸附、競爭、氧化、鐵氧化物覆膜矽藻土、混合型陰離子交換樹脂、地下水
外文關鍵詞：	arsenite (As(III)), arsenate (As(V)), adsorption, competition, oxidation, iron oxide coated diatomite (IOCD), hybrid anion exchange resins, groundwater
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本研究探討鐵氧化物吸附劑，對水中砷之吸附效能。研究中首先以矽藻土為基材，以鐵氧化物進行改質，製造鐵氧化物覆膜之矽藻土(Iron oxide coated diatomite, IOCD)，探討其材料特性及吸附特性，然後將其應用於天然地下水砷吸附，以探討地下水水質對其影響。為比較不同鐵氧化物吸附劑，研究並將IOCD與兩種商用型水合鐵礦改質之陰離子交換樹脂，進行吸附特性比較。
矽藻土經鐵氧化物覆膜後，其對五價砷之吸附量較原始矽藻土可明顯提升約30倍，惟其吸附效能與鐵氧化物覆膜次數並非成正比，以0.11 mm之矽藻土做為載體，最佳覆膜次數為2次；以0.43 mm做為載體，則最佳覆膜次數為3次。表面分析結果顯示，矽藻土上之鐵氧化物為赤鐵礦(Hematite, -Fe2O3)，表面積並可以由51 m2/g增加至93 m2/g，兩者(表面正電荷及表面積增加)為造成吸附量增加之主因。IOCD與五價砷之吸附反應係屬放熱反應，當溫度由20升高至50oC時，吸附量會由6.5降低至 5.7 mg/g，其吸附熱值(Isosteric heat, )介於-4至-9 kcal/mol間，推論同時存在物理及化學吸附力。平衡吸附試驗數據以Freundlich模式較Langmuir模式模擬較佳。動力吸附結果顯示IOCD對五價砷之吸附量會隨pH值升高而減少，動力數據除可以Pseudo-second-order方程式模擬外，Pore-diffusion model亦可成功用以模擬並預測孔隙擴散行為，而五價砷於IOCD之孔隙擴散係數(Dp)為3×10-7 cm2/sec。
研究中亦嘗試將IOCD應用於處理台灣嘉義地區之含砷地下水。所採集之地下水之砷濃度約30 g/L，且主要砷物種為五價砷。以高效粒徑排除層析儀(High performance size exclusion chromatography, HPSEC)分析含砷地下水顯示砷與鐵及錳無吸附作用，而此水樣於非厭氧狀態下，經約20天之觀測結果發現砷濃度並無顯著變化，故進而判定該天然砷為溶解態。平衡吸附結果指出，相較於以去離水配製之五價砷，IOCD對於含砷地下水之吸附量僅佔65%，其中以磷酸鹽及天然有機物(Natural organic matter, NOM)之影響最大。將經混凝後之地下水進行吸附試驗可進而得知，磷酸鹽之競爭吸附為對於五價砷吸附量降低之最主要原因。
本研究亦選用兩種商用型水合鐵礦改質之陰離子交換樹脂(A33E與FO36)，比較探討其與IOCD對於三價砷及五價砷於去離子水及天然含砷地下水之吸附特性。在以去離子水、中性pH下，IOCD對於三價砷之效附量明顯高於A33E及FO36。當三價砷物種為H2AsO3-時，三種吸附劑可呈現較高之吸附效能，而偶極力亦是三價砷吸附於吸附劑上的主要作用力之一。以五價砷而言，IOCD對於H2AsO4-之吸附量較大，亦即在低pH值條件下。但A33E及FO36則由於選擇性吸附特性，對於HAsO42-之去除率較好。台灣嘉義及鹽水地區地下水之主要砷物種組成分別為五價砷(~ 30 g/L)及三價/五價砷(總砷約1 mg/L；三價砷 : 五價砷 = 6.5 : 1)共存，三種吸附劑對其吸附效能之順序係與含砷去離子水之結果相同。利用同步輻射光源進行X光吸收光譜近邊緣結構 (X-ray absorption near edge structure, XANES)之分析結果顯示，以去離水配製之三價砷溶液吸附於IOCD、A33E及FO36上皆無發生氧化反應，但NOM為使三價砷氧化成五價砷之重要介質。此外，將XANES光譜與含砷地下水之吸附結果比對，可推論IOCD對於三價砷之吸附效能較高，且由於三價砷與五價砷可同時被吸附，因此三價砷之氧化反應較不明顯。
本研究成功開發IOCD吸附劑，並測試與應用於砷之吸附，發現其對三價砷之吸附效果較商用樹脂對五價砷吸附效果則相近。三種吸附劑測試結果顯示，水質特性影響吸附量至鉅，且存在天然有機物下，會造成三價砷氧化作用。在選用吸附程序以處理地下水中砷時，對於地下水中影響砷吸附之相關水質參數，應該全盤性的了解，以提升砷之吸附處理效能。

