Fate of pollutants in ozone treatment : antibiotics, marine dissolved organic matters, and microplastics

국문 초록 (Abstract)

수질 오염은 일반적으로 인간 활동으로 인해 수역에 부정적인 영향을 미치는 물질 또는 에너지 형태의 추가를 의미한다. 인간의 활동으로 인해 수질오염에 대한 문제는 항상 있어 왔으며, 오염 물질 검출 기술이 발달함에 따라 수계에서 검출되는 오염물질의 종류가 증가하여 수처리의 중요성은 더욱 높아지고 있다. 본 연구에서는 수계에서 문제가 되는 물질 중에서 연구의 필요성이 큰 항생제, 해양 용존유기물질, 미세플라스틱을 선정하여, 오존 기반 산화처리에서 항생제의 제거, 해양 용존유기물질의 영향, 미세플라스틱의 노화에 대해 평가하였다.
연구 대상으로 항생제는 수산용으로 판매량이 높은 옥솔린산과 플로르페니콜을 선정하였으며, 오존 공정을 이용하여 항생제의 제거를 평가하였다. 해수는 다양한 이온과 미네랄을 포함하고 있어 담수 오존 공정과 다른 산화 메커니즘을 갖는다. 해수 오존 공정에서 오존은 수체에 있는 브롬이온과 빠르게 반응하여 브로민을 생성하며, 생성된 브로민과 잔류 오존이 주요 산화제 역할을 한다. 선정한 항생제와 산화제의 고유 반응속도상수를 결정하기 위해 pH별 겉보기반응속도 상수를 구하였으며, 실제 해수 조건과 유사한 인공 해수에서 항생제 제거가 평가되었다. 플로르페니콜은 오존과 브로민과의 반응속도 상수가 낮은 반면 옥솔린산은 오존과 브로민과의 반응속도 상수가 높았다. 해수 오존 공정이 옥솔린산 제거에 효과적이었으나 플로르페니콜 제거에는 적합하지 않은 것으로 확인되었다.
우리나라의 해양 용존유기물질의 특성을 평가하기 위해 동해, 서해, 남해에서 분기별로 해수 시료를 채취하였다. 해수 시료에서 추출한 용존유기물질의 특성을 액체크로마토그래피-유기탄소 검출기와 형광 분광기를 이용하여 분석하였으며, Fluorescence excitation-emission matric 분석과 Parallel factor analysis 모델링을 통해 해양 용존유기물질의 구성 요소들을 통계학적으로 구분하였다. 해양 용존유기물질의 구성 요소들을 온라인 라이브러리인 OpenFluor를 이용하여 세계 환경의 유기물질과 비교 평가하였으며, 해역별로 해양 용존유기물질의 특성의 차이점이 확인되었다. 또한, 해수 오존 공정에서 산화제를 소모하는 요소를 밝혀냈으며, 산화제 소모 요소의 비율은 지역에 따라 다르기 때문에 해양 용존유기물질의 특성 분석이 선행되어야 함을 제안하였다.
세계 생산량의 87%를 차지하고 있는 폴리머 6종을 선정하였으며, 오존 공정에서 미세플라스틱 표준물질의 노화를 평가하였다. 세계적으로 미세플라스틱 분석 방법이 정립되어 있지 않아 전계방사형 주사전자현미경, 적외선 분광기, X선 광전자분광기, 접촉각 분석기와 같은 다양한 분석 기기를 활용하여 미세플라스틱의 물리 화학적 특성 변화를 확인하였다. 오존 공정에서 미세플라스틱의 표면은 산화되어 균열이 생성되었으며, carbonyl index와 X선 광전자분광기 분석 결과를 통해 미세플라스틱에 산소 작용기가 붙은 것을 확인하였다. 또한, 미세플라스틱의 Contact angle 수치 증가를 통해 오존 공정에서 미세플라스틱의 친수성이 증가한 것을 확인하였다. 산화로 인해 날카롭게 변한 미세플라스틱의 표면과 미세플라스틱의 친수화로 인한 중금속 흡착 가능성 증가는 노화된 미세플라스틱이 수생태계에 치명적인 영향을 미칠 수 있음을 시사한다.
본 연구는 오존 기반 산화처리에서 항생제의 제거, 해양 용존유기물질의 영향, 미세플라스틱의 노화에 대해 평가하였다. 항생제를 제거하기 위해 오존 공정이 적합한지 확인하였으며, 오존 공정에서 해양 용존유기물질이 미치는 영향을 평가하였고, 오존 공정에서 미세플라스틱의 노화를 평가하여 노화된 미세플라스틱이 초래할 수 있는 환경적인 영향에 대해 다루었다. 이러한 연구를 통하여, 항생제, 해양 용존유기물질, 미세플라스틱이 포함된 수계에 오존 공정을 적용 시 보다 안전하고 효율적인 운전이 가능할 것으로 기대된다.

