應用雷射剝蝕感應耦合電漿質譜儀及超音波影像系統探討以薄膜處理廢水的阻塞問題

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研究生：	徐建華 Hsu, Chien-Hua
論文名稱：	應用雷射剝蝕感應耦合電漿質譜儀及超音波影像系統探討以薄膜處理廢水的阻塞問題 Using LA-ICP-MS and ultrasound imaging system to investigate fouling of membrane in wastewater treatment
指導教授：	王竹方 Wang, Chu-Fang
口試委員:	張怡怡 Chang, E-E. 蔣本基 Chiang, Pen-Chi 林俊德 Lin, Justin Chun-Te
學位類別：	碩士 Master
系所名稱：	原子科學院 - 生醫工程與環境科學系 Department of Biomedical Engineering and Environmental Sciences
論文出版年：	2013
畢業學年度：	101
語文別：	英文
論文頁數：	125
中文關鍵詞：	薄膜、錯合物、金屬、雷射剝蝕感應耦合電漿質譜儀
外文關鍵詞：	membrane, complex, metal, laser ablation inductively coupled plasma mass spectrometer
相關次數：	點閱：3 下載：0
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近年來，化學工業所產生的重金屬是汙染環境水體主要來源，但現今廢水處理技術無法有效將重金屬物質清除乾淨。此外，如離子交換和溶劑萃取的預處理過程會產生有機物的二次性污染，因此本研究使用薄膜過濾技術，進行去除廢水中微量重金屬物質(Co)與螯合劑(APDC)與所形成錯合物的方法。本研究將探討不同追蹤物的溶質系統(Co、Sr及Cs)對APDC的影響，研究結果可發現在不同單溶質系統中，APDC的選擇性大小為Co>>Sr>Cs。LA-ICP-MS結合α-step輪廓分析儀驗證可應用在薄膜追蹤有機物的影像分佈情形。研究結果中利用Hermia模式進行分析阻塞機制，並以Co作為追蹤劑，探討不同有機物(APDC、LAS、SDS及CTAB)與Co元素的錯合能力，並搭配LA-ICP-MS去分析薄膜表面上有機物的影像分佈情形，其結果顯示以APDC-Co中的S和Co元素分佈最相似(R2= 0.9402)，代表有很強的結合能力。而為了將薄膜回收再利用，研究中亦探討使用不同化學藥劑(純水、2% HCl及1M NaOH)去除薄膜阻塞物，並搭配超音波影像系統觀察薄膜清洗後表面粗糙程度。

In recent years, industrial wastewater is a major source of metal polluting in the environment. However, there is still no effective way to remove heavy metal in the wastewater. In addition, pretreatment processes such as ion exchange and solvent extraction suffer from the secondary pollution caused by the spent resins/solvent. In this study, membrane filtration techniques to remove trace metals and spent resins/solvent in the simulated wastewater Co, Sr and Cs are selected to evaluate the chelating ability of APDC. The results show that the selectivity of APDC is in the following order: Co >> Sr> Cs. Through the LA-ICP-MS and α-step profilometer measurement, the obtained results are consistent with fouling mechanisms based on Hermia model and reveal that the chelating complex could be used as a tracer to demonstrate the phenomenon of organic fouling in the membrane filteration.. Thus Co is chosen to explore the complexation ability of different organics (APDC, LAS, SDS and CTAB) as well as a tracer to present the spatial distribution of organics on the membrane surface. The results show that the distribution of S and Co in the APDC-Co sample has high correlation (R2 = 0.9402) and reveals strong affinity between APDC and Co. The ultrasonic imaging system is also conducted to investigate the depth/ roughness of membrane surface before and after the foulant removing by different chemical agents (water, 2% HCl and 1M NaOH)).

