DIN EN ISO 15774-2017 Animal and vegetable fats and oils - Determination of cadmium content by direct graphite furnace atomic absorption spectrometry (ISO 15774 2017) German versio.pdf

1、May 2017 English price group 9No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 67.200.10!%eQ;“2664624www.din.deDIN E

2、N ISO 15774Animal and vegetable fats and oils Determination of cadmium content by direct graphite furnace atomic absorption spectrometry (ISO 15774:2017);English version EN ISO 15774:2017,English translation of DIN EN ISO 15774:2017-05Tierische und pflanzliche Fette und le Bestimmung von Cadmium mit

3、 DirektGraphitofenAtomabsorptionsspektrometrie (ISO 15774:2017);Englische Fassung EN ISO 15774:2017,Englische bersetzung von DIN EN ISO 15774:2017-05Corps gras dorigines animale et vgtale Dtermination de la teneur en cadmium par spectromtrie dabsorption atomique four graphite (ISO 15774:2017);Versio

4、n anglaise EN ISO 15774:2017,Traduction anglaise de DIN EN ISO 15774:2017-05SupersedesDIN EN ISO 15774:200202www.beuth.deDocument comprises 12 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.05.17 DIN EN ISO 15774:2017-05 2 A c

5、omma is used as the decimal marker. National foreword This document (EN ISO 15774:2017) has been prepared by Technical Committee ISO/TC 34 “Food products” (Secretariat: AFNOR, France) in collaboration with Technical Committee CEN/TC 307 “Oil seeds, vegetable and animal fats and oils and their by-pro

6、ducts Methods of sampling and analysis” (Secretariat: AFNOR, France). The responsible German bodies involved in its preparation were DIN-Normenausschuss Lebensmittel und landwirtschaftliche Produkte (DIN Standards Committee Food and Agricultural Products) and the Deutsche Gesellschaft fr Fettwissens

7、chaft (German Fat Research Society), Joint Working Committee NA 057-05-05 AA “Joint committee of DIN and DGF for the analysis of fats, oils and products thereof, related and primary products”. The DIN Standard corresponding to the European Standard referred to in this document is as follows: ISO 369

8、6 DIN ISO 3696 Amendments This standard differs from DIN EN ISO 15774:2002-02 as follows: a) milk and milk products (or fat coming from milk and milk products) are now excluded from the scope of the standard; b) the standard has been editorially revised and brought in line with the current rules of

9、presentation. Previous editions DIN EN ISO 15774: 2002-02 National Annex NA (informative) Bibliography DIN ISO 3696, Water for analytical laboratory use Specification and test methods EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 15774 February 2017 ICS 67.200.10 Supersedes EN ISO 15774:2

10、001English Version Animal and vegetable fats and oils - Determination of cadmium content by direct graphite furnace atomic absorption spectrometry (ISO 15774:2017) Corps gras dorigines animale et vgtale - Dtermination de la teneur en cadmium par spectromtrie dabsorption atomique four graphite (ISO 1

11、5774:2017) Tierische und pflanzliche Fette und le - Bestimmung von Cadmium mit Direkt-Graphitofen-Atomabsorptionsspektrometrie (ISO 15774:2017) This European Standard was approved by CEN on 15 February 2017. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate th

12、e 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 standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard

13、 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 the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the nationa

14、l standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia

15、, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2017 CEN All rights of exploitation in any form and by an

16、y means reserved worldwide for CEN national Members. Ref. No. EN ISO 15774:2017 EEuropean foreword .31 Scope . 52 Normative references 53 Terms and definitions . 54 Principle 55 Reagents 56 Apparatus . 67 Procedure. 77.1 General . 77.2 Treatment of samples, vegetable oil and standards . 77.3 Prepara

17、tion of apparatus . 77.4 Determination . 87.4.1 Graphite tube blank . 87.4.2 Vegetable oil . 87.4.3 Calibration of apparatus 87.4.4 Oil (liquid) samples . 87.4.5 Fat samples with melting point 40 C and higher . 87.4.6 Number of determinations 98 Expression of results 99 Precision . 99.1 Interlaborat

18、ory test. 99.2 Repeatability . 99.3 Reproducibility . 910 Test report . 9Annex A (informative) Results of interlaboratory test . 10Contents PageDIN EN ISO 15774:2017-05 EN ISO 15774:2017 (E)2Foreword 4European foreword This document (EN ISO 15774:2017) has been prepared by Technical Committee ISO/TC

19、 34 “Food products” in collaboration with Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats and oils and their by-products - Methods of sampling and analysis” the secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either

20、by publication of an identical text or by endorsement, at the latest by August 2017, and conflicting national standards shall be withdrawn at the latest by August 2017. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CE

21、NELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 15774:2001. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Be

22、lgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Swed

23、en, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 15774:2017 has been approved by CEN as EN ISO 15774:2017 without any modification. DIN EN ISO 15774:2017-05 EN ISO 15774:2017 (E) 3 ForewordISO (the International Organization for Standardization) is a worldwide feder

24、ation of national standards bodies (ISO member 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 commit

25、tee. International organizations, governmental 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.The procedures used to develop this document and

26、those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part

27、2 (see www .iso .org/ directives).Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of t

28、he document will be in the Introduction and/or on the ISO list of patent declarations received (see www .iso .org/ patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific

29、terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www .iso .org/ iso/ foreword .html.This document was prepared by Technical Committee IS

30、O/TC 34, Food products, Subcommittee SC 11, Animal and vegetable fats and oils.This second edition cancels and replaces the first edition (ISO 15774:2000), which has been technically revised to exclude its applicability for fat coming from milk and milk products.DIN EN ISO 15774:2017-05 EN ISO 15774

