The Swedish EPA (Naturv&#229;rdsverket) (agreement 2208-13-001) and Centre for Chemical Pesticides (CKB) are gratefully acknowledged for funding this project. We thank M&#228;rit Peterson, Henrik Jernstedt, Emma Gurnell and Elin Paulsson at the OMK-lab, SLU, for skillful assistance with analytical support and supply of pesticide standards.

1. 패시브 샘플러 설계 및 제조 <ol><li> 실리콘 고무 시트 <ol><li> (3.2 mm × 10 mm를 스테인리스 절단기를 사용하여 스테인리스 블라인드 리벳을 사용하여 연결 × 600 mm 2.5 mm 2.5 mm X 314mm의 줄무늬로 실리콘 고무 시트를 절단 부 (600 mm × 600 mm, 0.5 mm 두께) ) × 914mm 2.5 mm (면적 = 457cm 2 흡착제 집합체 = 15.6 g, 총 부피 샘플러 스트라이프 크기를 얻기 위해 리벳과 총 = 22.9 cm 3). </li></ol></li><li> 속 슬렛 장치의 추출 실에서 실리콘 고무를 놓습니다. 추출 실에 50 ㎖의 EA를 추가하고 250 ML의 EA와 500ml의 둥근 병 플라스크에 세 끓는 돌을 추가합니다. <ol><li> 병 플라스크 및 냉각기를 추출 챔버를 연결한다. 약 80 ° C에서 96 시간 동안 속 슬렛 추출하여 실리콘 고무를 청소하고 부드러운 질소 가스 하에서 그 후 그들을 건조. </li></ol></li><li> 실리콘 고무 스트를 부착홀더 (도 1)의로드 주위에 실리콘 고무를 배치하여 스트라이프 스테인리스 거미 샘플 홀더 퍼가기. 케이블 타이를 이용하여 홀더에로드에 실리콘 고무 스트라이프의 각 끝을 연결합니다. </li></ol><img alt="그림 1" src="/files/ftp_upload/54053/54053fig1.jpg" /> 실리콘 고무의 그림 1. 도식. 상단과 B) 측면보기에서 스테인리스 거미 샘플 홀더 (A)에 실리콘 고무 스트라이프의 부착)를 도시 실리콘 고무에 대한 패시브 샘플러 개략적 인. <a href="https://www.jove.com/files/ftp_upload/54053/54053fig1large.jpg" target="_blank">의 더 큰 버전을 보려면 여기를 클릭하십시오 이 그림.</a> <ol start="2"><li> POCIS-A 및 POCIS-B <ol><li> POCIS-A의 경우, 9.0 cm squar에 의해이 9.0 cm 사이 HLB 벌크 흡수제 (표면적 = 1.78 × 106 cm 2)의 220 mg의 배치전자 폴리 에테르 설폰 (PES) 멤브레인 (그림 2). </li><li> POCIS-B의 경우, 흡착제 혼합물을 220 mg의 배치 (즉, 하이드 록 실화 폴리스티렌 - 디 비닐 벤젠 수지 (80 %) 및 스티렌 - 디 비닐 벤젠 공중 합체에 분산 된 탄소 흡착제 (20 %)) (면적 = 2.82 × 106 cm2로) 둘 사이의 PES 멤브레인 (그림 2). </li><li> 흡착제 수동 개의 스테인레스 스틸 링 사이 개의 PES (내부 Ø = 5.4 cm)를 압축하여 스테인리스 샘플 홀더 (도 2)에 고정. </li></ol></li></ol><img alt="그림 2" src="/files/ftp_upload/54053/54053fig2.jpg" /> 패시브 샘플러 디스크 그림 2. 회로도. POCIS A에 대한 패시브 샘플러 설계도, B, SDB-RPS 디스크와 스테인레스 스틸 링, 폴리 에테르 설폰 사용) 패시브 샘플러의 조립을을 보여주는 C (18) 디스크 (PES) membran을 POCISES 및 수신 단계, 및 B) 스테인레스 스틸 샘플 홀더에 조립. <a href="https://www.jove.com/files/ftp_upload/54053/54053fig2large.jpg" target="_blank">이 그림의 더 큰 버전을 보려면 여기를 클릭하십시오.</a> <ol start="3"><li> SDB-RPS 디스크와 C (18) 디스크 <ol><li> SDB-RPS (면적 = 35cm 2, 흡착제의 질량 = 0.34 g, 볼륨 = 3 1.7 cm)와 C (18) 디스크 (표면적 = 35cm 2, 흡착제의 질량 = 0.58 g, 부피 = 1.7 cm 3) 사이에 배치 이 PES 멤브레인 (그림 2). 디스크 수동 개의 스테인레스 스틸 링 사이 개의 PES (내부 Ø = 5.4 cm)를 압축하여 스테인리스 샘플 홀더 (도 2)에 고정. </li></ol></li></ol> 2. 연구소 통풍 관 실험 참고 : 실험실 흡수 실험을 정량적으로 흡수 K의 특성을 실시 하였다통제 된 조건에서 다섯 가지 패시브 샘플러 장치에 대한 124 개별 농약에 대한 inetics. <ol><li> (N = 16) (N = 16), POCIS-B 탱크 1) 실리콘 고무 (N = 16)가 탱크 (2)) POCIS-A 및 조 3 : 직사각형 유리 용기 흡수 연구 (각 ~ 95 L)을 실시 ) SDB-RPS 디스크 (N = 16), C (18) 디스크 (N = 16). 세 개의 탱크에 자연 물을 채 웁니다. </li><li> 일정한 수온 (~ 20 ° C)에서 각면의 벽에 부착 된 두 개의 전기 펌프를 사용하여 난류 물 상태 (~ 10cm의 초 -1)에서 모든 실험을 수행합니다. 