1、BRITISH STANDARD BS 5766-22:2001 BS EN ISO 14181:2001 Methods for analysis of animal feeding stuffs Part 22: Determination of residues of organochlorine pesticides Gas chromatographic method The European Standard EN ISO 14181:2000 has the status of a British Standard ICS 07.100.30; 65.120 NO COPYING
2、 WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS 5766-22:2001 This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Committee, was published under the authority of the Standards Committee and comes into effect on 15 May 2001 BSI 05
3、-2001 ISBN 0 580 37279 0 National foreword This British Standard is the official English language version of EN ISO 14181:2000. It is identical with ISO 14181:2000. The UK participation in its preparation was entrusted to Technical Committee AW/10, Animal feeding stuffs, which has the responsibility
4、 to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally include an annex which lists normative references to international publications with their corresponding Eur
5、opean publications. The British Standards which implement these international or European publications may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A B
6、ritish Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; presen
7、t to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an in
8、side front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii to iv, pages 1 to 20, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Dat
9、e CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO14181 September2000 ICS06.012 Englishversion AnimalfeedingstuffsDeterminationofresiduesof organochlorinepesticidesGaschromatographicmethod(ISO 14181:2000) AlimentsdesanimauxDterminationdesrsidusde pesticidesorganochlorsMthodeparchromatogr
10、aphie enphasegazeuse(ISO14181:2000) FuttermittelBestimmungdesGehaltsan OrganochlorpestizidRckstnden GaschromatographischesVerfahren(ISO14181:2000) ThisEuropeanStandardwasapprovedbyCENon15September2000. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivin
11、gthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyoth
12、erlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Net
13、herlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2000CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers.
14、Ref.No.ENISO14181:2000EForeword ThetextoftheInternationalStandardISO14181:2000hasbeenpreparedbyTechnical CommitteeISO/TC34“Agriculturalfoodproducts“incollaborationwithTechnicalCommittee CEN/TC327“AnimalfeedingstuffsMethodsofsamplingandanalysis“,thesecretariatof whichisheldbyNEN. ThisEuropeanStandard
15、shallbegiventhestatusofanationalstandard,eitherbypublication ofanidenticaltextorbyendorsement,atthelatestbyMarch2001,andconflictingnational standardsshallbewithdrawnatthelatestbyMarch2001. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsof thefollowingcountriesareboundt
16、oimplementthisEuropeanStandard:Austria,Belgium, CzechRepublic,Denmark,Finland,France,Germany,Greece,Iceland,Ireland,Italy, Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandtheUnited Kingdom. NOTEFROMCEN/CS:Theforewordissusceptibletobeamendedonreceptionofthe Germanlanguageversion.The
17、confirmedoramendedforeword,andwhenappropriate,the normativeannexZAforthereferencestointernationalpublicationswiththeirrelevant EuropeanpublicationswillbecirculatedwiththeGermanversion. Endorsementnotice ThetextoftheInternationalStandardISO14181:2000wasapprovedbyCENasaEuropean Standardwithoutanymodif
18、ication. ENISO14181:2000 Reference number ISO 14181:2000(E) INTERNATIONAL STANDARD ISO 14181 First edition 2000-09-15 Animal feeding stuffs Determination of residues of organochlorine pesticides Gas chromatographic method Aliments des animaux Dtermination des rsidus de pesticides organochlors Mthode
