1、 - STD*BSI BS EM IS0 L4L82-ENGL 2000 1624669 0649682 b72 = BRITISH STANDARD Animal feeding stuffs - Determination of residues of organophosphorus pesticides - Gas chromatographic method The European Standard EN IS0 14182:1999 has the status of a British Standard ICs 65.120 NO COPYING WITHOUT BSI PER
2、MISSION EXCEPT AS PERMITED BY COPYRIGHT LAW BS EN IS0 14182:2000 BS 5766-20:2000 STDmBSI BS EN IS0 l14182-ENGL 2000 I1624669 0847683 505 BS EN IS0 14182:2000 been prepared under the direction of the Consumer AmdNo. Date Products and Semices Sector Committee, was pubiished under the authority of the
3、Standards Committee and comes into effect on 15 June 2000 Q BSI 06-2000 ISBN O 580 34809 1 National foreword Comments This British Standard is the officiai English language version of EN IS0 14182: 1999. It is identid with IS0 141821999. The UK participation in its preparation was entrusted to Techn
4、ical Committee AWAO, Animai feeding stuffs, which has the responsibility to: - aid enquirem to understand the text; - present to the responsible internationallEuropean commime any enquiries on the interpretation, or proposals for change, and keep the UK interests - monitor related international and
5、European developments and promulgate informed, them in the UK A list of oanizations represented on this committee can be obtained on request to its secretary. Cross-references Attention is dram to the fact that CEN and CENELEC Standards normally include an annex which lists nomative references to in
6、ternational publications with their corresponding European publications. The British Standards which implement these international or European publications may be found in the MI Standards Catalogue under the section entitled “InternationaJ Standards Correspondence Index”, or by using the “Find” fac
7、ility of the BSI Standards Electronic Catalogue. A British 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 obliga
8、tions. Summary of pages This document comprises a hnt cover, an inside front cover, the EN IS0 title page, the EN IS0 foreword page, the IS0 title page, pages ii to iv, pages 1 to 18, the annex ZA page and a back cover. The BSI copyright notice displayed in this document indides when the document wa
9、s last issued. STD-BSI BS EN IS0 14182-ENGL 2000 1624667 0849684 445 EUROPEAN STANDARD EN IS0 14182 NORME EUROPENNE EUROPISCHE NORM December 1999 ICs 65.120 English version Animal feeding stuffs - Determination of residues of organophosphorus pesticides - Gas chromatographic method (IS0 14182:1999)
10、Aliments des animaux - Dtermination des rsidus de pesticides organo-phosphors - Mthode par chromatographie en phase gazeuse (IS0 141 82:1999) Futtermittel - Bestimmung von Organophosphorpestizid- Rckstnden - Gaschromatographisches Verfahren (IS0 141 82:1999) This European Standard was approved by CE
11、N on 15 December 1999. CEN members are bound to comply with the CENICENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standar
12、ds may be obtained on application to the Central Secretariat or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to th
13、e Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United
14、Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION EUROPISCHES KOMITEE FR NORMUNG COMITE EUROPEEN DE NORMALISATION Central Secretariat: rue de Stassart, 36 6-1050 Brussels O 1999 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN IS0 141
15、82:1999 E STDaBSI BS EN IS0 14182-ENGL 2000 Lb24bb9 0849b85 381 EN IS0 14182:1999 I Corrected 2000-03-22 Foreword The text of the International Standard from Technical Committee ISOTC 34 “Agricultural food products“ of the International Organization for Standardization (ISO) has been taken over as a
16、n European Standard by Technical Committee CENC 327 “Animal feeding stuffs - Methods of sampling and analysis“, the secretariat of which is held by NNI. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the lates
17、t by June 2000, and conflicting national standards shall be withdrawn at the latest by June 2000. According to the CENKENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark
18、, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard IS0 14182:1999 has been approved by CEN as a European Standard without any modification