광분해 효과를 최소화하기 위해 암에 실험을 수행한다. </li><li> 유리 주사기를 사용하여 124 농약을 포함하는 농약 표준 혼합물로 각 유리 용기 스파이크 (c 400 NG의 L ≈ -1 수조 개별 살충제의 경우). 시간 간격의 5에서 탱크에서 수동으로 11, 20, 26 d의 패시브 샘플러를 꺼내AYS는 농약의 샘플링 속도를 결정합니다. </li><li> 다른 21 바와 같이 물 샘플의 분석 일 0, 5, 11, 20에서 100 ㎖의 물 샘플을 수집하여, 각 탱크 내의 농약의 농도를 모니터링하고, (26)이 수행된다. <ol><li> 품질 관리, 일 0에서 1 시간 동안 실내 공기에 빈 샘플을 노출하고 저장하고 실제 샘플로 취급합니다. 모든 추출물뿐만 아니라 추가 분석 할 때까지 -18 ℃에서 탱크에서 수집 된 100 ml의 물 샘플을 저장합니다. </li></ol></li></ol> 3. 샘플 추출 <ol><li> 실리콘 고무 <ol><li> 추출에 앞서, 고순도 질소 기류 하에서 실리콘 고무 스트라이프 건조. </li><li> 가스 크로마토 그래피 질량 분석 (GC-MS) 분석을 위해, 속 슬레 추출 (22)을 사용하여 고체 - 액체 추출을 수행한다. <ol><li> 속 슬레 추출기에 실리콘 고무를 놓습니다. 250 ml의 PE / ACE를 추가 (50/50, v / v)의 3 BOI둥근 병 플라스크에 넣고 링 돌입니다. </li><li> 100 ㎕로 실리콘 고무 스파이크 것은 유리 주사기를 사용하여 혼합물 (c = 5 ml의 NG-1)이다. 속 슬레 추출기에 50 ml의 PE / ACE를 (50/50, v / v)로 추가합니다. 히터에 전환하고 19 시간 동안 속 슬레 추출을 실행 한 후 히터를 끄고. </li><li> 1 ml의에 부드러운 질소 블로우 다운 다음에 회전 증발에 의해 추출물을 집중한다. 1 ml의에 질소 블로우 다운 동안 세 번 1 ML의 CH / ACE (90/10를, v / v)의 추가 / ACE를 (90/10, v / v)의 CH하는 용매 교환한다. </li></ol></li><li> 액체 크로마토 그래피 탠덤 질량 분석법 (LC-MS / MS) 분석을 위해, 속 슬레 추출 (22)을 사용하여 추출을 수행한다. <ol><li> 속 슬레 추출기에 실리콘 고무를 놓습니다. 속 슬레 추출기에 250 ML의 메탄올과 둥근 병 플라스크에 넣고 3 끓는 돌과 50 ㎖의 메탄올을 추가합니다. 혼합물 (c = 5 ml의 NG-1) 유리 SYR를 사용하는 100 ㎕와 실리콘 고무 스파이크인게. </li><li> 히터에 전환하고 19 시간 동안 속 슬레 추출을 실행 한 후 히터를 끄고. 1 ml의에 부드러운 질소 블로우 다운 다음에 회전 증발에 의해 추출물을 집중한다. 1 ml의에 질소 블로우 다운 중 1 ml의 ACN을 추가하여 ACN에 용매를 교환한다. </li></ol></li></ol></li><li> POCIS-A 및 POCIS-B <ol><li> 주의 POCIS 샘플러를 열고이 폴리에틸렌 (PE) 프릿을 함유하는 예비 세정 빈 프로필렌 고체 상 추출 (SPE) 카트리지 (6 mL)에 깔때기를 사용하여 초순수로 흡착제를 옮긴다. 물을 제거하기 위해 진공 흡착제를 건조. 흡착재의 중량을 제어 할 비어 충전 SPE 카트리지의 중량을 기록한다. 다른 카트리지 GC-MS 및 LC-MS / MS 분석을 위해 사용되는주의하시기 바랍니다. </li><li> 용출에 앞서, 유리 주사기를 사용하여 100 ㎕로 흡착제를 혼합물 (c = 5 ml의 NG -1)는 스파이크. (5)을 사용하여 용출 POCIS-A 및 POCIS-B 흡착제GC-MS 22 ml의 EA. <ol><li> 부드러운 질소 블로우 다운에 의해 1 ml의에 추출물을 집중한다. 1 ml의에 질소 블로우 다운 동안 세 번 1 ML의 CH / ACE (90/10를, v / v)의 추가 / ACE를 (90/10, v / v)의 CH하는 용매 교환한다. </li></ol></li><li> 8 ml의 DCM / 메탄올 다음에 1.5 ml의 메탄올 사용하여 용출 POCIS-A 및 POCIS-B 카트리지 (20 분의 80을, v / v)의 LC-MS / MS 분석 22. 부드러운 질소 블로우 다운에 의해 1 ml의에 추출물을 집중한다. 1 ml의에 질소 블로우 다운 중 1 ml의 ACN을 추가하여 ACN에 용매를 교환한다. </li></ol></li><li> SDB-RPS와 C (18) 디스크 <ol><li> 유리 비커에 SDB-RPS와 C (18) 디스크의 개별 디스크를 전송하고 질소 가스에서 그들을 건조. 3 ㎖의 다음 10 분간 EA 5 ㎖ 먼저, 혼합물 (c = 5 NG ml의 -1) 유리 주사기를 사용하여, 실온에서 유리 비이커들을 두 번 초음파 처리 된 100 ㎕와 디스크 스파이크 및 10 분 동안 EA의. </li><li> 전송 보한 유리관에 제 추출물을 아래 부드러운 질소 블로우에 의해이 용액으로 농축하고 (GC-MS 및 LC-MS / MS 분석을 위해 각각)이 1 ml의 분획물로 분할. </li><li> 부드러운 질소 블로우 다운 0.5 ml의의 추출물을 농축 및 CH / ACE에 용매를 교환 (90/10, v / v)의 GC-MS 분석 22. 부드러운 질소 블로우 다운 0.5 ml의의 추출물을 농축 및 LC-MS / MS 분석 22 ACN에 용매를 교환한다. </li></ol></li></ol> 4. 