다국어 초록 (Multilingual Abstract)

Water pollution is the addition of substances or energy forms negatively impacting a water body, usually due to human activities. With the development of pollutant detection technology, the number of pollutants detected in the water system has increased along with the importance of water treatment. In this dissertation, antibiotics, marine dissolved organic matter, and microplastics, which are in great need of research, were selected from among the substances that are problematic in aquatic systems. The removal of antibiotics in ozone-based oxidation treatment, the effect of marine dissolved organic matter, and the aging of microplastics were evaluated.
As antibiotics for the study, oxolinic acid and florfenicol, which have high sales for fishery products, were selected, and the removal of these antibiotics via the ozone process was evaluated. Seawater contains various ions and minerals; thus, it has a different oxidation mechanism from that of the freshwater ozone process. In the seawater ozone process, ozone rapidly reacts with bromide ions in the water matrix to produce bromine, and bromine and residual ozone act as the main oxidants. To determine the species-specific rate constants for the reaction of the selected antibiotics with the oxidants, the apparent rate constant for each pH was obtained, and antibiotic removal was evaluated in artificial seawater similar to actual seawater conditions. Florfenicol had a low rate constant with ozone and bromine, whereas oxolinic acid had a high rate constant with ozone and bromine. It was found that the seawater ozone process was effective in removing oxolinic acid but was not suitable for removing florfenicol.
Seawater samples were collected quarterly from the East Sea, Yellow Sea, and South Sea to evaluate the characteristics of marine dissolved organic matter in the Republic of Korea. The characteristics of dissolved organic matter extracted from seawater samples were analyzed using a liquid chromatography-organic carbon detector and fluorescence spectroscopy. The components of marine dissolved organic matter were statistically classified through fluorescence excitation-emission matrix analysis and parallel factor analysis modeling. The components of marine dissolved organic matter were compared and evaluated with organic matter in the global environment using OpenFluor, an online library, and the differences in the characteristics of dissolved organic matter in each sea area were identified. In addition, Component 1, which consumes oxidants in the seawater ozone process, was identified. Since the ratio of oxidant-consuming components differs depending on the region, it is suggested that the analysis of the characteristics of marine dissolved organic matter should precede the oxidation treatment.
Six polymers, which account for 87% of the global polymer production, were selected, and the aging of microplastics in the ozone process was evaluated. Because microplastic analysis methods have not been internationally established, several analytical method and instruments such as a field-emission scanning electron microscope/energy dispersive spectrometer, Fourier-transform infrared spectroscopy, X-ray photoelectron spectroscopy, and a contact angle analyzer were used to confirm the changes in the physicochemical properties of the microplastics. In the ozone process, the surfaces of the microplastics were oxidized, cracks were formed, and the carbonyl index and X-ray photoelectron spectroscopy analysis results confirmed that oxygen functional groups were attached to the microplastics. In addition, it was confirmed that the hydrophilicity of the microplastics increased in the ozone process through the increase in the contact angle of the microplastics. The sharpened surface of the microplastics due to oxidation and the increased possibility of adsorption of heavy metals due to the hydrophilization of the microplastics suggest that aged microplastics could have a fatal effect on aquatic ecosystems.
This dissertation confirms the suitability of the seawater ozone process to remove antibiotics, evaluates the effect of marine dissolved organic matter, and assesses the aging of microplastics that can cause environmental implications. These results can be used to apply ozonation in a water matrix that includes antibiotics, marine dissolved organic matter, and microplastics.