Methods to economically and efficiently remove arsenic (As) from drinking water supplies are urgently needed in many parts of the world. Iron oxides are known to have a strong affinity for As in water. However, they are commonly present in the forms of fine powder or floc, limiting the applicability in water treatment. In this study, a novel granular adsorbent, iron-oxide-coated diatomite (IOCD), was developed and examined for its adsorption of As from water. The iron-based adsorbent was first studied for its surface properties and adsorption equilibrium and kinetics for As in de-ionized water. To understand the effect of water matrix on the adsorption of As, IOCD was further tested for its adsorption in a groundwater collected from Chiayi and Yanshuei, Taiwan. Finally IOCD was compared with two commercially available iron-based anion exchange resins for their adsorption of As.
Iron-oxide (-Fe2O3, hematite) coated onto diatomite improves sharply (by about 30 times) the adsorption of arsenate (As(V)) from water by the IOCD compared with that by raw diatomite. This improvement was attributed to increases in both surface affinity and surface area of the IOCD. The surface area of IOCD increased to an optimal value with the iron-oxide coating on diatomite. However, as the IOCD surface area (93 m2/g) was only 45% higher than that of the raw diatomite (51 m2/g), the enhanced As(V) adsorption resulted primarily from the enhanced association of negatively charged As(V) ions with the partial positive surface charge of the iron oxide. The As(V) adsorption decreased with increasing solution pH from 3.5 to 9.5, as expected by the partial charge interaction between As(V) and IOCD. The adsorption data at pH 5.5 and 7.5 could be well fitted to the Freundlich equation, and both the pseudo-second-order model and the pore-diffusion model simulated well the adsorption kinetics. A moderately high exothermic heat was observed for the As(V) adsorption, with the calculated molar isosteric heat ranging from -4 to -9 kcal/mol. The observed heats fall between those for physical adsorption and chemisorption and are indicative of the formation of a series of ion-pair complexes of As(V) ions with iron-oxide surface groups. Compared with other iron oxide-based adsorbents reported in the literatures, the adsorption capacity of IOCD is relatively high, and the kinetics is fast.
Removal of As using IOCD was examined for the groundwater near a black foot disease epidemic area, Chiayi, Taiwan. The groundwater was first analyzed for As speciation and water quality that may influence As removal. In the present groundwater, As was present predominately as the penta-valent species and in dissolved form (< 1 kDa) with a concentration of ~ 30 g/L. Adsorption uptake of As(V) onto the studied IOCD in the groundwater was found to be only 2/3 of that from de-ionized water. Among the 10 anions, metals and organic species examined, only phosphate and natural organic matter (NOM) were found to influence the adsorption of As(V) onto iron oxide coated diatomite (IOCD). To further identify the major factor for the suppression of As(V) uptake on IOCD, adsorption experiments were conducted using coagulated groundwater to remove phosphate and NOM to different degrees. Experimental results confirmed that phosphate was the only important species to suppress the As(V) adsorption to IOCD in the studied groundwater.
IOCD and two hybrid anion exchange resins (A33E and FO36) were compared for their adsorption characteristics for arsenite (As(III)) and arsenate (As(V)) in synthetic As solution and natural groundwater. IOCD was found to outperform the two resins tested for adsorption of As(III). However, for As(V), the two resins had better As uptakes. It is found that in groundwater system, adsorption and oxidation of As(III) were both important processes for As(III). Oxidation of As(III) only occurred in the groundwater with NOM presence. Once adsorbed, no oxidation was observed. Since adsorption of As(III) is fast, no oxidation was found for As(III) on IOCD, while significant oxidation was observed for As(III) with A33E and FO36. The results were also confirmed by X-ray absorption near edge structure (XANES) spectra for As-loaded adsorbents.
This study provides some fundamental information on the adsorption equilibrium and kinetics of As onto three iron oxide based adsorbents. The iron oxide based adsorbent, iron oxide coated diatomite (IOCD), was successfully prepared and tested for the adsorption of As species. IOCD and the two commercially available hybrid anion exchange resins showed different adsorption properties. Depending on As speciation and water quality, they may reach different degrees of As uptakes. In addition, oxidation of As(III) may be observed in the presence of NOM in groundwater. It is suggested that in applying iron based adsorbents for the removal of As, an extensive investigation of groundwater components, particularly anions and NOM that may affect adsorption, should be conducted.

