DIN EN 13804-2013 Foodstuffs - Determination of elements and their chemical species - General considerations and specific requirements German version EN 13804 2013《食品 元素及其化学物种的测定 常.pdf

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1、June 2013 Translation by DIN-Sprachendienst.English price group 11No 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 6

2、7.050!%$lR“2017347www.din.deDDIN EN 13804Foodstuffs Determination of elements and their chemical species General considerations and specific requirements;English version EN 13804:2013,English translation of DIN EN 13804:2013-06Lebensmittel Bestimmung von Elementen und ihren Verbindungen Allgemeines

3、und spezielle Festlegungen;Englische Fassung EN 13804:2013,Englische bersetzung von DIN EN 13804:2013-06Produits alimentaires Dtermination des lments et de leurs espces chimiques Considrations gnrales et exigences spcifiques;Version anglaise EN 13804:2013,Traduction anglaise de DIN EN 13804:2013-06S

4、upersedesDIN EN 13804:2002-09www.beuth.deDocument comprises 17 pagesIn case of doubt, the German-language original shall be considered authoritative.05.13 DIN EN 13804:2013-06 2 A comma is used as the decimal marker. National foreword This document (EN 13804:2013) has been prepared by Technical Comm

5、ittee CEN/TC 275 “Food analysis Horizontal methods” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Lebensmittel und landwirtschaftliche Produkte (Food and Agricultural Products Standards Committee), Working Committee NA 057-01-09 AA Eleme

6、nte und ihre Verbindungen. Amendments This standard differs from DIN EN 13804:2002-09 as follows: a) the standard has been editorially revised; b) the former Clause 3 “Terms and definitions” has been deleted; c) the former Clause 4 “Performance characteristics” has been deleted; d) the former Clause

7、 5 “Sampling” has been deleted; e) the former Clause 6 “Sample preparation” (now Clause 2) has been updated and the wording has been rendered more precise; f) Subclause 2.3.2 “Storage for speciation purposes” has been added; g) Subclause 2.4.2, Table 2 “Examples of sample preparation procedures for

8、some foodstuffs” has been thoroughly updated; h) Subclause 2.4.3 “Drying and lyophilisation” has been added; i) the former Subclause 7.1 “Reagents” has been revised and incorporated in Subclause 3.1; j) the former Clause 8 “Laboratory quality standards” has been completely revised and is now Clause

9、4 “Performance requirements and characteristics”; k) the former Clause 9 “Expression of reults” has been revised and is now Clause 5 “Interpretation and expression of results”; l) the former Clause 10 “Test report” has been rendered more precise and is now Clause 6; m) the Bibliography has been upda

10、ted; n) the standard has been editorially revised. Previous editions DIN EN 13804: 2002-09 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 13804 March 2013 ICS 67.050 Supersedes EN 13804:2002English Version Foodstuffs - Determination of elements and their chemical species - General consideratio

11、ns and specific requirements Produits alimentaires - Dtermination des lments et de leurs espces chimiques - Considrations gnrales et exigences spcifiques Lebensmittel - Bestimmung von Elementen und ihren Verbindungen - Allgemeines und spezielle Festlegungen This European Standard was approved by CEN

12、 on 12 January 2013. CEN members are bound to comply with the CEN/CENELEC 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 standards

13、 may be obtained on application to the CEN-CENELEC 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 translation under the responsibility of a CEN member into its own language and notifi

14、ed to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Icel

15、and, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre

16、: Avenue Marnix 17, B-1000 Brussels 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13804:2013: EEN 13804:2013 (E) 2 Contents Page Foreword . 3 Introduction 4 1 Scope 5 2 Sample preparation 5 3 Specific requirements for analys

17、is of trace elements 9 4 Performance requirements and characteristics . 10 5 Interpretation and expression of results . 13 6 Test report 14 Bibliography 15 DIN EN 13804:2013-06 EN 13804:2013 (E) 3 Foreword This document (EN 13804:2013) has been prepared by Technical Committee CEN/TC 275 “Food analys