목차 (Table of Contents)

• CONTENTS
• CONTENTS ---------------------------------------------------------------------------------- i
• LIST OF TABLES ---------------------------------------------------------------------------------- iv
• LIST OF FIGURES -------------------------------------------------------------------------------- vi
• ABSTRACT ------------------------------------------------------------------------------------------- xi
• CHAPTER 1. Introduction --------------------------------------------------------------------------- 1
• 1-1. Issues of pollutants in water matrices -------------------------------------------------------- 1
• 1-2. Research objectives ---------------------------------------------------------------------------- 4
• CHAPTER 2. Literature review -------------------------------------------------------------------- 5
• 2-1. Antibiotics -------------------------------------------------------------------------------------- 5
• 2-2. Natural organic matters --------------------------------------------------------------------- 7
• 2-3. Microplastics ---------------------------------------------------------------------------------- 9
• 2-4. Ozone based oxidation treatment ---------------------------------------------------------- 13
• CHAPTER 3. [Antibiotics] Antibiotics oxidation using ozonation in seawater---------- 16
• 3-1. Introduction ------------------------------------------------------------------------------------- 16
• 3-2. Materials and methods ------------------------------------------------------------------------ 19
• 3-2-1. Materials ----------------------------------------------------------------------------------- 19
• 3-2-2. Experimental procedure ----------------------------------------------------------------- 21
• 3-2-3. Removal of antibiotics from bromide containing water ------------------------ 24
• 3-2-4. Analytical method ------------------------------------------------------------------------ 25
• 3-3. Results and discussion ------------------------------------------------------------------------ 26
• 3-3-1. Determination of ozone rate constants for the selected antibiotics ------------ 26
• 3-3-2. Determination of bromine rate constants for the selected antibiotics ------------- 31
• 3-3-3. Prediction of antibiotics removal efficiency in synthetic water -------------- 37
• 3-3-4. Removal of FF and OA by ozonation in water containing Br− -------------- 46
• 3-3-5. Reference-based potential by-products of antibiotics in ozonation -------------- 49
• 3-4. Conclusion ------------------------------------------------------------------------------------- 57
• CHAPTER 4. [Natural organic matters] Effect of marine dissolved organic matter in seawater ozonation -------------------------------------------------------------------------------- 58
• 4-1. Introduction ------------------------------------------------------------------------------------- 58
• 4-2. Materials and methods ------------------------------------------------------------------------ 62
• 4-2-1. Sampling strategy ----------------------------------------------------------------------- 62
• 4-2-2. Preparation of artificial seawater ----------------------------------------------------- 64
• 4-2-3. Oxidation experiment ------------------------------------------------------------------ 65
• 4-2-4. Analytical methods ---------------------------------------------------------------------- 66
• 4-3. Results and discussion ------------------------------------------------------------------------ 68
• 4-3-1. Seawater characteristics -------------------------------------------------------------- 68
• 4-3-2. Marine DOM modeling ------------------------------------------------------------- 74
• 4-3-3. Effect of the marine DOM on ozonation ----------------------------------------- 80
• 4-4. Conclusion ------------------------------------------------------------------------------------- 90
• CHAPTER 5. [Microplastics] Evaluation of oxidation treatment of microplastics in water matrices ---------------------------------------------------------------------------------------- 92
• 5-1. Introduction ------------------------------------------------------------------------------------- 92
• 5-2. Materials and methods ------------------------------------------------------------------------ 94
• 5-2-1. Selected polymers ---------------------------------------------------------------------- 94
• 5-2-2. Experimental procedure ---------------------------------------------------------------- 96
• 5-2-3. Characterization of microplastics ----------------------------------------------------- 97
• 5-3. Results and discussion ------------------------------------------------------------------------ 98
• 5-3-1. Microplastic surface changes in oxidation treatment ------------------------------- 98
• 5-3-2. Effect of alteration properties of microplastics in oxidation treatment -------- 103
• 5-3-3. Environmental implications ---------------------------------------------------------- 120
• 5-4. Conclusion ----------------------------------------------------------------------------------- 122
• CHAPTER 6. Conclusions ------------------------------------------------------------------------ 123
• 6-1. Antibiotics ------------------------------------------------------------------------------------ 123
• 6-2. Marine dissolved organic matters --------------------------------------------------------- 124
• 6-3. Microplastics -------------------------------------------------------------------------------- 124
• REFERENCES -------------------------------------------------------------------------------------- 126
• ABSTRACT (in Korean) -------------------------------------------------------------------------- 149

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