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研究生：	謝汶興 Hsieh, Wen-Hsing
論文名稱：	2-MIB與Geosmin在土壤-水系統分佈及淨水程序之處理研究 Distribution of 2-MIB and Geosmin in Soil-Water System and Their Treatment in Waterworks
指導教授：	林財富 Lin, Tsair-Fuh
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：	106
中文關鍵詞：	自來水、臭味、2-MIB 、Geosmin 、脫水效應、pH 、Freundlich模式、等溫吸附線
外文關鍵詞：	Drinking water, odor, 2-MIB, Geosmin, dehydration；pH；Freundlich model, adsorption isotherm
相關次數：	點閱：218 下載：5
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摘要

自來水中藻類代謝物為重要水質議題，其中2-Methylisoborneol (2-MIB) 及 trans-1,10-dimethyl-trans-9-decalol (geosmin)在為常見水中臭味的化學物質，在低濃度即可聞到味道，對自來水供水舒適性影響很大。為提升水中臭味物質之控制，良好之分析方法及對水系統的分布的了解，可以進步提升2-MIB及geosmin的控制。

本研究首先探討分析2-MIB及geosmin時，受pH值之影響、及其改善方法，以提升分析精準性。研究中針對固相微萃取、吹氣捕集及液向萃取等三種濃縮技術運用於2-MIB及geosmin之分析，發現水中之2-MIB及geosmin濃度與pH值相關。該兩種化合物在酸性條件下易引起脫水作用，pH值愈低、影響越明顯。在pH值5以下，分析結果開始明顯產生偏差，利用固相微萃取、吹氣捕集及液向萃取等濃縮技術，在pH值為2.5的條件下所得到的分析結果，相較於中性條件(pH=6~7)分別降低為87%, 16%, and 37%。研究亦顯示，分析結果與pH值變化的路徑無觀，顯示2-MIB及geosmin之脫水效應為可逆，可藉由調整pH值保障其分析準確性。

本研究亦對金門太湖及榮湖等兩座傳統流程淨水廠之原水及流程水取樣分析發現，金門水系統中，2-MIB較geosmin出線機率及濃度均高出許多，74%之原水及32%之處理水中2-MIB之濃度均高於閾值(~10 ng/L)，另外亦發現水體中的2-MIB大約70%均以溶解相存在。原水中的藍綠細菌在加氯6.4mg/L接觸15分鐘後，藍綠細菌的細胞會出現破裂。另外浮除程序可以有效去除藍率細菌且去除率大約為77-79%，但2-MIB在浮除之前的程序去除率僅17-28%，乃受限於細胞內的2-MIB較少所致。對於兩座淨水廠之快濾程序對2-MIB之去除率僅23-47%，亦可能為生物降解效應所致。有關此兩座淨水廠對2-MIB之總去除效率大約為74%，證實金門飲用水及處理水中2-MIB為臭味之主要來源，而濃度現有的處理程序已無法再使濃度降至閾值下，後續須由淨水高級處理程序負擔。

研究中亦初步探討兩種臭味物質在3種土壤、及1種底泥之吸附特性，研究結果顯示其吸附量與有機質含量有明顯相關，雖無法直接以線性關係與有機質含量相連結，可以以Freundlich等溫線描述。

關鍵辭：自來水、臭味、2-MIB、Geosmin、脫水效應、pH、Freundlich模式、等溫吸附線

Abstract

Cyanobacteria in drinking water sources and in recreational waters have received increasing attention worldwide because of their adverse effects on water quality. Not only cyanobacteria themselves are toxin producers, but also they may produce noxious metabolites, including taste and odor (T&O) substances. The two earthy-musty odorants, i.e., trans-1,10-dimethyl-trans-9-decalol (geosmin) and 2-methyl-isoborneol (2-MIB), are probably most frequently detected in drinking water systems. These two compounds can be detected by human noses at very low (~ ng/L) levels, deteriorating human perception to the water. To better control the two odorants, precise detection methods and understand their occurrence and fate in drinking water systems is therefore very important.

The effects of pH on the analysis of the two chemicals and method to mitigate the impact were first investigated. A gas chromatograph and mass spectrometric detector (GC/MSD) coupled with three preconcentration methods, namely solid-phase microextraction (SPME), purge-and-trap concentration (PTC), and liquid–liquid extraction (LLE), was employed for the analysis. Experimental results indicated that at neutral and alkaline pH conditions, the concentrations detected for both compounds remain constant. However, a substantial reduction of concentration for both chemicals is observed when the water solution pH is less than 5. Under acidic conditions (pH≅2.5), the 2-MIB concentrations detected by GC/MSD coupled with SPME, PTC, and LLE are 87%, 16%, and 37% lower than those measured at pH 6–7, respectively. The pH-dependent behavior was attributed to dehydration of the tertiary alcohols of 2-MIB and geosmin under acidic conditions. The dehydration for 2-MIB and geosmin is reversible, and the analysis can be mitigated by adjusting the water solution pH back to a neutral condition.

