EN 15550-2017 en Animal feeding stuffs Methods of sampling and analysis - Determination of cadmium and lead by graphite furnace atomic absorption spectrometry (GF-AAS) after pressu.pdf

1、Animal feeding stuffs: Methods of sampling and analysis - Determination of cadmium and lead by graphite furnace atomic absorption spectrometry (GF-AAS) after pressure digestion BS EN 15550:2017BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06EUROPEAN STANDARD NORME EU

2、ROPENNE EUROPISCHE NORM EN 15550 August 2017 ICS 65.120 Supersedes EN 15550:2007English Version Animal feeding stuffs: Methods of sampling and analysis - Determination of cadmium and lead by graphite furnace atomic absorption spectrometry (GF-AAS) after pressure digestion Aliments des animaux - Mtho

3、des dchantillonnage et danalyse - Dosage du cadmium et du plomb par spectromtrie dabsorption atomique laide dun four graphite aprs minralisation sous pression Futtermittel - Probenahme und Untersuchungsverfahren - Bestimmung von Cadmium und Blei mittels Graphitrohrofen-Atomabsorptionsspektrometrie (

4、GF-AAS) nach Druckaufschluss This European Standard was approved by CEN on 6 February 2017. 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

5、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 exists in three official versions (English, French, German). A version in any other language made by translation un

6、der 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 national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former

7、 Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION

8、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 any means reserved worldwide for CEN national Members. Ref. No. EN 15550:2017 ENational forewordThis British Standard

9、is the UK implementation of EN 15550:2017. It supersedes BS EN 15550:2007, which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee AW/10, Animal feeding stuffs.A list of organizations represented on this committee can be obtained on request to its secretary.Th

10、is publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2017 Published by BSI Standards Limited 2017ISBN 978 0 580 94542 7ICS 65.120Compliance with a British Standard cannot confer imm

11、unity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 August 2017.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS EN 15550:2017EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 1

12、5550 August 2017 ICS 65.120 Supersedes EN 15550:2007English Version Animal feeding stuffs: Methods of sampling and analysis - Determination of cadmium and lead by graphite furnace atomic absorption spectrometry (GF-AAS) after pressure digestion Aliments des animaux - Mthodes dchantillonnage et danal

13、yse - Dosage du cadmium et du plomb par spectromtrie dabsorption atomique laide dun four graphite aprs minralisation sous pression Futtermittel - Probenahme und Untersuchungsverfahren - Bestimmung von Cadmium und Blei mittels Graphitrohrofen-Atomabsorptionsspektrometrie (GF-AAS) nach Druckaufschluss

14、 This European Standard was approved by CEN on 6 February 2017. 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 re

15、ferences concerning such national standards 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

16、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 national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedo

17、nia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATI

18、ON 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 any means reserved worldwide for CEN national Members. Ref. No. EN 15550:2017 EBS EN 15550:2017EN 15550:2017 (E) 2 Contents Page European foreword

19、 . 3 1 Scope 4 2 Normative references 4 3 Terms and definitions . 4 4 Principle . 5 5 Reagents . 5 6 Apparatus . 6 7 Sampling . 7 8 Preparation of the test sample . 7 8.1 General 7 8.2 Animal feeding stuffs which can be ground as such . 7 8.3 Liquid animal feeding stuffs 8 8.3.1 General 8 8.3.2 Pre-

20、drying 8 8.3.3 Freeze-drying . 8 8.4 Mineral matrices . 8 9 Procedure. 8 9.1 Digestion 8 9.1.1 General 8 9.1.2 Pressure digestion 8 9.2 Extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay) extraction with diluted nitric acid . 9 9.3 Calibration . 9 9.4 Determinatio

21、n 9 9.4.1 General 9 9.4.2 Determination by AAS graphite furnace atomic absorption spectrometry 9 10 Calculation and expression of the result . 10 11 Precision 10 11.1 Inter-laboratory test . 10 11.2 Repeatability 10 11.3 Reproducibility . 10 12 Test report 12 Annex A (informative) Results of the int

22、er-laboratory tests . 13 Annex B (informative) Notes on the detection technique, interferences and quantification, and pressure digestion . 16 Bibliography . 18 BS EN 15550:2017EN 15550:2017 (E) 3 European foreword This document (EN 15550:2017) has been prepared by Technical Committee CEN/TC 327 “An

23、imal feeding stuffs: Methods of sampling and analysis”, 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 February 2018, and conflicting national standards s

24、hall be withdrawn at the latest by February 2018. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 15550:2007. WARNING The

25、 method described in this standard implies the use of reagents that pose a hazard to health. The standard does not claim to address all associated safety problems. It is the responsibility of the user of this standard to take appropriate measures for the health and safety protection of the personnel

26、 prior to use of the standard and to ensure that regulatory and legal requirements are complied with. According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia,

27、 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, Sweden, Switzerland, Turkey a

28、nd the United Kingdom. BS EN 15550:2017EN 15550:2017 (E) 4 1 Scope This European Standard specifies a method for the determination of the elements cadmium and lead in animal feeding stuffs by graphite furnace atomic absorption spectrometry (GF-AAS) after pressure digestion. The method was successful

29、ly tested in the range of 0,015 mg/kg to 5,65 mg/kg for Cd and 0,18 mg/kg to 40,3 mg/kg for lead in 11 animal feeds: 2 complete feeds (pig feed, sheep feed), 2 complementary feeds (2 mineral feeds), 1 mineral premixture, 4 feed materials (MgO, 2 phosphates, CaCO3) and 2 feed additives (CuSO4, benton