물 샘플 <ol><li> , 혼합물을 유리 주사기를 사용하여 (c = 5 NG ml의 -1) 인 100 ㎕와 20 ml의 물 샘플 스파이크 3 분 동안 DCM 3 ㎖, 소용돌이를 추가하고, GC-MS 분석 (22) 상 분리기로 가만히 따르다. <ol><li> 두 상을 분리 한 후, 유리 튜브에 DCM 상 삼출액. 3 ml의 DCM을 사용하여 추출을 반복하고, 2 mL의 DCM으로 튜브를 헹군다. 마지막으로, 부드러운 질소 블로우 다운 및 exchan 0.5 ml의 추출물을 집중GE의 CH하는 용매 / ACE (90/10, v / v)로. </li></ol></li><li> LC-MS / MS (21)에 의해 다른 곳에 기재된 방법과 유사한 대량 주사를 이용한 물 샘플을 분석한다. </li></ol> 5. 기기 분석 <ol><li> GC-MS 분석 <ol><li> 전자 이온화 (EI)과 부정적인 화학 이온화 (NCI) 모드로, 각각 22 GC-MS 시스템을 사용하여 CH / ACE 추출물의 기기 분석을 수행합니다. </li><li> EI를 이용하여 GC-MS 법 들어, HP-5MS UI 열에 비분 주입법 1 μL (30m, 0.25 mm의 내경, 0.25 ㎛의 막)의 분취 액을 주입. </li><li> GC의-MS 방법을 사용하여 CI를 들어, HP-5MS UI 열 3 μL (30m, 0.25 mm 내경, 0.25 μm의 필름)의 분취 액을 주입. </li></ol></li><li> HPLC-MS / MS 분석 <ol><li> (-) ESI ()와 긍정적 인 이온 m ACN의 기기 분석을 수행하여 추출물 HPLC-MS / MS는 전기 분무 부정적인 이온화 소스와 인터페이스ODE ((+) ESI) 22. </li><li> ACN은 FA를 사용하여 pH를 5로 조정 한 900 μL의 초순수로 추출물을 (+) ESI 들어, 100 ㎕의 희석. </li><li> (-)의 경우 ESI 상기 ACN 100 ㎕ 초순수 1 % FA 900 ㎕의 용액으로 추출하여 묽은. </li><li> (+) ESI 들어, 0.3 ml의 분 -1의 유속 2- 프로판올 / 메탄올 / 10 mM의 암모늄 포르 메이트 (6/2/92, V / V / V) 및 메탄올로 이루어진 바이너리 구배를 사용한다. </li><li> (-) ESI 들어, 0.3 ml의 분 -1의 유속 ACN / 초순수 0.1 % HAC 및 ACN + 0.1 % HAC 이루어진 바이너리 구배를 사용한다. </li><li> 두 온라인 SPE 칼럼 (20 × 2mm ID 및 20 내지 25 ㎛의 입자 크기 모두), 및 분석 컬럼 (C (18), 100 × 3mm, 3.5 μm의) (21)를 사용하여 500 μL 대량 주사를 사용하여 모든 샘플을 주입한다. </li></ol></li></ol> 수동 샘플링 6. 이론 참고 : 패시브 샘플러 mediu에 화학 물질의 흡수 프로필직선, 곡선 및 평형 (그림 3) : m (PSM)의 세 부분으로 나누어 져 있습니다. <img alt="그림 3" src="/files/ftp_upload/54053/54053fig3.jpg" /> 3. 패시브 샘플러 흡수 곡선을 그림. A) 및 C) 흡수 절대 ng를에서 수동 샘플러 (N의 t) 각각 아세 타미 프리드 및 디 메토 에이트의 축적 된 양 곡선 및 B) 및 D) 겨 L 각각 아세 타미 프리드 및 디 메토 에이트, 물 탱크 농도 - 1. <a href="https://www.jove.com/files/ftp_upload/54053/54053fig3large.jpg" target="_blank">이 그림의 더 큰 버전을 보려면 여기를 클릭하십시오.</a> <ol><li> (노광 t 일 후 패시브 샘플러 N &#39;t를 표적 화합물의 축적량 나누어 패시브 샘플러 동등 물의 양 (V의 이퀄라이저 L)를 계산 </su() NG의 L-1, w 다 잡아와 시간 통합 활성 샘플링을 사용하여 수상의 농도에 의해 P&gt;, NG). <img alt="식 (1)" src="/files/ftp_upload/54053/54053eq1.jpg" /> (1) </li><li> 전개 시간 대 V의 당량의 기울기를 고려하여, 흡수 프로파일의 선형 흡수 단계에서, 샘플링 레이트 (R S, L 일 -1)를 도출. </li><li> K 개의 PW 식을 사용하여 개별 살충제 (-1 L의 kg)을 계산합니다. 2. <img alt="식 (2)" src="/files/ftp_upload/54053/54053eq2.jpg" /> (2) m P가 샘플러 당 흡착제 집합체이고 (ng를). </li><li> 선형 흡수 단계에서 (TWA, NG의 L-1 C) 식을 이용하여 패시브 샘플러에 의해 도출 된 물에서 분석 물의 TWA 농도를 계산한다. 삼. <img alt="식 (3)" src="/files/ftp_upload/54053/54053eq3.jpg" /> (삼) 여기서 R의 S는 sa입니다mpling 속도 (L 일 -1), t는 배포 시간 (일)입니다. </li><li> 곡선 형 위상 식을 사용 TWA c를 구한다. 4. <img alt="식 (4)" src="/files/ftp_upload/54053/54053eq4.jpg" /> (4) </li><li> 평형 단계에서는 수학 식을 이용 TWA c를 구한다. 5. <img alt="식 (5)" src="/files/ftp_upload/54053/54053eq5.jpg" /> (5) </li></ol> 7. 통계 데이터 분석 <ol><li> 샤피로-Wilk 검사 (23)를 사용하여 데이터의 비 정규 분포를 테스트합니다. 시험 농약의 물리 화학적 특성 (24) (-1에서 1 사이의 스피어의 RHO) 대 K PW 및 R S 비 파라 메트릭 스피어 만의 순위 상관 관계를 사용합니다. </li></ol>

