EN 15621-2017 en Animal feeding stuffs Methods of sampling and analysis - Determination of calcium sodium phosphorus magnesium potassium sulphur iron zinc copper manganese and coba.pdf

1、Animal feeding stuffs: Methods of sampling and analysis - Determination of calcium, sodium, phosphorus, magnesium, potassium, sulphur, iron, zinc, copper, manganese and cobalt after pressure digestion by ICP-AESBS EN 15621:2017BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/20

2、13 15:06EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15621 August 2017 ICS 65.120 Supersedes EN 15621:2012English Version Animal feeding stuffs: Methods of sampling and analysis - Determination of calcium, sodium, phosphorus, magnesium, potassium, sulphur, iron, zinc, copper, manganese and c

3、obalt after pressure digestion by ICP-AESAliments pour animaux : Mthodes dchantillonnage et danalyse - Dosage du calcium, du sodium, du phosphore, du magnsium, du potassium, du soufre, du fer, du zinc, du cuivre, du manganse et du cobalt aprs digestion sous pression par ICP-AES Futtermittel - Proben

4、ahme- und Untersuchungsverfahren - Bestimmung von Calcium, Natrium, Phosphor, Magnesium, Kalium, Schwefel, Eisen, Zink, Kupfer, Mangan und Kobalt nach Druckaufschluss mittels ICP-AES This European Standard was approved by CEN on 6 February 2017. CEN members are bound to comply with the CEN/CENELEC I

5、nternal 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 may be obtained on application to the CEN-CENELEC Management Centre or to

6、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 the CEN-CENELEC Management Centre has the same status as the official

7、 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, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Nor

8、way, Poland, Portugal, Romania, Serbia, 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

9、 of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15621:2017 ENational forewordThis British Standard is the UK implementation of EN 15621:2017. It supersedes BS EN 15621:2012, which is withdrawn.The UK participation in its preparation was entruste

10、d to Technical Committee AW/10, Animal feeding stuffs.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The Brit

11、ish Standards Institution 2017 Published by BSI Standards Limited 2017ISBN 978 0 580 94543 4ICS 65.120Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 August 2

12、017.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS EN 15621:2017EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15621 August 2017 ICS 65.120 Supersedes EN 15621:2012English Version Animal feeding stuffs: Methods of sampling and analysis - Determination of cal

13、cium, sodium, phosphorus, magnesium, potassium, sulphur, iron, zinc, copper, manganese and cobalt after pressure digestion by ICP-AESAliments pour animaux : Mthodes dchantillonnage et danalyse - Dosage du calcium, du sodium, du phosphore, du magnsium, du potassium, du soufre, du fer, du zinc, du cui

14、vre, du manganse et du cobalt aprs digestion sous pression par ICP-AES Futtermittel - Probenahme- und Untersuchungsverfahren - Bestimmung von Calcium, Natrium, Phosphor, Magnesium, Kalium, Schwefel, Eisen, Zink, Kupfer, Mangan und Kobalt nach Druckaufschluss mittels ICP-AES This European Standard wa

15、s 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 references concerning such n

16、ational 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 CEN member into its own la

17、nguage 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 Macedonia, France, Germany, Gree

18、ce, 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 NORMALISATION EUROPISCHES KOMITEE FR

19、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 15621:2017 EBS EN 15621:2017EN 15621:2017 (E) 2 Contents Page European foreword . 4 1 Scope 5 2 Normative

20、 references 5 3 Terms and definitions . 5 4 Principle . 5 5 Reagents . 6 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 . 8 8.3 Liquid animal feeding stuffs 8 9 Procedure. 8 9.1 Pressure digestion Preparation of

21、 the blank test solution and the test solution . 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 Determination 9 Table 1 Selected emission wavelengths and interferences for determination wit

22、h ICP-AES . 10 10 Calculation and expression of the results . 11 10.1 General . 11 10.2 External calibration 11 10.3 Standard addition method with only one addition 11 10.4 Standard addition method with several additions 12 10.5 Calculation of the element content in the sample 12 11 Precision 13 11.

23、1 Inter-laboratory test . 13 11.2 Repeatability 13 11.3 Reproducibility . 13 Table 2 Precision data Ca, K, Mg, Na, P, S . 14 Table 3 Precision data Co, Cu, Fe, Mn, Mo, Zn, Cd, As, Pb . 17 12 Test report 21 Annex A (informative) Results of the inter-laboratory test . 22 Table A.1 Statistical results

24、of an inter-laboratory test Calcium (Ca) 23 Table A.2 Statistical results of an inter-laboratory test Potassium (K) . 24 Table A.3 Statistical results of an inter-laboratory test Magnesium (Mg) 25 Table A.4 Statistical results of an inter-laboratory test Sodium (Na) . 26 Table A.5 Statistical result

25、s of an inter-laboratory test Phosphorus (P) . 27 BS EN 15621:2017EN 15621:2017 (E) 3 Table A.6 Statistical results of an inter-laboratory test Sulphur (S) 28 Table A.7 Statistical results of an inter-laboratory test Cobalt (Co) 29 Table A.8 Statistical results of an inter-laboratory test Copper (Cu