The occurrence and treatment of the two earthy-musty odorants was also investigated at two conventional drinking water treatment plants (WTPs) in Kinmen Island, Taiwan. Samples of the source, processed, and finished waters and tap water at the two WTPs were collected and analyzed. Both geosmin and 2-MIB were commonly detected in most water samples, with the 2-MIB concentration much higher than the geosmin concentration. About 74% of the source water samples and 32% of the finished and tap water samples showed detected 2-MIB levels higher than the odor threshold concentration (OTC, ~10 ng/L). Sampling and analysis of the reservoir water indicated that 2-MIB is uniformly distributed in the reservoir, with ~70% of which existing in the dissolved phase. The chlorination study of the raw water indicates that both geosmin and 2-MIB are resistant to chlorine. However, the cyanobacterial cells in raw water were effectively ruptured within 15 minutes of the contact time when a chlorine dosage of 6.4 mg/L was applied at the WTPs. A monitoring of the processed water at WTPs shows that flotation process is most effective to the removal of cyanobacteria, with about 77-79% efficiency, compared to ~99.4% achieved with the whole treatment train. Removal of 2-MIB by the treatment processes before flotation was only about 17-28%, which may be limited to the low ratio of cell-bound 2-MIB. The two sand filtration processes removed 23-47% of 2-MIB, due probably to the biological degradation of dissolved 2-MIB. For the two WTP studied, the removal of 2-MIB was about 74%. It is shown that 2-MIB is a major odorant in the drinking water source and the finished water in Kinmen Island. The current processes are not sufficient to remove 2-MIB to a level below the OTC. Advanced processes are needed to effectively remove the odorant.

Adsorption of 2-MIB and geosmin is also investigated for three soils and one sediment. Preliminary results show that the capacity for the two odorants onto the tested soils increased with increasing soil organic content (SOM). However, no linear relationship can be established between SOM and corresponding capacity. Instead, Freundlich isotherm equations may be used to describe the distribution of the two odorants between soils/sediments and water.

Keywords: Drinking water, odor, 2-MIB, Geosmin, dehydration；pH；Freundlich model, adsorption isotherm

Contents


Abstract (in Chinese)---------------I 
Abstract------II
Acknowledgement-----------------V  
Contents-----VI
Contents of Table---------------VIII
Contents of Figure----------------IX
Chapter 1. Introduction------------1
Chapter 2. Literature Review--------6
2.1 Earthy and musty odour compounds in water-------6
2.2 The characteristics of 2-MIB and geosmin---6
2.3 Degradation pathways of 2-MIB and geosmin-----8
2.4 Fate of odourants in natural water-----11
2.4.1 Occurance of odours in natural water-------12
2.4.2 Influence of advective transport and volatilization on the responses of odourants----12  
2.4.3 Influence of sorption and partition on the responses of odours-----13
2.4.4 Influence of bioaccumulation on the responses of odours----16
2.5 Overview of technology for controlling odour compounds in drinking water----20
2.5.1 Conventional physical processes----20
2.5.2 Oxidation processes-------21
2.5.3 Adsorption---22
2.5.4 Advanced oxidation processes-------22
2.5.5 Membranes process-------23
Chapter 3. Methods and Materials---25
3.1 Materials and methods used for soil-water systems ---25
3.1.1 Soil samples----------------25
3.1.2 Chemicals and apparatus used -------25
3.1.3 Characterization of soil properties---26
3.1.4 Abiotic control--------------30
3.2 Standard solutions and pH adjustment-------30
3.3 Analysis of 2-MIB and geosmin-------31
3.3.1 Analysis methods----------31
3.3.2 Calibration curves----------34
3.4 Adsorption experiments--------37
3.5 Studied sites---38
3.5.1 Field sampling-------------38
3.5.2 Cell counting---------------40
3.5.3 Cell integrity----------------41
Chapter 4. Results and Discussion---42
4.1 Effect of pH on the analysis of 2-MIB and geosmin in water------42
4.1.1 Influence of pH on the responses of odorants in deionized and natural water---42
4.1.2 Dehydration of 2-MIB and geosmin---------------46
4.1.3 Mitigation by pH adjustment---49
4.2 Adsorption of earthy-musty odorants in soil-water systems-----51
4.2.1 Properties of studied soils----51
4.2.2 Adsorption experiments------52
4.2.3 Equilibrium isotherm------58
4.2.4 Adsorption and distribution equilibrium----61
4.3 Occurrence and removal of earthy-musty odorants in two waterworks in Kinmen Island, Taiwan------63
4.3.1 Occurrence of earthy/musty odorants in Kinmen Island’s drinking water systems-----63
4.3.2 Earthy/musty odorants in reservoir water---64
4.3.3 Effect of chlorination on Cyanobacteria cells and odorants---68
4.3.4 Removal of Cyanobacteria in water treatment processes---70
4.3.5 2-MIB removal in water treatment plants------73
Chapter 5. Summary and Conclusions-----76
References-----------------79
Appendix----90
VITA-------105