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The authors have nothing to disclose.

품질 관리, 표준 절차, 실험실 공백으로 검출 (LOD), 복구 및 반복성의 한계 (23)을 조사 하였다. 몇 살충제 낮은 농도 수준에서 블랭크 샘플에​​서 검출되었다. LOD를는 평균 LOD를 실리콘 고무 POCIS-A 1.7 PG 절대 1.6 열 분사 8.0 PG 절대했다 (3)의 잡음 비율로 신호의 조건에 맞는 검정 곡선의 최저점의 값으로 설정된 페이지 POCIS-B, SDB-RPS 디스크 3.0 페이지 절대 및 C (18) 디스크 절대 1.6 페...

살충제는 지속적으로 수생 환경 소개 및 수생 생물 1에 위험을 초래할 수 있습니다. 수성 환경에서 농약의 모니터링은 전형적으로 흐름 또는 일시적인 입력 (예를 들면, 침전, 결합 하수 오버 플로우, 하수 라군 자료) (2)의 변동에 잡아 샘플링 그러나,이 샘플링 기술은 완전히 농도의 시간적 변화를 고려하지 않습니다 사용하여 수행됩니다 3. 따라서, 모니터링 방법은 살충제와 관련된 환경 위험의 더 나은 추정을 개선 할 필요가있다. 수동 샘플링은 최소한의 인프라와 낮은 오염 물질 농도 4,5와 오랜 기간에 걸쳐 지속적으로 모니터링 할 수 있습니다. 패시브 샘플러는 지하수 (6) 모니터링, 신선한 물 7-10, 폐수 (11)와 해수 (12)에 대한 유용한 도구가 될 것으로 나타났다. 모니터링 목적 외에 <sup&gt; 13, 14는 패시브 샘플러는 비 표적 분석 15 일 독성 시험 (16, 17)에 이용되어 있고, 대안으로서 sediment- 18을하는 생체 모니터링. 패시브 샘플러는 물에서 지속적으로 화학 물질을 축적 가중 평균 (TWA)이 14 농도의 시간을 제공합니다. 오염 물질의 흡수는 수동 샘플러 설계 샘플러 물질, 오염물의 물리 화학적 특성 및 환경 조건 (예를 들면, 물에 따라 샘플링 레이트 (R S)와 패시브 샘플러 - 물 분배 계수 (K PW)에 따라 난류, 온도) 13,14,19,20. 자세한 동영상은 교정과 물에 농약에 대한 패시브 샘플러를 적용하는 방법을 보여하는 것을 목표로하고있다. 구체적인 목적은 i)는 수동 SAMPL의 다섯 가지 유형을 사용하여 124 개별 농약에 대한 준비, 추출 및 기기 분석을 수행하기 위해 포함실리콘 고무를 포함, ERS, 극성 유기 화학 통합 샘플러 (POCIS) -A, POCIS-B, SDB-RPS와 C (18) 디스크, ⅱ) 실험실 흡수 연구에서 농약에 대한 R S와 K PW을 평가하고 ⅲ) 관심 방법과 각각의 패시브 샘플러에 대한 TWA 농도를 계산하는 대상 화합물의 적절한 패시브 샘플러를 선택하는 방법을 설명합니다. 참조 표준 및 패시브 샘플러 장치 표적 화합물 124 레거시 및 제초제, 살충제 및 살 진균제 (표 1)을 포함하여 현재 사용되는 살충제를 포함했다. 내부 표준 혼합물 (혼합물 IS) 페 노프 로프 (2,4,5-TP), clothianidin-D 3, ethion 및 terbuthylazine-D (5)를 포함. 기타 사용되는 화학 물질이 메탄올 (메탄올), 아세토 니트릴 (ACN), 아세톤 (ACE), 디클로로 메탄 (DCM), 시클로 헥산 (CH), 에틸 아세테이트 (EA)를 포함 석유 외그녀 (PE), 2- 프로판올, 25 % 암모니아수, 아세트산 (HAC) 및 포름산 (FA). 다섯 가지 수동 샘플링 장치는 실리콘 고무 POCIS-A 및 B-POCIS, SDB-RPS 및 C (18)의 디스크 1,21 포함한 것을 특징으로 하였다. 표 1. 패시브 샘플러 샘플링 속도 (R &#39;S, L 일 -1), 샘플러 - 물 분배 계수 (K&#39;PW, L kg -1)과 방정식 (식.) 개인에 대한 현장 시료 농도의 계산에 사용 살충제가. (엘스 비어의 허가, 물, 1-11, 저작권 (2015)에서 농약의 모니터링을위한 크로마토 그래피 (A)의 저널, 1405, 루츠 렌스, Atlasi Daneshvar, 안나 E. 라우, 제니 Kreuger, 오 수동 샘플링 장치의 특성에서 재판 .) (22) <a href="https://www.jove.com/files/ftp_upload/54053/Table_1.xlsx" target="_blank">이 파일을 다운로드하려면 여기를 클릭하십시오.</a>