Table of Contents

Abstract (In Chinese)	i
Abstract	iv
Acknowledgements (In Chinese)	viii
Table of Contents	ix
List of Figures	xii
List of Tables	xiv


Chapter I: Introduction	1
1.1. Background	1
   1.1.1. Characteristics of arsenic (As)	1
   1.1.2. Removal of As	4
   1.1.3. Influence of water quality in As adsorption	10
1.2. Scope and objectives	11
1.3. Dissertation overview	12

Chapter II: Adsorption of arsenate (As(V)) by iron-oxide-coated diatomite (IOCD)	14
2.1. Introduction	14
2.2. Materials and methods	16
2.2.1. Preparation of IOCD	16
2.2.2. Characterization of IOCD	16
2.2.3. Adsorption experiments	17
2.2.4. Adsorption kinetics	18
2.2.5. Adsorption equilibrium	19
2.3. Results and discussion	20
2.3.1. Characteristics of the adsorbent	20
2.3.2. Effects of diatomite particle size and iron oxide coating level	26
2.3.3. Adsorption equilibrium	28
2.3.3.1. pH effect and adsorption model	28
2.3.3.2. Temperature effect on As(V) adsorption	31
2.3.4. Adsorption kinetics	36
2.3.4.1. Rate of adsorption	36
2.3.4.2. Simulation of pore-diffusion model (PDM) for adsorption kinetic data	39
2.3.5. Comparison of IOCD with other iron oxide materials	43
2.4. Summary	45

Chapter III: Impact of groundwater quality on the adsorption of arsenate (As(V)) onto an iron-oxide based adsorbent: a case study in Chiayi, Taiwan	46
   3.1. Introduction	46
   3.2. Materials and methods	48
      3.2.1. Measurement of groundwater properties	48
      3.2.2. Analytical methods	49
      3.2.3. Adsorption experiments	50
      3.2.4. Adsorption of As(V) after coagulation of the groundwater	51
   3.3. Results and discussion	51
      3.3.1. Groundwater properties	51
      3.3.2. Adsorption of As(V) in de-ionized water and groundwater	57
      3.3.3. Adsorption of anions	59
      3.3.4. Removal of phosphate and NOM from groundwater by coagulation	62
      3.3.5. Effect of phosphate and NOM on As(V) adsorption	67
   3.4. Summary	70

Chapter IV: Comparison of arsenic (As) adsorption by iron oxide based adsorbents in synthetic and natural groundwater	71
   4.1. Introduction	71
   4.2. Materials and methods	73
      4.2.1. Iron oxide based adsorbents	73
      4.2.2. Synthetic As water and natural As-laden groundwater	75
      4.2.3. Adsorption experiments	75
      4.2.4. Synchrotron analysis	75
   4.3. Results and discussion	76
      4.3.1. Adsorption of As in synthetic groundwater	76
4.3.1.1. Competition between adsorption of As(III) and As(V) on IOCD	76
4.3.1.2. pH dependent adsorption for IOCD and hybrid resins	79
      4.3.2. Adsorption of As in groundwater	84
      4.3.3. Determination of As speciation on adsorbents	88
   4.4. Summary	91

