Validacija metoda za određivanje prioritetnih pesticida u vodi
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1 MATCROSS HUSRB/1002/214/188 Validacija metoda za određivanje prioritetnih pesticida u vodi Dr Marijana Kragulj
2 Okvirna Direktiva o Vodama (WFD)-Aneks X Prioritetne supstance Uredba o graničnim i vrednostima prioritetnih it t ih i prioritetnih hazardnih supstanci (Sl.glasnik RS, br. 35/2011). Prioritetne supstance Predstavljaju značajan rizik za vodenu sredinu ili preko vodene sredine Cilj : progresivna redukcija ispuštanja, emisija i gubitaka Prioritetne hazardne supstance Podgrupa prioritetnih supstanci koje su: Toksične Perzistentne t Podložne bioakumulaciji Cilj: potpuno p ukidanje ispuštanja, emisija i gubitaka i onemogućavanje daljeg zagađenja životne sredine
3 Prioritetni pesticidi Uredba o graničnim vrednostima prioritetnih i prioritetnih hazardnih supstanci (Sl.glasnik l RS, br. 35/2011) Prioritetne hazardne supstance-(phs) Prosečna godišnja koncentracija (PGK) (μg/l) Maksimalno dozvoljena koncentracija (MDK) (μg/l) Atrazin 0,6 2,0 Ciklodienski pesticidi: Aldrin Dieldrin Endrin X Suma 0,01 / Ukupni DDT 0,025 / Para-para- DDT 0,01 / Endosulfan X 0,005 0,01 Heksahlorobenzen X 0,01 0,05 Heksahlorocikloheksan X 0,02 0,04 Simazin 1 4 Trihlorobenzeni (svi izomeri) i) 0,4 / Trifluralin 0,03 /
4 Analitički aspekti i izazovi Zahtevi u pogledu metoda Postojeće metode/standardi QA/QC Q zahtevi Problemi i novi prilazi
5 Član 8.3 Zahtevi WFD u pogledu primenjenih analitičkih metoda i kvaliteta rezultata Tehničke specifikacije i standardizovane metode za analize i monitoring statusa voda biće ustanovljene u postupku iz člana 21. Aneks V, paragraf Metode korišćene za monitoring definišu se u skladu sa međunarodnim standardima, ili s drugim nacionalnim ili međunarodnim standardima kojima se obezbeđuje prikupljanje uporedivih podataka odgovarajućeg naučnog kvaliteta. Alternativno, moguće je koristiti druge ne standardizovane validovane metode koje obezbeđuju isti ili bolji naučni kvalitet i uporedivost podataka.
6 Analitičke metode Direktiva 2009/90/EC Minimalni i i kriterijumi ij i za analitičke metode Sve metode analize korišćene u programu hemijskog monitoringa i bi trebale biti validovane i dokumentovane, a pogodan okvir za sprovođenje validacije predstavlja međunarodni standard EN ISO/IEC U cilju postizanja zahteva validacije i obezbeđivanja odgovarajućeg kvaliteta rezultata, koji obezbeđuje uporedivost rezultata između laboratorija, sve analitičke metode moraju zadovoljiti odgovarajuće minimalne kriterijume, uključujući odgovarajuću mernu nesigurnost i limit kvantitacije.