19、. NOTE: Normative references to International Standards are listed in annex ZA (normative). STDmBSI BS EN IS0 /4LBZ-ENGL 2000 Lb24bb9 0849b8b 218 EN IS0 14182:1999 INTERNATIONAL IS0 STANDARD 141 82 First edition 1999-1 2-1 5 Animal feeding stuffs - Determination of residues of organophosphorus pesti
20、cides - Gas chromatographic method Aliments des animaux - Dtermination des rsidus de pesticides organo- phosphors - Mthode par chromatographie en phase gazeuse Reference number IS0 14182:1999(E) STD-BSI BS EN IS0 141Z-ENGL 2000 II Lb24669 0847687 154 EN IS0 14182:1999 Contents Page Foreword . iv 1 2
21、 3 4 5 6 7 8 9 10 11 12 Scope 1 Normative references 1 Principle 1 Reagents and materials 1 Apparatus . 3 Sampling . 5 Preparation of test sample 5 Procedure . 6 Expression of results 7 Confirmation of identity 8 Precision . 8 Test report 8 Annex A (informative) Examples of gas chromatographic opera
22、ting conditions for organophosphorus pesticides . 9 Annex B (informative) Results of interlaboratory tests . 10 Bibliography 18 iii STD-BSI BS EN IS0 14182-ENGL 2000 W L624669 0849688 090 EN IS0 14182:1999 Foreword IS0 (the International Organization for Standardization) is a worldwide federation of
23、 national standards bodies (IS0 member bodies). The work of preparing International Standards is normally carried out through IS0 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. Int
24、ernational organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. IS0 collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with t
25、he rules given in the ISOAEC Directives, Part 3. Drafi 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 th
26、e possibility that some of the elements of this International Standard may be the subject of patent rights. IS0 shall not be held responsible for identifying any or all such patent rights. International Standard IS0 14182 was prepared by Technical Committee ISO/TC 34, Agricultural food products, Sub
27、committee SC 10, Animal feeding stuffs. Annexes A and B of this International Standard are for information only. iv STD.BSI BS EN IS0 24282-ENGL 2000 I Lb24bb9 0849689 T27 0 EN IS0 14182:1999 Animal feeding stuffs - Determination of residues of organophosphorus pesticides - Gas chromatographic metho
28、d 1 Scope This International Standard specifies a gas chromatographic method for the determination of the residues of organophosphorus pesticides in animal feeding stuffs. The method is applicable to animal feeding stuffs containing residues of one or more of the following organo- phosphorus pestici
29、des: azinphos-ethyl, azinphos-methyl, bromophos, carbophenothion, chlorpyrifos, chlorpyrifos- methyl, diazinon, dimethoate, ethion, fonofos, malathion, methidathion, parathion, parathion-methyl, pirimiphos-ethyl and pirimiphos-methyl. The lower limit of determination for these organophosphorus pesti
30、cides is 0,Ol pg/g. NOTE fenitrothion, but it has not been validated for these pesticides. The method is probably equally applicable to other organophosphorus pesticides such as methaccrifos and 2 Normative references The following normative documents contain provisions which, through reference in t
31、his text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, 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 m
32、ost recent editions of the normative documents indicated below. For undated references, the latest edition of the normative documents referred to applies. Members of IS0 and IEC maintain registers of currently valid International Standards. IS0 3696, Water for analytical laboratory use - Specificati
33、on and test methods. IS0 6498, Animal feeding stuffs - Preparation of test samples. 3 Principle A test portion is extracted with acetone. The filtered extract is diluted with water and a saturated sodium chloride solution. The pesticides are partitioned in dichloromethane. The concentrated extract i
34、s purified on a chromatographic column of 1 O % water-deactivated silica gel. Gas chromatographic determination is carried out with a phosphorus-selective detector or a mass-selective detector. 4 Reagents and materials Use only reagents of recognized analytical grade and with a purity suitable for p
35、esticide 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. WARNING - Some of the organic solvents are suspected carcinogens. Use with care. 1 STD-BSI BS EN IS0 1418