Contents
摘要    I
Abstract    II
謝誌    III
Contents    IV
Table index    VII
Figure index    IX
Chapter 1 Introduction    1
1.1. General overview    1
1.2. Aims of this study    3
Chapter 2 Literature Review    5
2.1. Introduction of membranes    5
2.1.1. Classification of membranes    5
2.1.2. Membrane materials    7
2.1.3. Transport mechanisms of membrane filtration     9
2.1.4. Scale formation    12
2.1.5. Hermia model for membrane fouling    14
2.2. Application of membrane technology to simulated radioactive laundry
wastewater treatment     17 
2.2.1. States-of-the arts in membrane surface characterization    17
2.2.2. Selection of inorganic species as model scalants    20
2.3. Identification of membrane fouling and surface analysis    24
2.3.1. Conventional analytical methods for fouled membranes    24
2.3.2. Developments and applications of LA-ICP-MS    29
2.3.3. Mapping technique of LA-ICP-MS    33
2.3.4. Depth profile of LA-ICP-MS    34
Chapter 3 Experimental    35
3.1. Reagents and materials    35
3.2. Apparatus and device    38
3.2.1. Three-channels high pressure plate-and-frame membrane 
filtration system    38
3.2.2. LA-ICP-MS    39
3.2.3. α-step profilometer    43
3.2.4. Total Organic Carbon(TOC) Analyzer    45
3.2.5. Ultrasound imaging system    45
3.3. Details of experimental methods    48
3.3.1. Filtration and cleaning protocols    48
3.3.2. MF/UF/NF/RO scaling tests    49
3.3.3. Mapping technique of LA-ICP-MS    50
3.3.4. Depth profile of fouled membranes    51
Chapter 4 Results and discussion    53
4.1. Study of tracing ability of APDC with different metal    53
  4.1.1. Effect of single-species (APDC-Co, APDC-Sr, APDC-Cs) on 
       fouling    53
  4.1.2. Membrane depth analysis of the obstructions    58
  4.1.3. The fouling distribution based on Hermia model    65
4.2. Study of tracing ability of diffent surfactant and chelating agent with Co    69
4.2.1. The effect of organics on the fouling of membrane    69
4.2.2.2-D distribution image of the fouling on the membrane surface
            71
4.2.3. Fouling mechanism identified by Hermia model    74
4.3. Application of ultrasonic image technology on fouled RO and NF Membranes    77
4.3.1. Membranes Comparison of two-dimensional image for 
      membrane after cleaning     77
4.3.2. Membranes Comparison of three-dimensional image for 
      membrane after cleaning     81
Chapter 5 Conclusions and future work    91
5.1. Conclusions    91 
5.2. Future work    93
Chapter 6 Reference    94 
Appendix    104 












Table index
Table 2.1 Characteristics of various membranes    9
Table 2.2 Fouling Index of various membrane types, filtration modes and 
equations    10
Table 2.3 Filtration mode, value of k2 and filtration equation    15
Table 2.4 Nomenclature    16
Table 2.5 Main radioactive elements from different sources    19
Table 2.6 Comparison of different treatment methods    19
Table 2.7 Classification of surfactants    23
Table 2.8 Recent applications of LA-ICP-MS    30
Table 2.9 Comparison of LA-ICP-MS and other analytical techniques    31
Table 3.1 General information of selected organics in the experiment    36
Table 3.2 Properties of the membranes employed in this study.    37
Table 3.3 Operation conditions for laser ablation    41
Table 3.4 The scan parameters of Dektak-150 profilometer system in this study
             44
Table 3.5 The scan parameters of utrasound imaging system in this study    47
Table 3.6 The concentration of complex used in the experiments    50
Table 4.1 The rejection of different species system [mean mg L−1 (S.D.) , n= 3]    54
Table 4.2 Intensity signal of each layer [mean (S.D.) , n= 3]    59
Table 4.3 K constants of four Hermia's model for individual cations and their complex    67
Table 4.4 R2 values of four Hermia's model for individual cations and their complex.    68
Table 4.5 K constants of four Hermia's model for individual cations and their complex.    75
Table 4.6 R2 values of different fouling model for different organic matter    76
Table 4.7 Signal intensity (in dB) of RO and NF membrane before and after cleaning by ultrasound. [mean db (S.D.) , n= 3]    80
Table 4.8 Total thickness of RO and NF membrane before and after cleaning by ultrasound. [mean μm (S.D.) , n= 3]    89
Table 4.9 Signal thickness of upper layer and inner layer for RO membrane before and after cleaning by ultrasound. [mean μm (S.D.) , n= 3]    89
Table 4.10 Signal thickness of upper layer and inner layer for NF membrane before and after cleaning by ultrasound. [mean μm (S.D.) , n= 3]    90
Table A.1 Complex permeability and linearity coefficient of test membranes    104
Table A.2 Effect of operational pressure on rejections [ mean mg L−1 (S.D.) , n= 
3] by TOC and ICP-MS analysis. (APDC-Co : 50 ppm and 10 ppm)    105
Table A.3 Effect of different membrane on rejections [mean mg L−1 (S.D.) , n= 3] 
by TOC and ICP-MS analysis. (APDC-Co : 50 ppm and 10 ppm)    106
Table A.4 R2 values of different fouling model for different membrane.    107
Table B.1 EDS of weight percent of element in APDC-Co, LAS-Co , SDS-Co and  
CTAB-Co    107