30、ite). For the determination of extractable lead in minerals and feeds, containing phyllosilicates (e.g. kaolinite clay) wet digestion with diluted nitric acid should be used. The method limit of quantification for each element is dependent on the sample matrix as well as the instrument. For cadmium

31、a limit of quantification of 0,05 mg/kg should normally be obtained while for lead, a limit of quantification of 0,5 mg/kg should be obtained. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. F

32、or dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696) EN ISO 6498, Animal feeding stuffs - Guidelines

33、for sample preparation (ISO 6498) 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 limit of detection (LOD) concentration (mass fraction) derived from the smallest measure that can be detected with reasonable certainty for a given analytical p

34、rocedure Note 1 to entry: xLOD denotes the limit of detection expressed as concentration (mass fraction). SOURCE: ISO 11843-1, see 1 Note 2 to entry: For analytical systems where the validation range does not include or approach it, the detection limit does not need to be part of a validation. SOURC

35、E: IUPAC 2002, see 2 Note 3 to entry: The various conceptual approaches to the subject depend on the estimate of precision at or near zero concentration (mass fraction) under repeatability or reproducibility conditions. BS EN 15550:2017EN 15550:2017 (E) 5 3.2 limit of quantification (LOQ) lowest con

36、centration (mass fraction) determined with satisfactory measurement uncertainty Note 1 to entry: xLOQ denotes the limit of quantification expressed as concentration (mass fraction) SOURCE: ISO 11843-1, see 1 Note 2 to entry: It is useful to state a concentration (mass fraction) below which the analy

37、tical method cannot operate with an acceptable precision. Such precision is arbitrarily defined as relative standard deviation of 10 %. Note 3 to entry: Usually the limit is set as a fixed multiple (e.g. 3.3) of the detection limit. Note 4 to entry: Measurements below LOQ are not devoid of informati

38、on content and are fit for purpose. SOURCE: IUPAC 2002, see 2 3.3 feed additives substances that comply with the definition of feed additives given in the Regulation (EC) No 1831/2003 of the European Parliament and of the Council of 22 September 2003 on additives for use in animal nutrition 3 3.4 an

39、imal feeding stuffs substances that comply with the definition of animal feeding stuffs given in the Regulation (EC) No 178/2002 4 4 Principle For the determination of the elements cadmium and lead, a test portion of the sample is digested under pressure. The concentration of the elements is determi

40、ned by graphite furnace atomic absorption spectrometry (GF-AAS) using external calibration. The method detection limit for each element is dependent on the sample matrix as well as the instrument, the type of atomizer and the use of chemical modifiers. A typical sample volume of 10 l to 20 l is used

41、. 5 Reagents Use only reagents of recognized analytical grade, and water conforming to grade 2 of EN ISO 3696. WARNING 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. I

42、t 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 Nitric acid, concentrated, not less than 65 % (mass fraction), c(HNO3) = 14,4 mol/l, having a density of appr

43、oximately (HNO3) = 1,42 g/ml. 5.2 Hydrogen peroxide, mass fraction not less than 30 %. BS EN 15550:2017EN 15550:2017 (E) 6 5.3 Element stock solutions Cd, Pb c = 1 000 mg/l The user should choose a suitable stock solution. Both single-element stock solutions and multi-element stock solutions with ad

44、equate specifications stating the acid used and the preparation technique are commercially available. It is advisable to use certified stock solutions. Stock solutions should not be used after expiration dates. Element stock solutions with concentrations different from 1 000 mg/l may also be used. 5

45、.4 Calibration solutions Prepare a range of standards including a blank calibration solution, which covers the linear range of the element to be determined by diluting the element stock solutions (5.3). Appropriate matrix matching of the calibration solutions shall be performed (see Annex B), e.g. a

46、djust the acid concentration of the standards to the acid concentration of the samples. Dilute to volume with water. 5.5 Matrix modifier (e.g. Palladium nitrate/magnesium nitrate modifier) Pd(NO3)2solution (Pd-nitrate solution) is commercially available (mass concentration 10 g/l). Dissolve 0,259 g

47、of Mg(NO3)26H20 (Mg-nitrate solution) in 100 ml of water. Mix the Pd-nitrate solution with twice as much Mg-nitrate solution. Ten l of the mixed solution is equal to 15 g Pd and 10 g Mg(NO3)2. It is advisable to use this solution for not longer than one week. NOTE The combination of Pd and Mg(NO3) i

48、s regarded as a “universal” modifier that is used for many elements. Other possible matrix modifiers are e.g. palladium nitrate modifier and ammonium dihydrogen phosphate modifier. 5.6 Purge and protective gas, Argon, Ar purity not less than 99,99 % by volume. 6 Apparatus The usual laboratory appara

49、tus and, in particular, the following should be used: 6.1 Laboratory Grinder 6.1.1 laboratory grinder that is equipped so that samples cannot be contaminated 6.1.2 laboratory grinder capable of grinding to a particle size of less than or equal to 0,5 mm, e.g. a knife mill or equivalent 6.1.3 laboratory grinder capable of grinding to a particle size of less than 0,5 mm or less than 0,1 mm for mineral matrices, e.g. a ball mill or equivalent 6.1.4 mortar with pestle, free of contamination 6.2 Analytical balance, capabl