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 dont la teneur en matières grasses peut s'élever jusqu'à 10 % du poids, ainsi qu'aux échantillons d'huile et graisses contenant des résidus d'un ou de plusieurs OC et PCB, toxaphène ou certains de leurs isomères et produits de dégradation, suivants :
Aldrine
Dieldrine
Camphéchlore (toxaphène)
Chlordane ( somme des isomères de chlordane et d'oxychlordane)
DDT ( somme des isomères de op'-DDT, pp'-DDT, pp'-TDE (pp'-DDD), et pp'-DDE)
Endosulfan (somme des isomères / et du sulfate d'endosulfan)
Endrine
Heptachlore ( somme d'heptachlore et d'heptachlore époxyde )
Hexachlorobenzène (HCB)
Isomères d'hexachlorocyclohexane -HCH (-BHC), -HCH (-BHC), -HCH (-BHC ou lindane)
PCB 28, 52, 101, 118, 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 (-, - et sulfate). Il incombe aux laboratoires de s'assurer que l'équipement utilisé permet d’atteindre ces limites de quantification.

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

General Information

Status
Withdrawn
Publication Date
24-Mar-2009
Withdrawal Date
05-Apr-2020
Current Stage
9900 - Withdrawal (Adopted Project)
Start Date
03-Apr-2020
Due Date
26-Apr-2020
Completion Date
06-Apr-2020

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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
SIST EN 15742:2009

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

EN 15742:2009 (E) 2 Contents Page Foreword ............................................................................................................................................................. 3 1 Scope ...................................................................................................................................................... 4 2 Normative references ............................................................................................................................ 4 3 Terms and definitions ........................................................................................................................... 4 4 Principle .................................................................................................................................................. 5 5 Reagents and materials ........................................................................................................................ 5 6 Apparatus ............................................................................................................................................. 12 7 Sampling ............................................................................................................................................... 13 8 Preparation of test sample ................................................................................................................. 13 9 Procedure ............................................................................................................................................. 13 10 Calculation and expression of results............................................................................................... 15 11 Precision ............................................................................................................................................... 18 12 Test report ............................................................................................................................................ 21 13 Important considerations ................................................................................................................... 21 Annex A (informative)

Results of interlaboratory tests ............................................................................... 22 Bibliography ...................................................................................................................................................... 23

SIST EN 15742:2009

EN 15742:2009 (E) 3 Foreword This document (EN 15742:2009) has been prepared by Technical Committee CEN/TC 327 “Animal feeding stuffs”, the secretariat of which is held by NEN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by August 2009, and conflicting national standards shall be withdrawn at the latest by August 2009. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association, and supports essential requirements of EC Directive(s). According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: 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 the United Kingdom. SIST EN 15742:2009

EN 15742:2009 (E) 4 1 Scope 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 α-/β-isomers and Endosulfan-sulphate);  Endrin;

 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

EN 15742:2009 (E) 5 NOTE The limit of detection is numerically equal to three times the standard deviation of the mean of blank determinations (n>10). 3.2 limit of quantification lowest content of the analyte which can be measured with reasonable statistical certainty NOTE If both accuracy and precision are constant over a concentration range around the limit of detection, then the limit of quantification is numerically equal to 6 times the standard deviation of the mean of blank determinations (n>10). 3.3 feed additives substances are feed additives when they comply with the definition of feed additives given in the Regulation 1831/2003 4 Principle A test portion of animal feeding stuff is fortified with internal standard (PCB 198), and is extracted with ethylacetate. The extract is concentrated and subsequently purified by:  Gel permeation chromatography (GPC), with cyclohexane/ethylacetate as eluting solvent

 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

EN 15742:2009 (E) 6 5.7 Hexane/toluene = 3+7, parts by volume Mix 30 ml of hexan (5.3) with 70 ml of toluene (5.6) thoroughly. Store at room temperature in a tightly closed glass bottle. 5.8 Sodium Sulphate, anhydrous Heated at 160°C during at least 24 h. 5.9 Ethylacetate/Cyclohexane = 1+1, parts by volume Mix 500 ml of ethylacetate (5.2) with 500 ml of cyclohexane (5.1) thoroughly. Store at room temperature in a tightly closed glass bottle. 5.10 Silica gel, deactivated with 3,5% water Heat silica gel 60 (63µm to 200µm = 70 mesh to 230 mesh), at 130ºC for at least 5 h, allow to cool in a desiccator, and store in a tightly stopped container in the desiccator. To 96,5 g dried silica gel in a 300 ml Erlenmeyer flask with a ground joint, add 3,5 ml water dropwise from a burette, with continuous swirling. Immediately stopper the flask with a ground stopper and shake vigorously for 5 min until all lumps have disappeared. Next shake for 2 h on a mechanical shaker, and then store in a tightly stoppered container. Deactivated silica gel is tenable during approximately 2 weeks if carefully stored. 5.11 Internal standard (PCB 198) 5.12 Internal Standard (PCB 209)

