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논문 기본 정보

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학위논문
저자정보

김무늬 (가톨릭관동대학교, 가톨릭관동대학교 대학원)

지도교수
이승목
발행연도
2017
저작권
가톨릭관동대학교 논문은 저작권에 의해 보호받습니다.

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A simple cyclic voltammetry(CV) analytical method with organo-modified sericite for the working electrode was investigated to detect As(III) in an aquatic environment and optimal conditions for the reliable measurement of trace amounts of As(III) were studied. A distinct, specific peak was clearly observed at 0.8 V due to the reduction of H3AsO4 to H3AsO3. The specific peak current of arsenic increased with increasing the concentration of As(III) and initially increased proportionally to the scan rates. However, it disappeared as the scan rate increased over 400 mV/s. Because the surface of the organo-modified sericite electrode rapidly became saturated with As(III) when the deposition time increased, an optimal deposition time was determined as 60 s. Pb2+had no significant influence on the peak signal of As(III), whereas it was reduced as the ratio of Cu/As increased. Considering the detection limit of arsenic (1 ppb), this system can be used to detect low levels of As(III) in water systems.

목차

. 서론 1
Ⅱ. 이론적 배경 5
Ⅲ. 연구방법 22
3.1. 연구재료 22
3. 1. 1. 견운모 22
3. 1. 2. Organo-sericite 제조 24
3. 2. 연구방법 26
3. 2. 1. As(III) 흡착 실험 26
3. 2. 2. Cyclic voltammetry(CV) settings 26
3. 2. 3. Cyclic voltammetry(CV) 측정 조건 28
3. 2. 4. Working Electrode(유기탄소전극) 29
3. 2. 5. Cyclic Voltammetry를 이용한 As(III) 측정 실험 30
1) Gamry사, Teflon Tube 30
① CPE, MCPE 비교 30
② Scan rate 영향 30
③ pH 영향 30
④ As(III) 농도별 분석 31
2) (주)카이넬 KY01, PEEK 32
① Teflon Tube, PEEk 비교 32
② Sericite의 입자 크기에 따른 CV 측정 32
③ Nujol 오일 함유량에 따른 CV 측정 32
④ 유기견운모 함유량에 따른 CV 측정 32
⑤ PEEK size 32
⑥ pH 영향 33
⑦ Scan rate에 의한 영향 34
⑧ As(III) 농도에 의한 영향 34
⑨ 침지시간에 따른 영향 34
⑩ solution volume 영향 34
⑪ 수온에 따른 영향 35
⑫ 간섭물질의 영향 35
3) (주)카이넬 PAA, PEEK 36
① 해외 현장(베트남 호치민) 샘플 채취 및 분석 36
② 국내 현장(폐광산) 샘플 채취 및 분석 37
4) 재현성 Test 39
Ⅳ. 결과 및 고찰 40
4. 1. Organo-sericite의 특성 40
4. 1. 1. SEM 40
4. 1. 2. XRD 41
4. 1. 3. FT-IR 42
4. 2. As(III) 흡착실험 43
4. 3. Cyclic Voltammetry를 이용한 As(III) 측정 실험 45
1) Gamry사, Teflon Tube 45
① CPE, MCPE 비교 45
② Scan rate 영향 46
③ pH 영향 47
④ As 농도별 분석 49
2) (주)카이넬 KY01, PEEK 51
① Teflon Tube, PEEk 비교 51
② Sericite의 입자 크기에 따른 CV 측정 52
③ Nujol 오일 함유량에 따른 CV 측정 54
④ 유기견운모 함유량에 따른 CV 측정 55
⑤ PEEK size 56
⑥ pH 영향 57
⑦ Scan rate에 의한 영향 58
⑧ As(III) 농도에 의한 영향(PEEK working electrode) 59
⑨ 침지시간에 따른 영향 61
⑩ Solution volume 영향 62
⑪ 수온에 따른 영향 63
⑫ 간섭물질의 영향 64
3) (주)카이넬 PAA, PEEK 68
① 해외 현장(베트남 호치민) 샘플 분석 68
② 국내 현장(폐광산) 샘플 채취 및 분석 70
4) 재현성 Test 72
Ⅴ. 결론 74
Ⅵ. 참고문헌 77
국문초록 82
영문초록 84
감사의 글 86
그 림 목 차
Fig. 1. Cells and circuits for electrochemical measurements(a) 2 electrode cell (b) 3 electrode cell 13
Fig. 2. Cyclic Voltammetry 15
Fig. 3. (a) Form of potential scanning in cyclic voltammetry, (b) current curve of cyclic voltammetry 17
Fig. 4. (a) CV curve of a typical reversible system with CV scan rate, (b) Irreversible CV curve 19