        Figure index
Figure 1.1 Research scopes and experiment flowcharts    4
Figure 2.1 The pore size and driving force of different filtration    6
Figure 2.2 Schematic diagram of scale formation    13
Figure 2.3 Schematic diagram of four types of fouling mechanisms    16
Figure 2.4 Stucture diagram of APDC combine with divalent metal ion    21
Figure 2.5 Micelle formation process    23
Figure 2.6 (a) Schematic diagram of UTDR measure (b) corresponding 
time-domain responses for the configuration.    25
Figure 2.7 Comparison of ultrasonic image with SEM for the control PES 
membrane (a) cross section, (b) layers upon the non-woven support, 
and (c) membrane layer    26
Figure 2.8 Ni-MOF-74 membrane surface image of (a) 1 cycle, (b) 2 cycle, (c) 4 
cycle, and (d) 8 cycle    27
Figure 2.9 Ni-MOF-74 membrane (a) surface image (d) cross-sectional image    28
Figure 3.1 A photograph of membrane filtration system    38
Figure 3.2 The schematic diagram of membrane filtration system (Dead-end)    39
Figure 3.3 A photograph of Newwave UP 213 laser system    40
Figure 3.4 The schematic diagram of the LA-ICP-MS system    41
Figure 3.5 A photograph of Agilent 7500a ICP-MS    42
Figure 3.6 The schematic diagram of ICP-MS    43
Figure 3.7 A photograph of α-step profilometer system    44
Figure 3.8 The meaning of IR spectrum    47
Figure 3.8 Schematic diagram of ultrasonic imaging system for membrane scaling    48
Figure 3.9 Illustrations of B-mode scanning    48
Figure 3.10 The image of the line scan mode after ablation    51
Figure 3.11 (a) Craters on the membrane surface ablated by laser system in 1, 5, 10, 20, 40, 60 seconds ; (b) Cross-section of the ablation craters measured by Dektak 150    52
Figure 4.1 The flux of (a) APDC-Co (b) APDC-Sr (c) APDC-Cs    54
Figure 4.2 The distribution image of elements on the membrane. APDC-Co: (a) S (b) Co; APDC-Sr: (c) S (d) Sr; APDC-Cs: (e) S (f) Cs.    56
Figure 4.3 The correlation matrix of analyzed elements in the APDC-Co: (a) S and Co; APDC-Sr: (b) S and Sr ; APDC-Cs: (c) S and Cs    57
Figure 4.4 Signal intensity of each element (pH = 3) in different depth of the fouled RO membranes (a) pure Co (b) pure Sr (c)  pure Cs (d) APDC-Co (e) APDC-Sr (f) APDC-Cs.    60
Figure 4.5 Elements fouling distribution in different depth (a) Co2+ (b)
APDC-Co    62
Figure 4.6 Elements fouling distribution in different depth (a) Sr2+ (b)
APDC-Sr    63
Figure 4.7 Elements fouling distribution in different depth (a) Cs + (b)
APDC-Cs.    64
Figure 4.8 Flux of different operation time for fitting model (a)Co2+ (b) APDC-Co (c) Sr2+ (d) APDC-Sr (e) Cs+(f) APDC-Cs    67
Figure 4.9 The flux of complexes    70
Figure 4.10 The rejection of complexes    70
Figure 4.11 shows imagines of elemental distributions of various samples on the membrane. (a) S of APDC-Co; (b) Co of APDC-Co; (c) S of LAS-Co; (d) Co of LAS-Co; (e) S of SDS-Co; (f) Co of SDS-Co; (g) S of CTAB-Co; (h) Co of CTAB-Co APDC-Co    72
Figure 4.12 The correlation matrix of analyzed elements in the APDC-Co:(a) S and Co ; LAS-Co/Cs : (b) S and Co ; SDS-Co:(c) S and Co CTAB-Co: (d)S and Cs    73
