EN 15742:2009

Animal feeding stuffs - Determination of OC-pesticides and PCB’s by GC/ECD

This European Standard specifies a gas chromatographic method with electron capture detection (ECD) for the determination of organochlorine pesticides (OC’s) and polychlorinated biphenyls (PCBs) in animal feeding stuffs.
The method is applicable to animal feeding stuffs with a water content up to about 20 wt% and oil/fatty samples containing residues of one or more of the following OC’s, PCBs, toxaphene and some of their isomers and degradation products:
-   Aldrin;
-   Dieldrin;
-   Chlorocamphene (Toxaphene);
-   Chlordane (= sum of Chlordane isomers and Oxychlordane);
-   DDT (= sum of isomers op'-DDT, pp'-DDT, pp'-TDE (pp'-DDD), and pp'-DDE);
-   Endosulfan (sum of -/-isomers and Endosulphanesulphate);
-   Endrin;
-   Heptachlor (= sum of Heptachlor and -Heptachlorepoxide);
-   Hexachlorobenzene (HCB);
-   Hexachlorocyclohexane isomers -HCH (-BHC), -HCH (-BHC), γ-HCH (γ-BHC or lindane);
-   PCB 28, 52, 101, 138, 153 and 180 (“Indicator PCBs”) and PCB 198, 209.
The limit of quantification for the mentioned organochlorine pesticides and PCBs is 5 ng/g in general. However, 10 ng/g applies for Heptachlor, Aldrin, Endrin, Dieldrin, and Endosulfan (-, - and sulphate). Individual laboratories are responsible to ensure that the equipment they used will achieve these limits of quantifications.

Futtermittel - Bestimmung der OC-Pestizide und PCB's mittels GC/ECD-Verfahren

Diese Europäische Norm legt ein gaschromatographisches Verfahren mit Elektroneneinfangdetektor (ECD)
für die Bestimmung von Organochlorpestiziden (OC-Pestizide) und polychlorierten Biphenylen (PCB’s) in
Futtermitteln fest.
Das Verfahren ist auf Futtermittel mit einem Wassergehalt bis zu etwa 20 % (Massenanteil) und für öl-/fetthaltige
Proben anwendbar, die Rückstände von einem oder mehreren der folgenden OC-Pestiziden und
PCB’s und einige von deren Isomeren und Abbauprodukten enthalten:
⎯ Aldrin;
⎯ Dieldrin;
⎯ Chlorcamphen (Toxaphen);
⎯ Chlordan (= Summe von Chlordanisomeren und Oxychlordan);
⎯ DDT (= Summe der Isomere von op'-DDT, pp'-DDT, pp'-TDE (pp'-DDD) und pp'-DDE);
⎯ Endosulfan (= Summe von α-/ β-Isomeren und Endosulfansulfat);
⎯ Endrin;
⎯ Heptachlor (= Summe von Heptachlor und β-Heptachlorepoxid);
⎯ Hexachlorbenzen (HCB);
⎯ Hexachlorcyclohexan-Isomere α-HCH ( α-BHC), β-HCH ( β-BHC), γ-HCH ( γ-BHC oder Lindan);
⎯ PCB 28, 52, 101, 138, 153 und 180 („Indikator-PCB's“) und PCB 198, 209.
Die Identifizierungsgrenze der betreffenden Organochlorpestizide und PCB’s beträgt gewöhnlich 5 ng/g.
Jedoch werden 10 ng/g für Heptachlor, Aldrin, Endrin, Dieldrin und Endosulfan ( α-, β- und Sulfat) angewendet.
Einzelne Laboratorien sind verantwortlich für die Absicherung, dass die von ihnen verwendete Ausrüstung
diese Quantifizierungsgrenzen erreichen.

Aliments des animaux - Détermination des pesticides organochlorés (OC) et des polychlorobiphényles (PCB) par GC/ECD