<table><tbody><tr><td>Methanol</td><td>Merck Millipore</td><td>1.06035.2500</td><td></td></tr><tr><td>Acetonitrile</td><td>Merck Millipore</td><td>1.00029.2500&amp;nbsp;</td><td></td></tr><tr><td>Acetone</td><td>Merck Millipore</td><td>1.00012.2500</td><td></td></tr><tr><td>2-propanol</td><td>Merck Millipore</td><td>1.00272.2500</td><td></td></tr><tr><td>Dichloromethane</td><td>Merck Millipore</td><td>1.06054.2500</td><td></td></tr><tr><td>Ammoniak</td><td>Merck Millipore</td><td>1.05428.1000</td><td>Purity 25%</td></tr><tr><td>Formic acid</td><td>Sigma-Aldrich</td><td>94318-50ML-F</td><td>Purity ~98%</td></tr><tr><td>Ethyl acetate&amp;nbsp;</td><td>Sigma-Aldrich</td><td>31063-2.5L</td><td>for pesticide residue analysis</td></tr><tr><td>Petroleum ether&amp;nbsp;</td><td>Sigma-Aldrich</td><td>34491-4X2.5L</td><td>for pesticide residue analysis</td></tr><tr><td>Acetic acid&amp;nbsp;</td><td>Sigma-Aldrich</td><td>320099-500ML</td><td>Purity &amp;ge;99.7%</td></tr><tr><td>Cyclohexane&amp;nbsp;</td><td>Fisher Chemicals</td><td>C/8933/17</td><td>for residue analysis</td></tr><tr><td>Empty polypropylene SPE Tube with PE frits, 20 &amp;mu;m porosity, volume 6&amp;nbsp;ml</td><td>Supelco</td><td>57026</td><td></td></tr><tr><td>Empore SPE Disks, C&lt;sub&gt;18&lt;/sub&gt;, diam. 47&amp;nbsp;mm</td><td>Supelco</td><td>66883-U</td><td>Passive sampler</td></tr><tr><td>Empore SPE Disks, SDB-RPS (Reversed-Phase Sulfonate), diam. 47&amp;nbsp;mm</td><td>Supelco</td><td>66886-U&amp;nbsp;</td><td>Passive sampler</td></tr><tr><td>POCIS-A&amp;nbsp;</td><td>EST</td><td>POCIS-HLB</td><td>Passive sampler</td></tr><tr><td>POCIS-B</td><td>EST</td><td>POCIS-Pesticide&amp;nbsp;</td><td>Passive sampler</td></tr><tr><td>Polyethersulfone (PES) membranes</td><td>EST</td><td>PES</td><td></td></tr><tr><td>Silicone rubber sheet</td><td>Altec</td><td>03-65-4516</td><td>Passive sampler</td></tr><tr><td>Agilent 5975C</td><td>Agilent Technologies</td><td>5975C</td><td>GC-MS</td></tr><tr><td>HP-5MS UI</td><td>J&amp;amp;W Scientific</td><td>HP-5MS</td><td>Analytical column for GC-MS</td></tr><tr><td>Agilent 6460</td><td>Agilent Technologies</td><td>6460</td><td>HPLC-MS/MS</td></tr><tr><td>Strata C18&amp;ndash;E, 20 x 2 mm id and 20&amp;ndash;25 &amp;mu;m particle size</td><td>Phenomenex</td><td>Strata C18&amp;ndash;E</td><td>Online SPE column for LC-MS/MS</td></tr><tr><td>Strata X, 20 x 2 mm id and 20&amp;ndash;25 &amp;mu;m particle size</td><td>Phenomenex</td><td>Strata X</td><td>Online SPE column for LC-MS/MS</td></tr><tr><td>Zorbax Eclipse Plus C18</td><td>Agilent Technologies</td><td>Zorbax Eclipse Plus C18</td><td>Analytical column for LC-MS/MS</td></tr><tr><td>Isolute phase separator, 25 ml</td><td>Biotage</td><td>120-1907-E</td><td></td></tr><tr><td>Stainless steel blind rivet, 3.2x10&amp;nbsp;mm</td><td>Ejot &amp;amp; Avdel</td><td>951222</td><td></td></tr></tbody></table>

characterization and application of passive samplers for monitoring of pesticides in water

다섯 가지 물 패시브 샘플러 (124) 기존의 측정 및 현재 사용되는 농약에 대한 실험실 조건에서 보정 하였다. 이 연구는 패시브 샘플러 준비, 교정, 추출 방법 및 기기 분석을위한 프로토콜을 제공합니다. 샘플링 레이트 (R 용 S) 및 수동 샘플러 - 물 분배 계수 (K PW)는 실리콘 고무, 극성 유기 화학 통합 샘플러 POCIS-A, POCIS-B, SDB-RPS 및 C (18)의 디스크에 대해 계산 하였다. 선택된 화합물의 흡수가 자신의 물리 화학적 특성에 의존, 즉, 실리콘 고무 POCIS-A 반면, POCIS-B 및 SDB-을, (옥탄 올 - 물 분배 계수 (K OW)&gt; 5.3 로그) 소수성 화합물에 대한 더 나은 이해를 보여 주었다 RPS 디스크는 친수성 화합물 (K OW &lt;0.70를 기록)에 더 적합했다.

다섯 가지 패시브 샘플러 기술은 124 유산의 흡수와 실리콘 고무 (그림 1) POCIS A, POCIS B, SDB-RPS와 C (18) 디스크 (그림 2)을 포함하여 현재 사용되는 농약에 대해 비교 하였다. 추출 방법 및 기기 분석의 성능을 최적화 하였다. 실험실 흡수 실험의 결과는 PW 값 개별 살충제 (도 3)에 대한 흡수 프로파일에 기초하여 <stro...