Contents of Table

Table 2.2.1 Chemical/physical characteristics of MIB and geosmin (Pirbazari et al., 1992; Nalinakumari, B. N., 2002).---7
Table 2.4.1 The loss mechanisms for 2-MIB and geosmin in natural water.-----------20
Table 3.3.1 The detailed programs of GC/MSD.-------33
Table 4.1.1 Effect of temperature on the analysis of 2-MIB and geosmin using SPME-GC-MS.----48
Table 4.2.1 Characteristics of site soils.---51
Table 4.2.2 Characteristics of sediments, Lake Tai.-----51
Table 4.2.3 Component of site soils and sediments, Lake Tai.---52
Table 4.2.4 Isotherm model and parameters for 2-MIB and geosmin on different soils/ Tai Lake sediments (Predicted of Freundlich Isotherm models).---59
Table 4.2.5 Isotherm model and parameters for 2-MIB and geosmin on different soils/ Tai Lake sediments (Predicted with Langmuir Isotherm models).--------60
Table 4.2.6 Koc of 2-MIB or geosmin adsorption on different soils/ Tai Lake sediments (Predicted with Freundlich Isotherm models).----62
Table 4.2.7 Koc of 2-MIB or geosmin adsorption on different soils/ Tai Lake sediments (Prediction of Langmuir Isotherm models).-------62
Table 4.3.1 Removal of 2-MIB in TL and LL waterworks.---75