7 Direktiva 2009/90/EC Minimalni kriterijumi za analitičke metode Minimalni kriterijumi za sve analitičke metode su bazirani na mernoj nesigurnosti od 50% ili niže (k=2) procenjenoj na nivou odgovarajućeg standarda kvaliteta životne sredine. U odsustvu odgovarajuće standardne metode koja zadovoljava zahteve, monitoring se sprovodi korišćenjem najbolje dostupne tehnike koja ne prouzrokuje dodatne troškove. Praktična granica kvantitacije (PQL) PQL 0, 3 PGK
8 Postojeće metode/standardi za analizu prioritetnih pesticida u vodi Prioritetna supstanca Standardni metod EN ISO 11369:1997 EN ISO 10695:2000 EN ISO 11370:2000 Atrazin, Simazin US EPA 505 US EPA 3510C ISO 11370:2000 DDT (4 izomera), Endosulfan, Heksahlorbenzen, Heksahlorcikloheksan EN ISO 6468:1996 Pentahlorbenzen EN ISO 6468:1996 Ciklodienski pesticidi: US EPA 505 Aldrin US EPA 1699 Dieldrin Endrin Trihlorbenzeni EN ISO 6468:1996 EN ISO 10695:2000 Trifluralin ISO 11370:2000 US EPA 3510C
9 ODABRANE ANALITIČKE METODE NAŠA ISKUSTVA Prioritetni pesticidi Metoda Priprema uzorka Tehnika detekcije Tečno-tečno Atrazin, Simazin EPA metod 3510C 1 ekstrakcija heksanom GC-MSD Ciklodienski pesticidi: Aldrin Dieldrin Endrin Ukupni DDT Para-para- DDT Endosulfan Heksahlorcikloheksan EPA SM Tečno-tečno ekstrakcija dihlormetanom GC-ECD Heksahlorobenzen Trifluralin Trihlorbenzeni Modifikovana EPA 3510C Tečno-tečno ekstrakcija heksanom GC-ECD 1. EPA Method 3510C Separatory funnel liquid-liquid extraction, Revision 3, December Method 6630 in Standard Methods For the Examination of Water and Wastewater, Edited by: Eugene W. Rice, Rodger B. Baird, Andrew D. Eaton, Lenore S. Clesceri, 22nd Edition. American Public Health Association, American Water Association, Water Environment Federation, Washington, Method 1699: Pesticides in Water, Soil, Sediment, Biosolids, and Tissue by HRGC/HRMS, EPA methods, December, 2007.
10 QA/QC zahtevi Prioritetna supstanca (PS) Prosečna godišnja koncentracija (PGK) (μg/l) Maksimalno dozvoljena koncentracija (MDK) (μg/l) PQL potrebna (µg/l) PQL postignuta (µg/l) Atrazin 0,6 2,0 0,180 0,120 Ciklodienski pesticidi: Aldrin Dieldrin Endrin Izodrin Suma 0,01 / Suma 0,0030 0,0025-0,0065 Ukupni DDT 0,025 / 0,0075 0,0050 Para-para- DDT 0,01 / 0,0030 0,0050 Endosulfan 0,005 0,01 0,0015 0,0025 Heksahlorobenzen 0,01 0,05 0,0030 0,0030 Heksahlorocikloheksan 0,02 0,04 0,0060 0,0050 Simazin 1 4 0,300 0,120 Trihlorobenzeni (svi izomeri) i) 0,4 / 0,120 0,100 Trifluralin 0,03 / 0,0090 0,0075
11 Prioritetni pesticidi Karakteristike odabranih analitičkih metoda Tačnost* Preciznost* MDL % recovery % RSD ng/l Atrazin, Simazin ,0 Ciklodienski pesticidi ,00-2,60 DDT Endosulfan ,00-2,50 Heksahlorobenzen ,87 Heksahlorocikloheksan ,30-2,00 Trihlorbenzeni ,0 Trifluralin ,02 *EPA8000B: Recovery %; RSD < 30%
12 Merna nesigurnost Direktiva 2009/90/EC Minimalni kriterijumi za sve analitičke metode su bazirani na mernoj nesigurnosti od 50% ili niže (k=2) procenjenoj na nivou odgovarajućeg standarda kvaliteta životne sredine. Dobijene proširene merne nesigurnosti za sve prioritetne pesticide su u opsegu od 20-40% (koncentracioni nivo od ng/l).
13 PESTICIDI-PROBLEMI Primena gasne hromatografije u kombinaciji sa ECD ili MS daje zadovoljavajuće PQL vrednosti za većinu prioritetnih pesticida. Granica kvantitacije metoda su na nivou od ng/l (dovoljno da se zadovolje zahtevi PGK za većinu prioritetnih pesticida prema Uredbi o graničnim vrednostima prioritetnih i prioritetnih hazardnih supstanci). Dobijene PQL vrednosti za endosulfan i sumu ciklodienskih pesticida (aldrin, dieldrin, endrin) su više od potrebnih PQL vrednosti da se zadovolje zahtevi PGK.
14 Prioritetni pesticidi za koje je neophodna dalja optimizacija analitičkih metoda Ciklodienski pesticidi Aldrin, dieldrin, endrin Endosulfan: Zahtevi u pogledu PQL: predloženi PGK je 5 ng/l!
15 Hvala na pažnji!
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