19、 par chromatographie en phase gazeuse ENISO14181:2000 ii ENISO14181:2000 ISO 18141:(0002)Eiii Contents Page Foreword.iv 1 Scope 1 2 Normative references 1 3 Principle1 4 Reagents and materials 1 5 Apparatus .3 5.1 Grinder 5 6 Sampling.5 7 Preparation of test sample5 8 Procedure .5 8.1 General5 8.2 T
20、est portion 5 8.3 Extraction .5 8.4 Column clean-up6 8.5 Gas chromatography.6 9 Expression of results 7 9.1 Calculation7 9.2 Recovery.8 10 Confirmation of identity 8 11 Precision.8 11.1 Interlaboratory test 8 11.2 Repeatability.8 11.3 Reproducibility.8 12 Test report 9 Annex A (informative) Examples
21、 of GC operating conditions for organochlorine pesticides10 Annex B (informative) Results of interlaboratory test.11 Bibliography20 ENISO14181:2000 ISO 18141:(0002)E iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO membe
22、r bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmenta
23、l and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directi
24、ves, Part 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the eleme
25、nts of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 14181 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 10, Animal feeding stuffs. Annexes A
26、 and B of this International Standard are for information only. ENISO14181:2000 INTENRATIONAL TSANDADR ISO 18141:(0002)E1 Animal feeding stuffs Determination of residues of organochlorine pesticides Gas chromatographic method 1 Scope This International Standard specifies a gas chromatographic method
27、 for the determination of residues of organochlorine pesticides in animal feeding stuffs. The method is applicable to animal feeding stuffs containing residues of one or more of the following organochlorine pesticides and some of their isomers and degradation products: aldrin, op-DDE, pp-DDE, op-DDT
28、, pp-DDT, dieldrin, endosulfan, endrin, HCB, -HCH ( -BHC), -HCH ( -BHC), -HCH ( -BHC), -HCH ( -BHC), heptachlor, heptachlor epoxide, op-TDE (op-DDD), pp-TDE (pp-DDD) and methoxychlor. The lower determination limit for these organochlorine pesticides is 0,005 g/g. However, the lower determination lim
29、it is 0,01 g/g for op-DDT and pp-DDT, and 0,05 g/g for methoxychlor. 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions o
30、f, any of these publications do not apply. However, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent edition of the normative document indicated below. For undated references, the latest edition of the normative docu
31、ments referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 3696:1987, Water for analytical laboratory use Specification and test methods. ISO 6498, Animal feeding stuffs Preparation of test samples. 3P r i n c i p l e A test portion is extrac
32、ted with acetone. The filtered extract is diluted with water and saturated sodium chloride solution. The pesticides are partitioned into dichloromethane. The concentrated extract is purified on a chromatographic column of 10 % water-deactivated silica gel. The pesticide residues are determined by ga
33、s chromatography using an electron capture detector or a mass selective detector. 4 Reagents and materials Use only reagents of recognized analytical grade and with a purity suitable for pesticide residue analysis. Check the purity of the reagents by performing a blank test under the same conditions
34、 as used in the method. The chromatogram should not show any interfering impurity. WARNING Some of the organic solvents are suspected carcinogens. Use with care. 4.1 Water, complying with at least grade 3 in accordance with ISO 3696. ENISO14181:2000 ISO 18141:(0002)E 2 4.2 Hexane. 4.3 Acetone. 4.4 D
35、ichloromethane. 4.5 Silica gel 60, with a mass fraction of water of 10 %. Activate silica gel 60, particle size 63 mt o2 0 0 m, at 130 C overnight, then cool in a desiccator. After cooling to room temperature, pour the silica gel into an airtight glass container and add sufficient distilled water to