La présente Norme européenne spécifie une méthode de chromatographie en phase gazeuse (CPG) avec détection par capture d'électrons (ECD) pour la détermination de pesticides organochlorés (OC) et de polychlorobiphényles (PCB) dans les aliments pour animaux.
La méthode est applicable aux aliments pour animaux dont la teneur en eau s'élève jusqu’à environ 20 % du poids et aux échantillons d'huile/graisses contenant des résidus d'un ou de plusieurs OC et PCB, du toxaphène ou certains de leurs isomères et produits de dégradation suivants :
- Aldrine ;
- Dieldrine ;
- camphéchlore (toxaphène) ;
- Chlordane (= somme des isomères de Chlordane et Oxychlordane) ;
- DDT (= somme des isomères de op'-DDT, pp'-DDT, pp'-TDE (pp'-DDD), et pp'-DDE) ;
- Endosulfan (somme des isomères a-/b et sulfate d’Endosulfan) ;
- Endrine ;
- Heptachlore (= somme d’Heptachlore et d'Heptachlor époxyde b) ;
- Hexachlorobenzène (HCB) ;
- Isomères Hexachlorocyclohexane a-HCH (a-BHC), b-HCH (b-BHC), ###-HCH (###-BHC ou lindane) ;
- PCB 28, 52, 101, 138, 153 et 180 ("PCB indicateurs") et PCB 198, 209.
La limite de quantification des pesticides organochlorés et des PCB mentionnés est en général de 5 ng/g. Cependant, 10 ng/g s’applique à l’heptachlore, l’aldrine, l’endrine, le dieldrine et l’endosulfan (a-, b- et sulfate). Il incombe aux laboratoires individuels de garantir que les appareils qu’ils utilisent atteignent ces limites de quantification.

Krma - Določevanje OC-pesticidov in PCB z GC/ECD

General Information

• Status: Withdrawn
• Publication Date: 24-Feb-2009
• Withdrawal Date: 24-Mar-2020
• ICS: 65.120 - Animal feeding stuffs
• Technical Committee: CEN/TC 327 - Animal feeding stuffs - Methods of sampling and analysis
• Drafting Committee: CEN/TC 327 - Animal feeding stuffs - Methods of sampling and analysis
• Current Stage: 9960 - Withdrawal effective - Withdrawal
• Completion Date: 25-Mar-2020
• Directive: 70/373/EC - Council Directive 70/373/EEC of 20 July 1970 on the introduction of Community methods of sampling and analysis for the official control of feeding-stuffs
• Mandate: M/315 - Mandate to CEN for standardization in the field of methods of analysis for animal feedingstuffs
• Ref Project: SIST EN 15742:2009 - Animal feeding stuffs - Determination of OC-pesticides and PCB’s by GC/ECD

Relations

• Replaced By: EN 15742:2020 - Animal feeding stuffs: Methods of sampling and analysis - Determination of OCPs by GC-ECD
• Effective Date: 01-Apr-2020

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Futtermittel - Bestimmung der OC-Pestizide und PCB's mittels GC/ECD-VerfahrenAliments des animaux - Détermination des pesticides organochlorés (OC) et des polychlorobiphényles (PCB) par GC/ECDAnimal feeding stuffs - Determination of OC-pesticides and PCB’s by GC/ECD65.120KrmilaAnimal feeding stuffsICS:Ta slovenski standard je istoveten z:EN 15742:2009SIST EN 15742:2009en,fr,de01-maj-2009SIST EN 15742:2009SLOVENSKI
STANDARD
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 15742February 2009ICS 65.120 English VersionAnimal feeding stuffs - Determination of OC-pesticides andPCB's by GC/ECDAliments des animaux - Détermination des pesticidesorganochlorés (OC) et des polychlorobiphényles (PCB) parGC/ECDFuttermittel - Bestimmung der OC-Pestizide und PCB'smittels GC/ECD-VerfahrenThis European Standard was approved by CEN on 24 January 2009.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre:
Avenue Marnix 17,
B-1000 Brussels© 2009 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15742:2009: ESIST EN 15742:2009

Results of interlaboratory tests . 22 Bibliography . 23
 Heptachlor (= sum of Heptachlor and β-Heptachlorepoxide);  Hexachlorobenzene (HCB);  Hexachlorocyclohexane isomers α-HCH (α-BHC), β-HCH (β-BHC), -HCH (-BHC or lindane);  PCB 28, 52, 101, 138, 153 and 180 (“Indicator PCBs”) and PCB 198, 209. The limit of quantification for the mentioned organochlorine pesticides and PCBs is 5 ng/g in general. However, 10 ng/g applies for Heptachlor, Aldrin, Endrin, Dieldrin, and Endosulfan (α-, β- and sulphate). Individual laboratories are responsible to ensure that the equipment they used will achieve these limits of quantifications. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 6498, Animal feeding stuffs – Preparation of test samples 3 Terms and definitions For the purpose of this document, the following terms and definitions apply. 3.1 limit of detection smallest measured content, from which it is possible to deduce the presence of the analyte with reasonable statistical certainty SIST EN 15742:2009