Fig. 5. Anodic Stripping Voltammetry 20
Fig. 6. Schematic diagram of sericite 22
Fig. 7. Schematic diagram of organo-sericite mechanism 25
Fig. 8. Preparation of HDTMA-sericite 25
Fig. 9. Image of instrument (a)Gamry (b)KY01 (c) PAA 27
Fig. 10. A schematic diagram of the three electrode system 28
Fig. 11. Electrode (a)reference (b)working (c)auxiliary/counter 28
Fig. 12. Preparation of working electrode 29
Fig. 13. Sectional view of PEEK working electrode 33
Fig. 14. Solution volume 34
Fig. 15. Place of sampling in Vietnam 37
Fig. 16. Place of sampling in Ganwondo 38
Fig. 17. SEM of (a)sericite, (b)HDTMAsericite 40
Fig. 18. XRD analyses of sericite and organo-sericite 41
Fig. 19. FT-IR analyses of sericite and organo-sericite 42
Fig. 20. Removal of As(III) using sericite and organo-sericite 43
Fig. 21. As(III) for the redox reaction analysis of cv 44
Fig. 22. CV curve obtained for As(Ⅲ) using the CPE and MCPE 45
Fig. 23. Effect of scan rate on the redox behavior of As(III) using MCPE 46
Fig. 24 Effect of pH on anodic current in the oxidation of arsenic using HDTMA-Sericite modified carbon paste electrode 47
Fig. 25. Mechanism of Adsorption As(III) 48
Fig. 26. Effect of concentration in the redox behavior of As(III) using HDTMA-Sericite modified carbon paste electrode 50
Fig. 27. Effect of different kinds of case material for working electrode on the peak current 51
Fig. 28. Effect of sericite size on the peak current(A:11 μm, B: 20 μm, C:40 μm) 53
Fig. 29. Effect of oil ratio on the peak current of As(III) 54
Fig. 30. Effect of organo sericite ratio on the peak current of As(III) 55
Fig. 31. Effect of electrode housing size on the current of As(III) 56
Fig. 32. Effect of pH on cathodic current in the reduction of arsenic using MCPE 57
Fig. 33. Effect of scan rate on the peak current of As(III) 58
Fig. 34. Effect of As(III) concentration on the peak current 59
Fig. 35. Linear relationship between the peak current and As(III) concentration 61
Fig. 36. Effect of deposition time on the current of As(III) 61
Fig. 37. Effect of solution volume on the current of As(III) 62
Fig. 38. Effect of temperature on the peak current of As(III) 63
Fig. 39. Effect of Pb on the peak current of As(III) 65
Fig. 40. Effect of Cu on the peak current of As(III) 65
Fig. 41. Effect of Fe on the peak current of As(III) 66
Fig. 42. Effect of the (a) Mn (b) Zn peak current 67
Fig. 43. Linear relationship between ICP and PA water in vietnam 69
Fig. 44. Linear relationship between ICP and PA water in Korea 71
Fig. 45. Reproducibility test of arsenic 10 ppb 72
Fig. 46. Reproducibility test of arsenic 100 ppb 73
표 목 차
Table 1. Classification of electrochemical measurement(analysis) 10
Table 2. Chemical composition of sericite 23
Table 3. Different four type of working electrode(PEEK) 33
Table 4. 베트남 현지 지하수 성분 분석(ICP) 68
Table 5. 베트남 현지 지하수 분석 69
Table 6. 폐광산 하천수 성분분석(ICP) 70
Table 7. 폐광산 하천수 As 분석 70
Table 8. 10 ppb 비소 용액을 이용한 재현성 Test 72
Table 9. 100 ppb 비소 용액을 이용한 재현성 Test 73

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