Research Agendas
질량분석법을 이용한 다항목 동시분석법 표준화에 관한 연구(3차년도)
Director
Period
2007.01.01 ~2009.12.31
Performer
오은정,김정희,최재원,이규철,김윤석
File
Main works of the 3dr yesrs project were divided into 3 parts.
First, validation study for the suggested methods for nitrosamines and persistent organic pollutants(POPs) by the international cooperative researches in 2007~2008. CI method for the simultaneous measurement of 9 nitrosamines was suggested by Orange County Water District. There were no differences in MDL just for NDMA by the both ionization methods up to 0.5 ng/L. However, CI method showed improved MDL ranges for 34~69% than those by EI methods. In future, CI methods should be applied in multi-residue monitoring for treated water. Multi-residue method was combined using large volume field sampler by Kwater and sample cleanup and GC-HRMS methods by NIAES. By this method, monitoring for both PCDD/Fs and POPs are available. Reliable recovery rates and relative TEQs with 134% to the conventional method was obtained. HCB and DDE were widely detected from raw water samples from 6 DWTP with now ng/L ranges. POPs compounds should be surveyed widely from next year including treated water to validated the removal rates.
Second, international collaborative researches for the 2nd year were completed with great success. Participants and main topics were as following ; 17 organophosphours pesticides using GC-MS/MS and GC-HRMS by Water Analysis & Research Center, K water; polychlorinated Naphthalenes and Polychlorinated Paraffins by GC-MS and GC-HRMS by NIER (Korea); 67 human pharmaceuticals from Waste water treatments by TZW (Germany); 10 metabolites of organophosphorous pesticides by NIAES (Japan); improvement of Quality Control and Quality Assurances of Unregulated Contaminants Monitoring Rule II by OCWD (USA). Reports written by English version covers for 7 chapters. Each parts of reports details about validated analytical procedures for emerging contaminants up to 138 lists.
Third, multi residue method for most potent brominated flame retardants PBDE(Polybrominated Diphenyl Ethers) was developed by SPE-GC-HRMS. This method covers more congeners up to 27 lists for mono~decaBDE than those by EPA method 1614 often found in environmental metrices including surface water. Averaged slope of calibration curves were >0.999 with low MDL belows 1ng/L. This method will be applied surface water survey in 2010, particularly for the four big river project.
제 출 문 i
연구개발결과 활용보고서 ii
요 약 문 vi
<제목 차례> xxi
<표 차례> xxiii
<그림 차례> xxv
제 1 장 수질오염물질 확대와 동시분석의 배경 1
1.1 연구배경 1
1.1.1 수질오염물질의 기존 분석체계와 동시분석의 필요성 1
1.1.2 국내·외 신규물질의 수질동향 2
1.1.3 국내·외 동시분석 기술현황 2
1.1.4 국제 공동연구 추진 현황 3
1.2 연구 목표 및 주요 내용 5
1.2.1 연구의 목표 5
1.2.2 연구의 주요 내용 5
제 2장 동시분석 기술개발 내용 및 방법 6
2.1 다항목 동시분석 체계 6
2.2 첨단 장비를 활용한 고감도 동시분석 체계 6
제 3 장 연구 결과 10
3.1 국제공동연구 1차년도 제안 방법의 자체검증 10
3.1.1 미국제안) 나이트로사민류 소독부산물의 이온화 방법에 따른 검출한계 개선 10
3.1.2 일본제안) 대용량 포집장치를 적용한 POPs 동시분석방법 검토 및 실태조사 15
3.1.3 잔류성 유기오염물질의 분석방법 최적화 및 분석지침서 제작 20
3.2 국제공동연구 2차년도 수행 및 영문보고서 작성 41
3.2.1 유기인계 농약류 동시분석법 정립 (수돗물분석연구센터) 41
3.2.2 유기인계 농약 대사물질 동시분석법 정립 (일본농업환경기술원) 50
3.2.3 염화나프탈렌 및 염화파라핀 동시분석법 정립 (국립환경과학원) 54
3.2.4 하수처리장 시료의 의약물질 동시분석법 정립 (독일수도기술원) 58
3.2.5 분석법 비교를 통한 정도관리 개선 (미국 오렌지카운티수도국) 61
3.2.6 영문보고서 작성 63
3.3 신규오염물질의 동시분석법 정립 : 67
3.3.1 분석원리 및 분석대상물질 67
3.3.2 표준물질 및 시약 68
3.3.3 기기 및 장치 70
3.3.4 시험방법 71
3.3.5 시험결과 : 항목별 크로마토그램 및 스펙트럼 78
3.3.6 검량곡선 81
3.3.7 검출한계 및 회수율 84
3.3.8 요 약 86
제 4 장 결 론 87
참 고 문 헌 89
서 지 자 료 96
First, validation study for the suggested methods for nitrosamines and persistent organic pollutants(POPs) by the international cooperative researches in 2007~2008. CI method for the simultaneous measurement of 9 nitrosamines was suggested by Orange County Water District. There were no differences in MDL just for NDMA by the both ionization methods up to 0.5 ng/L. However, CI method showed improved MDL ranges for 34~69% than those by EI methods. In future, CI methods should be applied in multi-residue monitoring for treated water. Multi-residue method was combined using large volume field sampler by Kwater and sample cleanup and GC-HRMS methods by NIAES. By this method, monitoring for both PCDD/Fs and POPs are available. Reliable recovery rates and relative TEQs with 134% to the conventional method was obtained. HCB and DDE were widely detected from raw water samples from 6 DWTP with now ng/L ranges. POPs compounds should be surveyed widely from next year including treated water to validated the removal rates.