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

EN 15742:2009 (E) 7 pp'-DDT
[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

EN 15742:2009 (E) 8 PCB 101 (2,2’,4,5,5’ pentachlorobiphenyl) ; CAS Number: 37680-73-2 PCB 138 (2,2’,3’,4,4’,5 hexachlorobiphenyl) ; CAS Number: 35065-28-2 PCB 153 (2,2’,4,4’,5,5’ hexachlorobiphenyl) ; CAS Number: 35065-27-1 PCB 180 (2,2’,3,4,4’,5,5’ heptachlorobiphenyl) ; CAS Number: 35065-29-3 Or a Certified Mixture at a concentration of 10 µg/ml. 5.15 Chlorocamphene (Toxaphene) Technical mixture. 5.16 Stock solutions, 100 µg/ml Weigh 5 -10 mg (± 0,01 mg) of each compound (5.11, 5.12, 5.13, 5.14 and 5.15) in seperate brown medicine glass bottles of 100 ml and add iso-octane (5.5) to achieve a concentration of 100 µg/ml. Store the solutions in a refrigerator at 4°C (± 3°C). The solution is tenable under these conditions during at least 5 years if the weight is carefully controled. Dissolve ß-HCH in 10 ml toluene (5.6), to achieve complete solvability and dilute further with iso-octane (5.5) to achieve a concentration of 100 µg/ml. 5.17 Mixed stock solutions 5.17.1 Mixed stock solution OC (without Endosulfan and Toxaphene) Pipet of each OC-stock solution (5.16) the indicated volume (Table 1) in a volumetric flask of 100 ml. Fill up to 100 ml with iso-octane (5.5) and mix. The achieved concentration is given in Table 1. Transport this solution to a brown medicine glass bottle of 100 ml and store it in a refrigerator at 4°C (± 3°C). The solution is tenable under these conditions during at least 5 years if the weight is carefully controled. 5.17.2 Mixed stock solution Endosulfan Pipet of each Endosulfan-stock solution (5.16) the indicated volume (Table 1) in a volumetric flask of 100 ml. Fill up to 100 ml with iso-octane (5.5) and mix. The achieved concentration is given in Table 1. Transport this solution to a brown medicine glass bottle of 100 ml and store it in a refrigerator at 4°C (± 3°C). The solution is tenable under these conditions during at least 5 years if the weight is carefully controled. SIST EN 15742:2009

EN 15742:2009 (E) 9

Table 1 — Concentration of OCs in Mixed stock solution (5.17) and mixed standard solution (5.18) Compound Pipet volume (ml) Mixed stock solution (5.17 1&2)

(µg/ml) Mixed standard solution (5.18.1 1&2) (µg/ml) Aldrin 2,0 2,0 0,10 Dieldrin 2,0 2,0 0,10 α-Chlordane 1,0 1,0 0,05 γ-Chlordane 1,0 1,0 0,05 Oxychlordane 1,0 1,0 0,05 o,p'-DDT 4,0 4,0 0,20 p,p'-DDT 4,0 4,0 0,20 p,p'-TDE 4,0 4,0 0,20 p,p'-DDE 4,0 4,0 0,20 α-Endosulfan 2,0 2,0 0,10 β-Endosulfan 2,0 2,0 0,10 Endosulfan-sulphate 1,0 1,0 0,05 Endrin 1,0 1,0 0,05 Heptachlor 2,0 2,0 0,10 Heptachlor epoxide 2,0 2,0 0,10 HCB 1,0 1,0 0,05 α-HCH 2,0 2,0 0,10 ß-HCH 1,0 1,0 0,05 γ-HCH (Lindane) 1,0 1,0 0,05