36、 bring the final mass fraction of water to 10 %. Shake the container mechanically or by hand vigorously for 30 s and allow to stand for 30 min with occasional shaking. After 30 min the silica gel is ready for use. It should not be stored for mo reth a n6h . 4.6 Eluting solvent: dichloromethane in he
37、xane, 20 % (by volume). Mix 1 volume of dichloromethane with 4 volumes of hexane. 4.7 Inert gas, for example nitrogen. 4.8 Sodium sulfate, anhydrous. 4.9 Sodium chloride, saturated solution. 4.10 Pesticide reference standards, as follows: aldrin (1R,4S,4aS,5S,8R,8aR)-1,2,3,4,10,10-hexachloro-1,4,4a,
38、5,8,8a-hexahydro-1,4:5,8-dimethano- naphthalene; op-DDE o,p-(1,1-dichloro-2,2-bis(4-chlorophenyl) ethylene); pp-DDE p,p-(1,1-dichloro-2,2-bis(4-chlorophenyl) ethylene); op-DDT o,p-(1,1,1-trichloro-2,2-bis(4-chlorophenyl) ethane); pp-DDT p,p-(1,1,1-trichloro-2,2-bis(4-chlorophenyl) ethane); dieldrin
39、(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; endosulfan (6,7,8,9,10,10-hexachloro-1,5,5a,6,9,9a-hexahydro-6,9-methano-2,4,3-benzodioxathiepin 3-oxide); endrin (1R,4S,4aS,5S,6S,7R,8R,8aR)-1,2,3,4,10,10-hexachloro-1,4,4a,5,6,7
40、,8,8a-octahydro-6,7-epoxy- 1,4:5,8-dimethanonaphthalene; HCB (hexachlorobenzene); -HCH ( -BHC) ( -1,2,3,4,5,6-hexachlorocyclohexane); -HCH ( -BHC) ( -1,2,3,4,5,6-hexachlorocyclohexane); -HCH ( -BHC; lindane) ( -1,2,3,4,5,6-hexachlorocyclohexane); -HCH ( -BHC) ( -1,2,3,4,5,6-hexachlorocyclohexane); h
41、eptachlor (1,4,5,6,7,8,8-heptachloro-3a,4,7,7a-tetrahydro-4,7-methanoindene); heptachlor epoxide (heptachloroepoxy-tetrahydromethanoindene); ENISO14181:2000 ISO 18141:(0002)E3 op-TDE (op-DDD) o,p-1,1-dichloro-2,2-bis(4-chlorophenyl) ethane; pp-TDE (pp-DDD) p,p-1,1-dichloro-2,2-bis(4-chlorophenyl) et
42、hane; methoxychlor 1,1,1-trichloro-2,2-bis(4-methoxyphenyl) ethane. 4.11 Internal standard: mirex (1,3,5-tribromobenzene) or pentachloronitrobenzene. 4.12 Pesticide standard and internal standard solutions. 4.12.1 Stock solutions, of concentration 1 000 g/ml. Prepare a stock solution of each pestici
43、de reference standard (4.10) and of the internal standard (4.11) as follows. Weigh, to the nearest 0,1 mg, a mass of a pesticide reference standard (4.10) or the internal standard (4.11) which will result in a solution with a content of reference standard or internal standard of 1 000 g/ml. While we
44、ighing, observe the cleanness of the standard matrial. Transfer the weighed mass into a volumetric flask, dissolve in hexane or in an other solvent such as toluene or iso octane. However, dissolve -HCH in acetone. Dilute to volume with the same solvent and mix well. These solutions are stable for 6
45、months when stored at 4 Cinth eda r k. 4.12.2 Intermediate solutions, of concentration 10 g/ml. Pipette 1 ml of each stock solution (4.12.1) into individual 100 ml volumetric flasks. Dilute to volume with hexane. The solutions are stable for at least 3 months when stored at 4 C in the dark. NOTE The
46、 stability of properly stored pesticide standards is very widely known. Investigations have shown that all neat pesticide standards tested are stable for 15 years when stored at 18 C and that stock solutions of pesticide standards in toluene of 1mg/ml are stable for at least 3 years when stored at 1
47、8 C. The following recommended practice may be used for longer storage. Transfer portions of the prepared standard solutions to amber vials with PTFE-lined screwcaps. Weigh the vials and store at 20 C. When needed, remove a vial from the freezer, bring to room temperature and weigh. If the accumulat
48、ed loss in mass due to evaporation is 10 % or more of the prefrozen net mass, discard the vial. Weigh and refreeze stock standards and intermediate solutions that are in use for more than 3 months (usually in 25 ml vials). Otherwise the prepared standard solutions (usually in 2 ml vials) may be stored at 4 C an