Figure 4.13 Flux of different operation time for fitting model (a) APDC-Co (b) LAS-Co (c) SDS-Co (d) CTAB-Co    75
Figure 4.14 Two-dimensional ultrasonic image of RO membrane surface (a) Virgin ; (b),(c) and (d) without cleaning ; (e) pure water cleaning ; (f) 2% HCl cleaning (g) 1M NaOH cleaning    79
Figure 4.15 Two-dimensional ultrasonic image of NF membrane surface (a) Virgin ; (b),(c) and (d) without cleaning ; (e) pure water cleaning ; (f) 2% HCl cleaning (g) 1M NaOH cleaning    79
Figure 4.16 Three-dimensional ultrasonic thickness image of RO membrane (a)Virgin; (b),(c) and (d) without cleaning ; (e) pure water cleaning ; (f) 2% HCl cleaning (g) 1M NaOH cleaning    83
Figure 4.17 Three-dimensional ultrasonic thickness image of NF membrane (a Virgin; (b),(c) and (d) without cleaning ; (e) pure water cleaning ; (f) 2% HCl cleaning (g) 1M NaOH cleaning.    84
Figure 4.18 Three-dimensional ultrasonic thickness image of RO membrane. Upper layer:(a),(b),(c) without cleaning,(d)pure water cleaning, (e) 2% HCl cleaning, (f) 1M NaOH cleaning.    85
Figure 4.19 Three-dimensional ultrasonic thickness image of RO membrane. Lower layer:(g),(h),(i) without cleaning,(j)pure water cleaning, (k) 2% HCl cleaning, (l) 1M NaOH cleaning    86
Figure 4.20 Three-dimensional ultrasonic thickness image of NF membrane. 
Upper layer:(a),(b),(c) without cleaning,(d)pure water cleaning, (e) 2% HCl cleaning, (f) 1M NaOH cleaning.    87
Figure 4.21Three-dimensional ultrasonic thickness image of NF membrane. Lower layer:(g),(h),(i) without cleaning,(j)pure water cleaning, (k) 2% HCl cleaning, (l) 1M NaOH cleaning.    88
Figure A.1 Effect of pressure on permeate flux    109
Figure A.2 Photographs of fouled membranes (a) RO; (b)NF; (c) UF; (d) MF    109
Figure A.3 Permeate flux of the four membranes in filtration the APDC-Co solution: (a) RO (b) NF (c) UF (d) MF.    110
Figure A.4 The fouling mode fitting of operation time for (a) RO (b) NF (c) UF 
(d) MF.    111
Figure A.5 Saturation index of Co species at different pH    112
Figure A.6 The flux of (a) pH3 (b) pH7 (c) pH9    113
Figure A.7 Effect of the pH value on rejections.TOC and ICP-MS analysis: 
APDC-Co; 50 ppm; 10 ppm    114
Figure A.8 The photos of different APDC concentrations on binding of Co. (a) 
1:1(b) 2:1 (c) 3:1    115
Figure A.9 The flux of (a) APDC-Co (1:1) (b) APDC-Co (2:1) 
(c) APDC-Co (3:1)..    116
Figure A.10 The rejection of APDC-Co under different APDC concentration    117
Figure B.1 FT-IR spectrum of (a) APDC (b)APDC-Co (c) LAS (d) LAS-Co (e) SDS (f) SDS-Co (g) CTAB (h) CTAB-Co    120
Figure B.2 (A) The photograph and (B) DLS spectrum of (a) APDC-Co (b) LAS-Co (c) SDS-Co (d) CTAB-Co    121
Figure B.3 SEM-EDX of complexes. APDC-Co: (a) and (b); LAS-Co: (c) and (d) ; SDS-Co: (e) and (f) ; CTAB-Co: (g) and (h)    123
Figure B.4 The photos of different complexes fouling (a) APDC-Co(b) LAS-Co (c) SDS-Co (d) CTAB-Co    124 
Figure B.5 The photo of fouled membrane is respective (a)APDC-Co; (b) APDC-Sr; (c) APDC-Cs    124
Figure B.6 SEM of fouled membranes..(a) MF, (b)UF, (c) NF and (d) RO    125



                                

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