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Characterization and Application of Passive Samplers for Monitoring of Pesticides in Water

A protocol about the characterization and application of five different passive sampling devices is presented.

물에 농약의 모니터링을위한 특성화 및 패시브 샘플러의 응용 프로그램

Five different water passive samplers were calibrated under laboratory conditions for measurement of 124 legacy and current used pesticides. This study ...

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JoVE Journal

Environment

9.4K 조회수.  Swedish University of Agricultural Sciences. A protocol about the characterization and application of five different passive sampling devices is presented.

비디오: Characterization and Application of Passive Samplers for Monitoring of Pesticides in Water

Integrated Field Lysimetry and Porewater Sampling for Evaluation of Chemical Mobility in Soils and Established Vegetation

Potentially toxic chemicals are routinely applied to land to meet growing demands on waste management and food production, but the fate of these chemicals is often not well understood. Here we demonstrate an integrated field lysimetry and porewater sampling method for evaluating the mobility of chemicals applied to soils and established vegetation. Lysimeters, open columns made of metal or plastic, are driven into bareground or vegetated soils. Porewater samplers, which are commercially available and use vacuum to collect percolating soil water, are installed at predetermined depths within the lysimeters. At prearranged times following chemical application to experimental plots, porewater is collected, and lysimeters, containing soil and vegetation, are exhumed. By analyzing chemical concentrations in the lysimeter soil, vegetation, and porewater, downward leaching rates, soil retention capacities, and plant uptake for the chemical of interest may be quantified. Because field lysimetry and porewater sampling are conducted under natural environmental conditions and with minimal soil disturbance, derived results project real-case scenarios and provide valuable information for chemical management. As chemicals are increasingly applied to land worldwide, the described techniques may be utilized to determine whether applied chemicals pose adverse effects to human health or the environment.

Field lysimetry and porewater sampling allow researchers to evaluate the fate of chemicals applied to soils and established vegetation. The goal of this protocol is to demonstrate how to install required instrumentation and collect samples for chemical analysis during integrated field lysimetry and porewater sampling experiments.

통합 필드 Lysimetry 및 Porewater 샘플링 토양에서 화학 이동성의 평가 및 설립 식물

Potentially toxic chemicals are routinely applied to land to meet growing demands on waste management and food production, but the fate of these chemicals ...

연구

환경과학

Calibrated Passive Sampling - Multi-plot Field Measurements of NH3 Emissions with a Combination of Dynamic Tube Method and Passive Samplers

Agricultural ammonia (NH3) emissions (90% of total EU emissions) are responsible for about 45% airborne eutrophication, 31% soil acidification and 12% fine dust formation within the EU15. But NH3 emissions also mean a considerable loss of nutrients. Many studies on NH3 emission from organic and mineral fertilizer application have been performed in recent decades. Nevertheless, research related to NH3 emissions after application fertilizers is still limited in particular with respect to relationships to emissions, fertilizer type, site conditions and crop growth. Due to the variable response of crops to treatments, effects can only be validated in experimental designs including field replication for statistical testing. The dominating ammonia loss methods yielding quantitative emissions require large field areas, expensive equipment or current supply, which restricts their application in replicated field trials. This protocol describes a new methodology for the measurement of NH3 emissions on many plots linking a simple semi-quantitative measuring method used in all plots, with a quantitative method by simultaneous measurements using both methods on selected plots. As a semi-quantitative measurement method passive samplers are used. The second method is a dynamic chamber method (Dynamic Tube Method) to obtain a transfer quotient, which converts the semi-quantitative losses of the passive sampler to quantitative losses (kg nitrogen ha-1). The principle underlying this approach is that passive samplers placed in a homogeneous experimental field have the same NH3 absorption behavior under identical environmental conditions. Therefore, a transfer co-efficient obtained from single passive samplers can be used to scale the values of all passive samplers used in the same field trial. The method proved valid under a wide range of experimental conditions and is recommended to be used under conditions with bare soil or small canopies (&#60;0.3 m). Results obtained from experiments with taller plants should be treated more carefully.

Calibrated Passive Sampling - Multi-plot Field Measurements of NH3 Emissions with a Combination of Dynamic Tube Method and Passive Samplers

Ammonia emissions are a major threat to the environment by eutrophication, soil acidification and fine particle formation and stem mainly from agricultural sources. This method allows ammonia loss measurements in replicated field trials enabling statistical analysis of emissions and of relationships between crop development and emissions.

보정 수동 샘플링 - NH의 다중 플롯 필드 측정<sub&gt; 3</sub동적 튜브 방법 및 패시브 샘플러의 조합으로&gt; 배출

Agricultural ammonia (NH3) emissions (90% of total EU emissions) are responsible for about 45% airborne eutrophication, 31% soil acidification and 12% ...

A Simple Method for Automated Solid Phase Extraction of Water Samples for Immunological Analysis of Small Pollutants

A new method for solid phase extraction (SPE) of environmental water samples is proposed. The developed prototype is cost-efficient and user friendly, and enables to perform rapid, automated and simple SPE. The pre-concentrated solution is compatible with analysis by immunoassay, with a low organic solvent content. A method is described for the extraction and pre-concentration of natural hormone 17&#946;-estradiol in 100 ml water samples. Reverse phase SPE is performed with octadecyl-silica sorbent and elution is done with 200 &#181;l of methanol 50% v/v. Eluent is diluted by adding di-water to lower the amount of methanol. After preparing manually the SPE column, the overall procedure is performed automatically within 1 hr. At the end of the process, estradiol concentration is measured by using a commercial enzyme-linked immune-sorbent assay (ELISA). 100-fold pre-concentration is achieved and the methanol content in only 10% v/v. Full recoveries of the molecule are achieved with 1 ng/L spiked de-ionized and synthetic sea water samples.