 chromatography on partially deactivated silica gel. The collected fraction containing the compounds of interest is concentrated and re-dissolved in a solution containing another internal standard (PCB 209) as a reference standard. After cleanup the analytes are measured using GC-ECD. Indentification is done on the basis of comparing retention times on capillary columns of different polarity. Quantification is done using the internal standard method. 5 Reagents and materials Use only reagents of recognized analytical grade and with a purity suitable for OC and PCB residue analysis. Check the purity of the reagents by performing a blank test under the same conditions as used in the method. The chromatogram should not show any interfering impurity at the retention time of compounds of interest. WARNING — The use of this European Standard can involve hazardous materials, operations and equipment. This standard does not purport to address all the safety problems associated with its use. It is the responsibility of the user of this European Standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 5.1 Cyclohexane
5.2 Ethylacetate
5.3 Hexane 5.4 Dichloromethane 5.5 Iso-octane 5.6 Toluene SIST EN 15742:2009

5.13 OC-pesticide reference standards Each with a purity not less than 99%. Aldrin ((1R,4S,4aS,5S,8R,8aR)-1,2,3,4,10,10-hexachloro-1,4,4a,5,8,8a-hexahydro-1,4:5,8-dimethanonaphthalene) CAS Number: 309-00-2 Dieldrin ((1R,4S,4aS,5R,6R,7S,8S,8aR)-1,2,3,4,10,10-hexachloro-1,4,4a,5,6,7,8,8a-octahydro-6,7epoxy-1,4:5,8-dimethanonaphthalene) CAS Number: 60-57-1 Chlordane (1,2,4,5,6,7,8,8-octachloro-2,3,3a,4,7,7a-hexahydro-4,7-ethano-1H-indene); α and β isomer CAS Numbers: 5103-71-9 and 5103-74-2 Oxychlordane
(4,7-Methanoindan, 1,2,4,5,6,7,8,8-octachloro-2,3-epoxy-3a,4,7,7a-tetrahydro-, exo,endo-) CAS Number: 27304-13-8 op'-DDT
[o,p'-(1,1,1-trichloro-2,2-bis(4-chlorophenyl)ethane)] CAS Number: 789-02-6 SIST EN 15742:2009

[p,p'-(1,1,1-trichloro-2,2-bis(4-chlorophenyl) ethane)]
CAS Number: 50-29-3 pp'-TDE
(p,p'-DDD) [ p,p'-1,1-dichloro-2,2-bis(4-chlorophenyl) ethane]
CAS Number: 72-54-8 pp'-DDE
[p,p'-(1,1-dichloro-2,2-bis(4-chlorophenyl) ethylene)]
CAS Number: 72-55-9 Endosulfan
(6,7,8,9,10,10-hexachloro-1,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-benzodioxathiepin 3-oxide) two stereoisomers, α, (I), CAS Number: 959-98-8
and
β, (II), CAS Number: 33213-65-9. Endosulfan-sulphate;
CAS Number: 1031-07-8 Endrin
[(1R,4S,4aS,5S,6S,7R,8R,8aR)-1,2,3,4,10,10-hexachloro-1,4,4a,5,6,7,8,8a-octahydro-6,7-epoxy-1,4:5,8-dimethanonaphthalene]
CAS Number: 72-20-8 Heptachlor (1,4,5,6,7,8,8-heptachloro-3a,4,7,7a-tetrahydro-4,7-methanoindene)
CAS Number: 76-44-8 β-Heptachlorepoxide
(1,4,5,6,7,8,8-heptachloro-3a,4,7,7a-tetrahydro-4,7-methanoindene(exo)) CAS Number: 1024-57-3 HCB (hexachlorobenzene)
CAS Number: 118-74-1 α-HCH (α-BHC)
(α-1,2,3,4,5,6-hexachlorocyclohexane) CAS Number: 319-84-6 β-HCH (β-BHC)
(β-1,2,3,4,5,6-hexachlorocyclohexane)
CAS Number: 319-85-7 -HCH (-BHC; lindane)
(1,2,3,4,5,6-hexachlorocyclohexane)
CAS Number: 58-89-9 Or a Certified Mixture at a concentration of 10 µg/ml. 5.14 PCBs reference standards Each with a purity not less than 99%. PCB 28 (2,4,4’ trichlorobiphenyl) ; CAS Number: 7012-37-5 PCB 52 (2,2’,5,5’ tetrachlorobiphenyl) ; CAS Number: 35693-99-3 SIST EN 15742:2009
...