18、is - Horizontal methods”, the secretariat of which is held by DIN. 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 September 2013, and conflicting national standards shall be withdrawn at the late

19、st by September 2013. 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 supersedes EN 13804:2002. Compared to EN 13804:200

20、2, the following changes were made: a) the Scope was updated; b) former Clause 3, “Terms and definitions“ was deleted; c) former Clause 4, “Performance characteristics“ was deleted; d) former Clause 5, “Sampling“ was deleted; e) former Clause 6, “Sample preparation“ was updated and wording is now mo

21、re precise and appears in the new Clause 2; f) Subclause 2.3.2, “Storage for speciation purposes“ was added; g) Subclause 2.4.2, Table 2 on “Examples of sample preparation procedures for some foodstuffs“ was thoroughly updated; h) Subclause 2.4.3, “Drying and lyophilisation“ was added; i) Former Sub

22、clause 7.1, “Reagents“ was revised and introduced in 3.1; j) Former Clause 8, “Laboratory Quality standards“ was completely revised and appears now as Clause 4, “Performance requirements and characteristics“; k) Former Clause 9, “Expression of results“ was revised and appears now as Clause 5, “Inter

23、pretation and expression of results“; l) Former Clause 10, “Test report“ was specified and appears now as Clause 6; m) the Bibliographic references were completed; n) the whole document was editorially revised. According to the CEN/CENELEC Internal Regulations, the national standards organisations o

24、f the following countries are bound to implement this European Standard: 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, Net

25、herlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 13804:2013-06 EN 13804:2013 (E) 4 Introduction The Working Group, CEN/TC 275/WG 10 “Elements and their chemical species“, selects and elaborates methods of analysis of e

26、lements and their chemical species in foodstuffs. There are many methods of analysis for the determination of elements in foodstuffs which have been validated and published; the analyst is often required to make a choice between several established methods all of which purport to be applicable to th

27、e same analyte/matrix combination. The Working Group decided to establish specific criteria to guide the analyst in the selection between several methods of analysis. As a general rule, analysts should give preference to methods of analysis which comply with the provisions given in Clauses 1 and 2 o

28、f the annex to 1, with the Decision in 2 and with the General Principles for Methods of Analysis of the Codex Alimentarius Commission (CAC), as defined in the CAC Procedural Manual and further developed in the ”criteria approach“ to methods of analysis developed by the Codex Committee of Methods of

29、Analysis and Sampling (CCMAS). The performance criteria laid down in this European Standard are based on published data or collected from official reports on European interlaboratory studies. When such performance characteristics are not available, the criteria were established based on the experien

30、ce and opinions of the experts of CEN/TC 275/WG 10. The criteria included in this European Standard have also been used as guidance in the Working Group 10 for the selection of specific methods of analysis of trace elements to be standardised. In addition, the Working Group 10 also decided to provid

31、e some general information on sample handling and sample preparation, laboratory organisation and equipment. This document does not deal with sampling issues. It provides an overview of the processes involved from receipt of the laboratory sample to the end result. General sample preparation procedu

32、res are specified, as well as examples for some foodstuffs. DIN EN 13804:2013-06 EN 13804:2013 (E) 5 1 Scope This European Standard specifies performance criteria for the selection of methods of analysis of elements and their chemical species in foodstuffs and contains performance requirements and c

33、haracteristics, guidelines for laboratory set-up, sample preparation and test reports. 2 Sample preparation 2.1 General Food samples are commonly treated in the same way as is done before consumption (washed, peeled, removal of non-edible parts). Apart from the treatments that are just mentioned and

34、 that are clarified in some more detail in 2.4.1 and 2.4.2, samples should not undergo further processing (i.e. samples should not be boiled, steamed, fried, heated or the like). Extra treatments, like drying, may be performed to prevent the sample from decaying. In particular, for speciation analys