A protocol for the extraction and pre-concentration of estradiol from water samples by using an automated and miniaturized system is presented.

작은 오염 물질의 면역 학적 분석을위한 물 샘플의 자동화 된 고체상 추출을위한 간단한 방법

A new method for solid phase extraction (SPE) of environmental water samples is proposed. The developed prototype is cost-efficient and user friendly, and ...

Clean Sampling and Analysis of River and Estuarine Waters for Trace Metal Studies

Most of the trace metal concentrations in ambient waters obtained a few decades ago have been considered unreliable owing to the lack of contamination control. Developments of some techniques aiming to reduce trace metal contamination in the last couple of decades have resulted in concentrations reported now being orders of magnitude lower than those in the past. These low concentrations often necessitate preconcentration of water samples prior to instrumental analysis of samples. Since contamination can appear in all phases of trace metal analyses, including sample collection (and during preparation of sampling containers), storage and handling, pretreatments, and instrumental analysis, specific care needs to be taken in order to reduce contamination levels at all steps. The effort to develop and utilize "clean techniques" in trace metal studies allows scientists to investigate trace metal distributions and chemical and biological behavior in greater details. This advancement also provides the required accuracy and precision of trace metal data allowing for environmental conditions to be related to trace metal concentrations in aquatic environments.
This protocol that is presented here details needed materials for sample preparation, sample collection, sample pretreatment including preconcentration, and instrumental analysis. By reducing contamination throughout all phases mentioned above for trace metal analysis, much lower detection limits and thus accuracy can be achieved. The effectiveness of "clean techniques" is further demonstrated using low field blanks and good recoveries for standard reference material. The data quality that can be obtained thus enables the assessment of trace metal distributions and their relationships to environmental parameters.

Special care using "clean techniques" is required to properly collect and process water samples for trace metal studies in aquatic environments. A protocol for sampling, processing, and analytical procedures with the aim of obtaining reliable environmental monitoring data and results with high sensitivity for detailed trace metal studies is presented.

클린 샘플링 및 추적 금속 연구 강 하구 바다의 분석

Most of the trace metal concentrations in ambient waters obtained a few decades ago have been considered unreliable owing to the lack of contamination ...

Protocols for Quantifying Transferable Pesticide Residues in Turfgrass Systems

Plant canopies in established turfgrass systems can intercept an appreciable amount of sprayed pesticides, which can be transferred through various routes onto humans. For this reason, transferable pesticide residue experiments are required for registration and re-registration by the United States Environmental Protection Agency (USEPA). Although such experiments are required, limited specificity is required pertaining to experimental approach. Experimental approaches used to assess pesticide transfer to humans including hand wiping with cotton gloves, modified California roller (moving a roller of known mass over cotton cloth) and soccer ball roll (ball wrapped with sorbent strip) over three treated turfgrass species (creeping bentgrass, hybrid bermudagrass and tall fescue maintained at 0.4, 5 and 9 cm, respectively) are presented. The modified California roller is the most extensively utilized approach to date, and is best suited for use at low mowing heights due to its reproducibility and large sampling area. The soccer ball roll is a less aggressive transfer approach; however, it mimics a very common occurrence in the most popular international sport, and has many implications for nondietary pesticide exposure from hand-to-mouth contact. Additionally, this approach may be adjusted for other athletic activities with limited modification. Hand wiping is the best approach to transfer pesticides at higher mowing heights, as roller-based approaches can lay blades over; however, it is more subjective due to more variable sampling pressure. Utility of these methods across turfgrass species is presented, and additional considerations to conduct transferable pesticide residue research in turfgrass systems are discussed.

Transferable pesticide residue experiments in turfgrass systems are integral components of human risk exposure assessments. Experimental approaches to measure transferable residues should be adjusted to the human interaction of interest and turfgrass system dynamics. Three transferable pesticide residue protocols are presented and the suitability across three turfgrass systems is discussed.

잔디가 시스템에 양도 잔류 농약을 정량화하기위한 프로토콜

Plant canopies in established turfgrass systems can intercept an appreciable amount of sprayed pesticides, which can be transferred through various routes ...

Vegetated Treatment Systems for Removing Contaminants Associated with Surface Water Toxicity in Agriculture and Urban Runoff

Urban stormwater and agriculture irrigation runoff contain a complex mixture of contaminants that are often toxic to adjacent receiving waters. Runoff may be treated with simple systems designed to promote sorption of contaminants to vegetation and soils and promote infiltration. Two example systems are described: a bioswale treatment system for urban stormwater treatment, and a vegetated drainage ditch for treating agriculture irrigation runoff. Both have similar attributes that reduce contaminant loading in runoff: vegetation that results in sorption of the contaminants to the soil and plant surfaces, and water infiltration. These systems may also include the integration of granulated activated carbon as a polishing step to remove residual contaminants. Implementation of these systems in agriculture and urban watersheds requires system monitoring to verify treatment efficacy. This includes chemical monitoring for specific contaminants responsible for toxicity. The current paper emphasizes monitoring of current use pesticides since these are responsible for surface water toxicity to aquatic invertebrates.

This article summarizes the design attributes and the effectiveness of treatment systems that treat urban stormwater and agriculture irrigation runoff to remove pesticides and other contaminants associated with aquatic toxicity.

농업과 도시 유출수의 지표수 독성과 관련된 오염 물질 제거를위한 식물 처리 시스템

Urban stormwater and agriculture irrigation runoff contain a complex mixture of contaminants that are often toxic to adjacent receiving waters. Runoff may ...