Contents of Figure

Figure 2.2.1 2-MIB & geosmin chemical structure.(Li, Z., 2003)-7
Figure 2.3.1 Dehydration products of 2-MIB. (Martin et al., 1988)-8
Figure 2.3.2 Structure of possible dehydration products for geosmin.(Bamuza-Pemu et al., 2011)-9
Figure 2.3.3(a) Scheme 1-proposed products from sonolysis of 2-MIB in aqueous solution based on GC/MS analyses. (Song et al., 2007)-10
Figure 2.3.3(b) Scheme 2-proposed products from sonolysis of geosmin in aqueous solution based on GC/MS analyses. (Song et al., 2007)-11
Figure 2.4.1 The releases of 2-MIB and geosmin of natural water includes several loss mechanisms.-12
Figure 2.4.2 Correlation of log Koc and log Kow of neutral organic chemicals. (Karickhoff, 1981)-14
Figure 2.4.3 Relationship between geosmin concentration in the sediment and 
overlying water of Xionghe Reservoir. Values are averages (n= 2). (Zuo et al., 2010).-15
Figure 2.4.4 Correlation of log BCF and log Kow of neutral organic chemicals. (Nendza M., 1991)-17
Figure 3.1.1 Appearance of test soils.-25
Figure 3.1.2 Textural triangle of soil.-28
Figure 3.3.1 SPME concentration system.-33
Figure 3.3.2 Concentration calibration curve of 2-MIB.-35
Figure 3.3.3 Concentration calibration curve of geosmin.-35
Figure 3.3.4 Lower concentration calibration curve of 2-MIB.-36
Figure 3.3.5 Lower concentration calibration curve of geosmin.-36
Figure 3.4.1 Schematic flow chart of the adsorption experiments.-37
Figure 3.5.1 Map of the studied sites in Kinmen Island.-40
Figure 3.5.2 Common treatment trains for Tai Lake and Long Lake water treatment. plants.-40
Figure 4.1.1 The concentrations of 2-MIB and geosmin (GSM) in deionized water (DW) and Lake Tai (LT) at different water solution pH using GC/MSD-SPME. The initial concentrations of 2-MIB and geosmin in DW were 294 and 380 ng/L, respectively, while that of 2-MIB for LT was 131 ng/L.-44
Figure 4.1.2 The concentrations of 2-MIB and geosmin (GSM) in deionized water (DW) at different water solution pH, where a is analyzed using GC/MSD-PTC (initial 2-MIB concentration=350 ng/L and initial GSM concentration=208 ng/L), and b is GC/MSD-LLE (initial 2-MIB concentration=360 ng/L and initial GSM concentration=392 ng/L).-45
Figure 4.1.3 The concentration recovery of 2-MIB and geosmin (GSM) at different pH after the water solution pH is adjusted to pH 6–7.-50
Figure 4.2.1 The time course of 2-MIB or geosmin concentrations for the adsorption in soil-water systems. -53
Figure 4.2.2 The time course of 2-MIB or geosmin concentrations for the adsorption in sediment-water systems.-53
Figure 4.2.3 Adsorption of 2-MIB and geosmin on different soils (Prediction of Freundlich Isotherm models).-54
Figure 4.2.4 Adsorption of 2-MIB and geosmin on different soils (Prediction of Langmuir Isotherm models).-55
Figure 4.2.5 The observed and predicted sorption of 2-MIB and geosmin on different sediments at different equilibrium concentration (Predicted with Freundlich Isotherm models)-56
Figure 4.2.6 The observed and predicted sorption of 2-MIB and geosmin on different sediments at different equilibrium concentration (Predicted with Langmuir Isotherm models).-57
Figure 4.3.1 Cumulative distribution of 2-MIB concentrations detected in Tai-Lake Reservoir (TLR, Sample Number (N) = 54), Long Lake (LLR, N = 11), and tap and finished water (N = 58) in Kinmen Island. -64
Figure 4.3.2 Diurnal concentration changes of 2-MIB and geosmin for the samples taken at the raw water intake of Tai-Lake Waterworks (TLW), where (a) is for the samples taken at depth = 4.0 m in August 2005, and (b) is for the samples taken at different depths in September 2005. (Yen, 2010)-67
Figure 4.3.3 Chlorination of raw water from Tai-Lake Waterworks (TLW), (a) effect on cyanobacteria (initial concentration = 1.1105 cells/mL) and (b) effect on 2-MIB and geosmin concentrations.-69
Figure 4.3.4 Removal of cyanobacteria cells in (a) Tai-Lake Waterworks (TLW), and (b) Long-Lake Waterworks (LLW).-72
Figure S-4.2.1 Microstructure of Chenggong soil.-90
Figure S-4.2.2 Microstructure of Linnei soil.-90
Figure S-4.2.3 Microstructure of Taoyuan soil.-90
Figure S-4.2.4 BET surface area of Chenggong soil.-91
Figure S-4.2.5 Pore volume of Chenggong soil.-92
Figure S-4.2.6 Pore area of Chenggong soil.-92
Figure S-4.2.7 Volume adsorbed of Chenggong soil.-93
Figure S-4.2.8 Volume adsorbed of Linnei soil.-93
Figure S-4.2.9 BET surface area of Linnei soil.-94
Figure S-4.2.10 Pore volume of Linnei soil.-95
Figure S-4.2.11 Pore area of Linnei soil.--95
Figure S-4.2.12 BET surface area of Taoyuan soil.-96
Figure S-4.2.13 Pore volume of Taoyuan soil.-97
Figure S-4.2.14 Pore area of Taoyuan soil.-97
Figure S-4.2.15 Volume adsorbed of Taoyuan soil.-98
Figure S-4.2.16 Volume adsorbed of sediment, 0~0-15cmD, Lake Tai.-98
Figure S-4.2.17 BET surface area of sediment, 0~0-15cmD, Lake Tai.-99
Figure S-4.2.18 Particle size distribution of sediment, 0~0-15cmD, Lake Tai.-100
Figure S-4.2.19 Volume adsorbed of sediment, 0-15~0-30cmD, Lake Tai.-100
Figure S-4.2.20 BET surface area of sediment, 0-15~0-30cmD, Lake Tai.-101
Figure S-4.2.21 Particle size distribution of sediment, 0-15~0-30cmD, Lake Tai.-102
Figure S-4.2.22 Volume adsorbed of sediment, 0-30~0-60cmD, Lake Tai.-102
Figure S-4.2.23 BET surface area of sediment, 0-30~0-60cmD, Lake Tai.-103
Figure S-4.2.24 Particle size distribution of sediment, 0-30~0-60cmD, Lake Tai.-104

                                    

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