35、es, the potential loss or change of analytes shall be considered carefully though. Finally the sample needs to be homogenised (for example by grinding) to obtain a homogenous test portion. Contamination and uncontrolled loss of liquid, e.g. during operations such as grinding and cutting, shall be av

36、oided to the greatest extent possible. 2.2 Reagents, apparatus and equipment No reagents and chemicals other than water shall be used in sample preparation. Water with the quality of drinking water may be used for washing some samples, e.g. vegetables. However, depending on the purpose of the analys

37、is and the element to be determined, it may be necessary to use purified water (see 3.1). Apparatuses and equipment should preferably be designated for trace element analysis. Typical kitchen utensils (e.g. plastic dishes, plastic salad spinner, and coffee grinder) may also be used for sample prepar

38、ation steps as long as they do not affect both the sample and the elements to be determined. Any equipment coming into direct contact with the sample shall, if necessary, be cleaned with detergent and hot water. Equipment cleaned with detergent, and containers for storage of homogenised samples, sho

39、uld be treated with diluted nitric acid (approximately 6 % by volume) followed by purified water, if appropriate. Contamination problems may arise when stainless steel or iron equipment is used for analysis of elements such as chromium, molybdenum, nickel and iron. Special apparatus shall be used in

40、 such cases, e.g. titanium or ceramic knives, agate mortar or ball mill for size reduction and homogenisation. Ceramic materials show a high degree of mechanical and chemical stability, but they might have varying compositions (e.g. Al-oxides, Zr-oxides). Homogenisers shall be chosen carefully as no

41、t to cause losses of volatile elements (e.g. by heating up the sample during mixing) or to cause contamination of the elements to be determined or modification of species (e.g. due to warm-up by friction) in the case of speciation analyses. 2.3 Storage 2.3.1 General Both laboratory samples and test

42、samples shall be stored in such a way that the composition and sample mass does not change as a result of, for instance, drying out, evaporative loss, spoilage or decay. The test sample should be prepared as quickly as possible after arrival of the laboratory sample. Test samples may be stored in a

43、refrigerator or frozen depending on the nature of the material and the expected storage time. Suitable storage material may be made of glass, plastic containers closed with a screw cap or plastic bags. Dry products may be stored at room temperature. DIN EN 13804:2013-06 EN 13804:2013 (E) 6 2.3.2 Sto

44、rage for speciation purposes Some considerations shall be kept in mind when storing samples for speciation purposes. Parameters with a strong influence in speciation analysis are (see Table 1): a) Temperature: Storage temperature shall be low enough to prevent microbial activity resulting in reactio

45、ns, e.g. methylation and biodegradation (see Table 1). b) pH: The pH of the media may strongly affect the stability of the inorganic species. Samples intended for species analysis shall not be changed in their acidity for preservation purposes. c) Light: Light may cause instability of organometallic

46、 compounds by photodegrading. When analysing organometallic compounds storage shall be done in dark or in opaque containers. d) Storage time: Generally, storage should be kept as short as possible. Table 1 Examples of storage conditions for samples intended for speciation purposes Element (species)

47、Storage conditions Hg (Hg(II), methylmercury) Keep samples at 4 C or lower in darkness. Dilution shall be done only immediately before the analysis. Sn (butylated organotin compounds) PVC containers shall not be used to avoid contamination by organotin compounds. Store samples in borosilicate glass

48、bottles in the dark, at least at 4 C or lower. Cr (Cr (III) and Cr (VI) Only borosilicate or quartz glass should be used for handling and storage. Some glassware may cause contamination with chromium. Keep samples at 4 C or lower. The pH has different effect on the stability of Cr (III) and Cr (VI). Se (Se (IV), Se (VI) and methylated compounds) Avoid the use of poly tetra fluoro ethylene containers 3. Keep at -20 C or lower to avoid any change of the inorganic species. Acid media (pH 1,5 to 2) avoid oxidation of Se (IV) to