Continuous Instream Monitoring of Nutrients and Sediment in Agricultural Watersheds

Pollutant concentrations and loads in watersheds vary considerably with time and space. Accurate and timely information on the magnitude of pollutants in water resources is a prerequisite for understanding the drivers of the pollutant loads and for making informed water resource management decisions. The commonly used &#34;grab sampling&#34; method provides the concentrations of pollutants at the time of sampling (i.e., a snapshot concentration) and may under- or overpredict the pollutant concentrations and loads. Continuous monitoring of nutrients and sediment has recently received more attention due to advances in computing, sensing technology, and storage devices. This protocol demonstrates the use of sensors, sondes, and instrumentation to continuously monitor in situ nitrate, ammonium, turbidity, pH, conductivity, temperature, and dissolved oxygen (DO) and to calculate the loads from two streams (ditches) in two agricultural watersheds. With the proper calibration, maintenance, and operation of sensors and sondes, good water quality data can be obtained by overcoming challenging conditions such as fouling and debris buildup. The method can also be used in watersheds of various sizes and characterized by agricultural, forested, and/or urban land.

With the advancement of technology and the rise in end-user expectations, the need and use of higher temporal resolution data for pollutant load estimation has increased. This protocol describes a method for continuous in situ water quality monitoring to obtain higher temporal resolution data for informed water resource management decisions.

연속 Instream 영양분과 농업 Watersheds에 앙금의 모니터링

Pollutant concentrations and loads in watersheds vary considerably with time and space. Accurate and timely information on the magnitude of pollutants in ...

Capturing Flow-weighted Water and Suspended Particulates from Agricultural Canals During Drainage Events

The purpose of this study is to describe the methods used to capture flow-weighted water and suspended particulates from farm canals during drainage discharge events. Farm canals can be enriched by nutrients such as phosphorus (P) that are susceptible to transport. Phosphorus in the form of suspended particulates can significantly contribute to the overall P loads in drainage water. A settling tank experiment was conducted to capture suspended particulates during discrete drainage events. Farm canal discharge water was collected in a series of two 200 L settling tanks over the entire duration of the drainage event, so as to represent a composite subsample of the water being discharged. Imhoff settling cones are ultimately used to settle out the suspended particulates. This is achieved by siphoning water from the settling tanks via the cones. The particulates are then collected for physico-chemical analyses.

Nutrients present in particulate form can contribute significantly to the overall loads in agricultural drainage waters. This study describes a novel method to capture flow-weighted water and suspended particulates from farm canal drainage over the entire duration of the drainage event.

배수 이벤트 기간 동안 흐름 중 물과 농업 운하에서 일시 중단 된 입자를 캡처

The purpose of this study is to describe the methods used to capture flow-weighted water and suspended particulates from farm canals during drainage ...

Continuous Hydrologic and Water Quality Monitoring of Vernal Ponds

Vernal ponds, also referred to as vernal pools, provide critical ecosystem services and habitat for a variety of threatened and endangered species. However, they are vulnerable parts of the landscapes that are often poorly understood and understudied. Land use and management practices, as well as climate change are thought to be a contribution to the global amphibian decline. However, more research is needed to understand the extent of these impacts. Here, we present methodology for characterizing a vernal pond's morphology and detail a monitoring station that can be used to collect water quantity and quality data over the duration of a vernal pond's hydroperiod. We provide methodology for how to conduct field surveys to characterize the morphology and develop stage-storage curves for a vernal pond. Additionally, we provide methodology for monitoring the water level, temperature, pH, oxidation-reduction potential, dissolved oxygen, and electrical conductivity of water in a vernal pond, as well as monitoring rainfall data. This information can be used to better quantify the ecosystem services that vernal ponds provide and the impacts of anthropogenic activities on their ability to provide these services.

Understanding the ecosystem services and processes provided by vernal ponds and the impacts of anthropogenic activities on their ability to provide these services requires intensive hydrologic monitoring. This sampling protocol using in-situ monitoring equipment was developed to understand the impact of anthropogenic activities on water levels and quality.

지속적인 문학적 품질 모니터링 Vernal 연못의 물

Vernal ponds, also referred to as vernal pools, provide critical ecosystem services and habitat for a variety of threatened and endangered species. ...

Identifying Per- and Polyfluorinated Chemical Species with a Combined Targeted and Non-Targeted-Screening High-Resolution Mass Spectrometry Workflow

Historical and emerging per- and polyfluoroalkyl substances (PFASs) have garnered significant interest from the public and government agencies from the local to federal levels. The continuing evolution of PFAS chemistries presents a challenge to the environmental monitoring, where ongoing development of targeted methods necessarily lags the discovery of new chemical compounds. There is a need, therefore, to have forward-looking methodologies that can detect emerging and unexpected compounds, monitor these species over time, and resolve details of their chemical structure to enable future work in human health. To this end, non-targeted analysis by high-resolution mass spectrometry offers a broad base detection approach that can be combined with almost any sample preparation scheme and provides significant capabilities for compound identification after detection. Herein, we describe a solid-phase extraction (SPE) based sample concentration method tuned for shorter chain and more hydrophilic PFAS chemistries, such as per fluorinated ether acids and sulfonates, and describe analysis of samples prepared in this fashion in both targeted and non-targeted modes. Targeted methods provide superior quantification when reference standards are available but are intrinsically limited to expected compounds when performing analysis. In contrast, a non-targeted approach can identify the presence of unexpected compounds and provide some information about their chemical structure. Information about chemical features can be used to correlate compounds across sample locations and track abundance and occurrence over time.

Here, we present a protocol for the sequential targeted quantification and non-targeted analysis of fluorinated compounds in water by mass spectrometry. This methodology provides quantitative levels of known fluorochemical compounds and identifies unknown chemicals in related samples with semi-quantitative estimates of their abundance.

당 식별-및 결합된 대상 및 비 대상 심사 고해상도 질량 분석 워크플로 Polyfluorinated 화학 종

Historical and emerging per- and polyfluoroalkyl substances (PFASs) have garnered significant interest from the public and government agencies from the ...