SIST EN 15742:2009

EN 15742:2009 (E) 10 5.17.3 Mixed stock solution Toxaphene, 10,0 µg/ml Pipet 10,0 ml of the Toxaphene-stock solution (5.16) in a volumetric flask of 100 ml. Fill up to 100 ml with iso-octane (5.5) and mix. Transport this solution to a brown medicine glass bottle of 100 ml and store it in a refrigerator at 4°C (± 3°C). The solution is tenable under these conditions during at least 5 years if the weight is carefully controled. 5.17.4 Mixed stock solution PCBs, 1,0 µg/ml Pipet 1,0 ml of each stock solution PCBs (5.16) in a volumetric flask of 100 ml. Fill up to 100 ml with iso-octane (5.5) and mix. Transport this solution to a brown medicine glass bottle of 100 ml and store it in a refrigerator at 4°C (± 3°C). The solution is tenable under these conditions during at least 5 years if the weight is carefully controled. 5.17.5 Internal standard stock solution PCB 198, 2,0 ug/ml Pipet 2,0 ml of the PCB 198-stock solution (5.16) in a volumetric flask of 100 ml. Fill up to 100 ml with iso-octane (5.5) and mix. Transport this solution to a brown medicine glass bottle of 100 ml and store it in a refrigerator at 4°C (± 3°C). The solution is tenable under these conditions during at least 5 years if the weight is carefully controled. 5.17.6 Internal standard stock solution PCB 209, 2,0 ug/ml Pipet 2,0 ml of the PCB 209-stock solution (5.16) in a volumetric flask of 100 ml. Fill up to 100 ml with iso-octane (5.5) and mix. Transport this solution to a brown medicine glass bottle of 100 ml and store it in a refrigerator at 4°C (± 3°C). The solution is tenable under these conditions during at least 5 years if the weight is carefully controled. 5.18 Mixed standard solution 5.18.1 Mixed standard solution OCs Pipet 5,0 ml of the mixed stock solution OCs (5.17.1) in a volumetric flask of 100 ml. Fill up to 100 ml with iso-octane (5.5) and mix. The achieved concentration is given in Table 1. Transport this solution to a brown medicine glass bottle of 100 ml and store it in a refrigerator at 4°C (± 3°C). The solution is tenable under these conditions during at least 5 years if the weight is carefully controled. 5.18.2 Mixed standard solution Endosulfan Pipet 5,0 ml of the mixed stock solution Endosulfan (5.17.2) in a volumetric flask of 100 ml. Fill up to 100 ml with iso-octane (5.5) and mix. The achieved concentration is given in Table 1. Transport this solution to a brown medicine glass bottle of 100 ml and store it in a refrigerator at 4°C (± 3°C). The solution is tenable under these conditions during at least 5 years if the weight is carefully controled. 5.18.3 Mixed standard solution Toxaphene, 0,5 µg/ml Pipet 5,0 ml of the mixed stock solution Toxaphene (5.17.3) in a volumetric flask of 100 ml. Fill up to 100 ml with iso-octane (5.5) and mix. Transport this solution to a brown medicine glass bottle of 100 ml and store it in a refrigerator at 4°C (± 3°C). The solution is tenable under these conditions during at least 5 years if the weight is carefully controled. 5.18.4 Mixed standard solution PCBs, 0,05 µg/ml Pipet 5,0 ml of the mixed stock solution PCBs (5.17.4) in a volumetric flask of 100 ml. Fill up to 100 ml with iso-octane (5.5) and mix. Transport this solution to a brown medicine glass bottle of 100 ml and store in a refrigerator at 4°C (± 3°C). The solution is tenable under these conditions during at least 5 years if the weight is carefully controled. SIST EN 15742:2009

EN 15742:2009 (E) 11 5.19 Internal standard solutions 5.19.1 PCB 198, 0,1 µg/ml Pipet 5,0 ml PCB 198 standard solution (5.17.5) in a volumetric flask of 100 ml. Fill up with ethylacetat/cyclohexane (5.9) and mix. Transport this solution to a brown medicine glass bottles of 100 ml and store it in a refrigerator at 4°C (± 3°C). The solution is tenable under these conditions during at least 5 years. 5.19.2 PCB 209, 0,1 µg/ml Pipet 5,0 ml PCB 209 standard solution (5.17.6) in a volumetric flask of 100 ml. Fill up with ethylacetat/cyclohexane (5.9) and mix. Transport this solution to a brown medicine glass bottles of 100 ml and store it in a refrigerator at 4°C (± 3°C). The solution is tenable under these conditions during at least 5 y

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