36、2-ENGL 2000 Lb24bb9 0849690 749 W EN IS0 14182:1999 4.1 Water, complying with at least grade 3 in accordance with IS0 3696. 4.2 Hexane 4.3 Acetone 4.4 Dichloromethane 4.5 Ethyl acetate 4.6 Silica gel, with a mass fraction of water of 10 %. Activate silica gel 60, particle size 63 pm to 200 pm, at 13
37、0 OC overnight and cool in a desiccator. After cooling to room temperature, pour the silica gel into an air-tight glass container and add sufficient distilled water to bring the final mass fraction of water to 10 %. Shake the container mechanically or by hand vigorously for 30 s and allow to stand f
38、or 30 min with occasional shaking. After 30 min the silica gel is ready for use. It may not be stored for more than 6 h. 4.7 Eluting solvent, dichloromethane in hexane (50 % volume fraction). Mix equal volumes of dichloromethane (4.4) and hexane(4.2). 4.8 Inert gas, e.g. nitrogen. 4.9 Sodium sulfate
39、, anhydrous. 4.1 O Sodium chloride saturated solution 4.1 1 Pesticide reference standards, as follows: - azinphos-ethyl S(3,4-dihydro-4-oxobenzol,2,3triazin-3-ylmethyl) O,O-diethyl phosphorodithioate; - azinphos-methyl S(3,4-dihydro-4-oxobenzol,2,3triazinS-ylmethyl) 0,O-dimethyl phosphorodithioate;
40、- bromophos O-4-bromo-2,5-dichlorophenyl O, O-dimethyl phosphorothioate; - carbophenothion S4-chlorophenylthiomethyl 0,O-diethyl phosphorothioate; - chlorpyrifos O,O-diethyl 63,5,6-trichloro-2-pyridyl phosphorothioate; - chlorpyrifos-methyl O, O-dimethyl O-3,5,6-trichloro-2-pyridyl phosphorothioate;
41、 - diazinon O, O-diethyl 02-isopropyl-6-methylpyrmidin-4-yl phosphorothioate; - dimethoate O,O-dimethyl Smethylcarbamoylmethyl phosphorodithioate; - ethion O,O, O, Otetraethyl S,S-methylene di(phosphorodithioate); - fonofos O-ethyl Sphenyl ethylphosphonodithioate; - malathion diethyl (dimethoxythiop
42、hosphorylthio)succinate; - methidathion S2,3-dihydro-5-methoxy-2-oxo-l,3,4-thiadiazol-3-ylmethyl O, O-dimethyl phosphorodithioate; - parathion O,O-diethyl O-4-nitrophenyl phosphorothioate; - parathion-methyl O, O-dimethyl O-4-nitrophenyl phosphorothioate; - pirimiphos-ethyl O-2-diethylamino-6-methyl
43、pyrimidin-4-yl O,O-diethyl phosphorothioate; - pirimiphos-methyl 0-2-diethylamino-6-methylpyrimidin-4-yl 0,Gdimethyl phosphorothioate; NOTE accordance with IS0 1750 l. The common names and the chemical names (between square brackets) according to IUPAC nomenclature, are in 2 STD-BSI BS EN IS0 LLiLBZ
44、-ENGL 2000 3624669 0849693 685 I EN IS0 14182:1999 4.12 Internal standard: tributylphosphate. 4.13 Pesticide standard solutions 4.13.1 Stock solutions, of concentration 1 O00 pg/ml. Prepare a stock solution of each pesticide reference standard (4.1 1) and of the internal standard (4.12) as follows.
45、Weigh, to the nearest 0,l mg, a mass of a pesticide reference standard (4.11) or the internal standard (4.12) which will result in a solution with a content of reference standard or internal standard of 1 O00 pg/ml. While weighing, observe the cleanness of the standard material. Transfer the weighed
46、 mass into a volumetric flasks, dissolve in ethyl acetate (4.5) and dilute to volume with ethyl acetate. These solutions are stable for 6 months when stored at 4 OC in the dark. 4.13.2 Intermediate solutions, of concentration 1 O pg/ml. Pipette 1 ml of each stock solution (4.13.1) into individual 10
47、0 ml volumetric flasks. Dilute to volume with ethyl acetate (4.5). The solutions are stable for 1 month when stored at 4 OC in the dark. NOTE The stability of properly stored pesticide standards is very widely known. Investigations have shown that all neat pesticide standards tested are stable for 1
48、5 years when stored at -18 OC and that stock solutions of pesticide standards in toluene of 1 mgikg are stable for at least 3 years when stored at -1 8 “C. A recommended practice for longer storage is as follows. Transfer portions of the prepared standard solutions to amber vials with PTFE-lined scr
49、ewcaps. Weigh the vials and store at -20 OC. When needed, remove a vial from the freezer, bring to room temperature and weigh. If accumulated 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 1 month (usually in 25 ml vials). Otherwise, the prepared standard solutions (usually in 2 ml vials) may be stored at 4 “C and shall be discarded after
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