Second, international collaborative researches for the 2nd year were completed with great success. Participants and main topics were as following ; 17 organophosphours pesticides using GC-MS/MS and GC-HRMS by Water Analysis & Research Center, K water; polychlorinated Naphthalenes and Polychlorinated Paraffins by GC-MS and GC-HRMS by NIER (Korea); 67 human pharmaceuticals from Waste water treatments by TZW (Germany); 10 metabolites of organophosphorous pesticides by NIAES (Japan); improvement of Quality Control and Quality Assurances of Unregulated Contaminants Monitoring Rule II by OCWD (USA). Reports written by English version covers for 7 chapters. Each parts of reports details about validated analytical procedures for emerging contaminants up to 138 lists.
Third, multi residue method for most potent brominated flame retardants PBDE(Polybrominated Diphenyl Ethers) was developed by SPE-GC-HRMS. This method covers more congeners up to 27 lists for mono~decaBDE than those by EPA method 1614 often found in environmental metrices including surface water. Averaged slope of calibration curves were >0.999 with low MDL belows 1ng/L. This method will be applied surface water survey in 2010, particularly for the four big river project.
제 출 문 i
연구개발결과 활용보고서 ii
요 약 문 vi
<제목 차례> xxi
<표 차례> xxiii
<그림 차례> xxv
제 1 장 수질오염물질 확대와 동시분석의 배경 1
1.1 연구배경 1
1.1.1 수질오염물질의 기존 분석체계와 동시분석의 필요성 1
1.1.2 국내·외 신규물질의 수질동향 2
1.1.3 국내·외 동시분석 기술현황 2
1.1.4 국제 공동연구 추진 현황 3
1.2 연구 목표 및 주요 내용 5
1.2.1 연구의 목표 5
1.2.2 연구의 주요 내용 5
제 2장 동시분석 기술개발 내용 및 방법 6
2.1 다항목 동시분석 체계 6
2.2 첨단 장비를 활용한 고감도 동시분석 체계 6
제 3 장 연구 결과 10
3.1 국제공동연구 1차년도 제안 방법의 자체검증 10
3.1.1 미국제안) 나이트로사민류 소독부산물의 이온화 방법에 따른 검출한계 개선 10
3.1.2 일본제안) 대용량 포집장치를 적용한 POPs 동시분석방법 검토 및 실태조사 15
3.1.3 잔류성 유기오염물질의 분석방법 최적화 및 분석지침서 제작 20
3.2 국제공동연구 2차년도 수행 및 영문보고서 작성 41
3.2.1 유기인계 농약류 동시분석법 정립 (수돗물분석연구센터) 41
3.2.2 유기인계 농약 대사물질 동시분석법 정립 (일본농업환경기술원) 50
3.2.3 염화나프탈렌 및 염화파라핀 동시분석법 정립 (국립환경과학원) 54
3.2.4 하수처리장 시료의 의약물질 동시분석법 정립 (독일수도기술원) 58
3.2.5 분석법 비교를 통한 정도관리 개선 (미국 오렌지카운티수도국) 61
3.2.6 영문보고서 작성 63
3.3 신규오염물질의 동시분석법 정립 : 67
3.3.1 분석원리 및 분석대상물질 67
3.3.2 표준물질 및 시약 68
3.3.3 기기 및 장치 70
3.3.4 시험방법 71
3.3.5 시험결과 : 항목별 크로마토그램 및 스펙트럼 78
3.3.6 검량곡선 81
3.3.7 검출한계 및 회수율 84
3.3.8 요 약 86
제 4 장 결 론 87
참 고 문 헌 89
서 지 자 료 96