Chapter V: Conclusions	92
5.1. Summary	92
5.2. Implication and future research directions	94
5.3. Closing remark	95

References	96

VITA	111

List of Figures

Chapter II
Figure 2-1 SEM image of (a) acidified diatomite, (b) IOCD-20.11, and (c) IOCD-30.43	22
Figure 2-2 Thickness of coated layer onto (a) IOCD-10.43 and (b) IOCD-50.43	23
Figure 2-3 X-ray diffraction (XRD) patterns of raw diatomite and IOCD-20.11	25
Figure 2-4 Adsorption of As(V) on (a) IOCD-1~30.11 and (b) IOCD-1~50.43	27
Figure 2-5 Equilibrium data and fitted models for As(V) onto IOCD-20.11	30
Figure 2-6 Effect of temperature on equilibrium adsorption	33
Figure 2-7 The isosteric heat as a function of As(V) uptake at pH = 7.5	35
Figure 2-8 Adsorption kinetics of As(V) on (a) IOCD-20.11 and (b) IOCD-30.43 at different pHs, where the solid lines represent best fits of the pseudo-second-order model	37
Figure 2-9 Experimental data (symbols) and fitted pore diffusion model (lines) for As(V) adsorption onto IOCD-20.21	42

Chapter III
Figure 3-1 (a) Ultrafiltration results for As, iron, and manganese and (b) time course of As concentration for the studied groundwater	56
Figure 3-2 Adsorption of As(V) onto ICOD in de-ionized water and groundwater	58
Figure 3-3 Adsorption isotherms of anions onto IOCD	61
Figure 3-4 Change of As(V) concentration and pH in the groundwater after coagulation with ferric chloride	64
Figure 3-5 HPSEC spectra of the coagulated groundwater with different coagulant dosages	66
Figure 3-6 Effect of phosphate and NOM on the adsorption of As(V) onto IOCD in coagulated groundwater	69
	
Chapter IV
Figure 4-1 Kinetic adsorption of artificial (a) As(III) and (b) As(V) by IOCD in single (As(III) or As(V)) and binary (As(III) + As(V)) species systems	78
Figure 4-2 pH dependent adsorption for (a) 1 mg/L As(V) and (b) 10 mg/L As(V) onto IOCD, A33E, and FO36 in synthetic groundwater systems	82
Figure 4-3 pH dependent adsorption for (a) 1 mg/L As(III) and (b) 10 mg/L As(III) onto IOCD, A33E, and FO36 in synthetic groundwater systems	83
Figure 4-4 Batch kinetic adsorption of As in (a) Chiayi and (b) Yanshuei groundwater	86
Figure 4-5 Changes of As species upon kinetic adsorption in Yanshuei groundwater with (a) blank (no adsorbent), (b) IOCD, (c) FO36, and (d) A33E	87
Figure 4-6 XANES spectra of As(III) and As(V)-laden IOCD, A33E, and FO36	90

List of Tables

Chapter I
Table 1-1 Major As-laden minerals in the natural environment	3
Table 1-2 Common techniques for the removal of As	6
Table 1-3 A review of iron oxide coating method	8

Chapter II
Table 2-1 Physical properties and elemental compositions of the studied adsorbents	24
Table 2-2 Parameters of Freundlich and Langmuir equations for IOCD-20.11	34
Table 2-3 Parameters in the pseudo-second-order model	38
Table 2-4 Comparison of As(V) adsorption efficiencies among different adsorbents	44

Chapter III
Table 3-1 Characteristics of the studied groundwater	53
Table 3-2 Concentrations of phosphate and NOM in the coagulated groundwater	65

Chapter IV
Table 4-1 Characterizations of studied adsorbents	74
                                    

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