31、:2017 (E)4 1 ScopeThis document describes a method for the determination of trace amounts (micrograms per kilogram) of cadmium in all types of crude or refined edible oils and fats.Milk and milk products (or fat coming from milk and milk products) are excluded from the scope of this document.2 Norma

32、tive referencesThe following documents are referred to in the text in such a way that some or all of their content constitutes requirements of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any ame

33、ndments) applies.ISO 3696, Water for analytical laboratory use Specification and test methods3 Terms and definitionsNo terms and definitions are listed in this document.ISO and IEC maintain terminological databases for use in standardization at the following addresses: IEC Electropedia: available at

34、 h t t p :/ www .electropedia .org/ ISO Online browsing platform: available at h t t p :/ www .iso .org/ obp4 PrincipleThe oil or fat is incinerated and atomized in a suitable graphite tube furnace with a platform connected to an atomic absorption spectrometer, previously calibrated using standard s

35、olutions of an organo-compound of cadmium. The metal content is determined from the observed absorption at a wavelength of 228,8 nm. Palladium is added as a matrix modifier in order to prevent loss of cadmium during the thermal pretreatment.5 ReagentsUse only reagents of recognized analytical grade,

36、 unless otherwise specified.5.1 Water, of grade 1 according to ISO 3696.5.2 Cyclohexane.5.3 Hydrochloric acid.5.4 Palladium chloride.DIN EN ISO 15774:2017-05 EN ISO 15774:2017 (E) 5 5.5 Matrix modifier, 0,1 % (mass/volume) palladium solution.Dissolve 0,167 g of palladium chloride (5.4) in 50 ml wate

37、r (5.1) in a 100 ml volumetric flask (6.4), adding 1 ml hydrochloric acid (5.3) and making up to volume with water.5.6 Vegetable oil, refined.Any liquid edible oil is suitable. It shall be stored in a metal-free polyethylene bottle. The cadmium content of the oil shall not be greater than 0,2 g/kg.5

38、.7 Organometallic cadmium standard, e.g. Conostan, 5 000 mg/kg1).5.8 Standard stock solution, of concentration 10 mg/kg cadmium, prepared by diluting 200 mg of the organometallic standard (5.7) with 100 g of vegetable oil (5.6).5.9 Standard working solutionsPrepare daily working solutions containing

39、 2,5 g/kg, 5,0 g/kg and 10,0 g/kg of cadmium by diluting 25 mg, 50 mg and 100 mg, respectively, of the stock solution (5.8) with 100 g of vegetable oil (5.6).5.10 Argon, of 99,99 % minimum purity.6 Apparatus6.1 Polyethylene or polypropylene bottles, of capacities 20 ml and 50 ml, metal free, with ca

40、ps.The bottles are made metal free in the following way. Clean the bottles thoroughly with warm nitric acid (2 mol/l). Rinse with distilled water and dry the bottles in a dust-free drying oven at about 80 C.6.2 Micropipettor, to deliver 10 l and 20 l.6.3 Pipettor tips.6.4 Volumetric flask, of capaci

41、ty 100 ml.6.5 Electric oven, capable of being maintained at 60 C 2 C.6.6 Atomic absorption spectrometer, equipped with “peak area” mode and “autocalibrate” mode, together with an appropriate electrode-less discharge lamp (or hollow cathode lamp) and deuterium background corrector (or Zeeman atomic a

42、bsorption spectrometer).6.7 Graphite furnace atomizer, placed in the atomic absorption spectrometer (6.6), equipped with a control unit for temperature programming.6.8 Graphite tube, uncoated.6.9 Platform, pyrolytic.1) Conostan, available from Continental Oil Company, Ponca City, Oklahoma, USA, is a

43、n example of a suitable product available commercially. This information is given for the convenience of users of this document and does not constitute an endorsement by ISO of this product. Equivalent products may be used if it can be shown that they lead to the same results.DIN EN ISO 15774:2017-0

44、5 EN ISO 15774:2017 (E)6 6.10 Autosampler for graphite furnace atomizer (optional), with polyethylene sample cups.To use an autosampler equipped with a heating device, regulated at 60 C 10 C, fill sample cups with vegetable oil (5.6), standard working solutions (5.9) and oil samples. Fat samples wit

45、h a melting point of 40 C and higher shall be diluted 1:1 (by mass) with blank oil (5.6). The volume of sample injected shall be 15 l.To use an autosampler with no heating device, dilute 1:1 (mass/volume) the vegetable oil (5.6), the standard working solutions (5.9) and oil or fat samples with an or

46、ganic solvent e.g. cyclohexane (5.2) at ambient temperature. The volume of sample injected shall be 20 l.The use of an organic solvent e.g. cyclohexane (5.2) as a rinse for the autosampler is required.7 Procedure7.1 GeneralEnvironmental dust may contribute to background contamination. It is recommen

47、ded that the analyses be carried out in a dust-free environment.7.2 Treatment of samples, vegetable oil and standards7.2.1 Place all samples, standard working solutions (5.9) and vegetable oil (5.6) in the oven (6.5) set at 60 C.If an autosampler is used, dilute 1:1 (mass/volume) all solutions (vege

48、table oil, standard working solutions, samples) with an appropriate solvent e.g. cyclohexane (5.2). Homogenize well before pouring the solution into the sample cups of the autosampler.7.2.2 Shake the samples vigorously if the metal content of a sample is known to be outside the given range (5.9). Dilute (by mass) with vegetable oil (5.6).7.3 Preparation of apparatus7.3.1 Switch on the atomic absorption spectrometer and the b