26、) 30 Table A.9 Statistical results of an inter-laboratory test Iron (Fe). 31 Table A.10 Statistical results of an inter-laboratory test Manganese (Mn) 32 Table A.11 Statistical results of an inter-laboratory test Molybdenum (Mo) . 33 Table A.12 Statistical results of an inter-laboratory test Zinc (Z

27、n) 34 Table A.13 Statistical results of an inter-laboratory test Cadmium (Cd) . 35 Table A.14 Statistical results of an inter-laboratory test Arsenic (As) . 36 Table A.15 Statistical results of an inter-laboratory test Lead (Pb) 37 Annex B (informative) Notes on the detection technique, interference

28、s and quantification, pressure digestion 38 B.1 General . 38 B.2 Interferences 38 B.2.1 General . 38 B.2.2 Spectral line interference 38 B.2.3 Ionization interferences . 38 B.2.4 Physical interferences 38 B.3 Quantification and matrix matching 39 B.3.1 General . 39 B.3.2 Calibration curve 39 B.3.3 M

29、atrix matching 39 B.3.4 Standard addition . 39 B.4 Pressure digestion conditions . 40 B.4.1 General . 40 B.4.2 Initial sample mass and acid volumes. 40 B.4.3 Digestion temperature . 40 B.4.4 Digestion time 40 B.4.5 Digestion solution. 40 B.4.6 Blank solution 40 Bibliography . 41 BS EN 15621:2017EN 1

30、5621:2017 (E) 4 European foreword This document (EN 15621:2017) has been prepared by Technical Committee CEN/TC 327 “Animal 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 p

31、ublication of an identical text or by endorsement, at the latest by February 2018, and conflicting national standards shall 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

32、 be held responsible for identifying any or all such patent rights. This document supersedes EN 15621:2012. WARNING The 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 respons

33、ibility of the user of this standard to take appropriate measures for the health and safety protection of the personnel 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 organ

34、isations of 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,

35、Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 15621:2017EN 15621:2017 (E) 5 1 Scope This European Standard specifies a method for the determination of the elements calcium, sodium, phosphorus, magne

36、sium, potassium, sulphur, iron, zinc, copper, manganese and cobalt in animal feeding stuffs by inductively coupled plasma atomic emission spectrometry (ICP-AES) after pressure digestion. The method was fully statistically tested and evaluated for the elements calcium, sodium, phosphorus, magnesium,

37、potassium, sulphur, iron, zinc, copper, manganese and cobalt within the following 11 animal feeds: 2 complete feeds (pig feed, sheep feed), 3 complementary feeds (3 mineral feeds), 1 mineral premixture, 3 feed materials (MgO, phosphate, CaCO3) and 2 feed additives (CuSO4, bentonite). For elements wi

38、th a HORRAT values higher than 2 (e.g. potassium and sulphur, see Annex A), the method is more applicable as a screening method and not for confirmatory purposes. Other elements like molybdenum, lead, cadmium, arsenic were not fully statistically tested and evaluated within 11 animal feeding stuff s

39、amples because these elements did not occur in concentrations higher than the limit of quantification in most of these samples. A single laboratory validation is therefore necessary for the use of this multi element method for these elements. For the determination of extractable lead in minerals and

40、 feeds, containing phyllosilicates (e.g. kaolinite clay) wet digestion with nitric acid should be used. The method limit of quantification for each element is dependent on the sample matrix as well as on the instrument. The method is not applicable for determination of low concentrations of elements

41、. A limit of quantification of 1 mg/kg should normally be obtained. NOTE 1 This method can also be used for the determination of minerals in products with high mineral content (5 %). For this purpose the accuracy of the method has to be checked individually. Other more matrix-specific analytical tec

42、hniques are also available. NOTE 2 Results using this European Standard EN 15621 may be higher than those obtained when applying EN 15510 as pressure digestion is used in EN 15621. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and ar

43、e indispensable for its application. For 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 649

44、8, Animal feeding stuffs - Guidelines for sample preparation (ISO 6498) 3 Terms and definitions For the purposes of this document the terms and definitions given in the European legislation apply. 4 Principle For the determination of calcium, sodium, phosphorus, magnesium, potassium, sulphur, iron,

45、zinc, copper, manganese, cobalt, molybdenum, lead, cadmium and arsenic a test portion of the sample is digested under pressure. The concentration of the elements is determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) using external calibration or standard addition techniq

46、ue. BS EN 15621:2017EN 15621:2017 (E) 6 5 Reagents Use only reagents of recognized analytical grade, and water conforming to grade 2 of EN ISO 3696. WARNING The use of this European Standard can involve hazardous materials, operations and equipment. This standard does not purport to address all the

47、safety problems associated with its use. It 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 % (m/m), c(HNO3) = 14,4

48、 mol/l, having a density of approximately (HNO3) 1,42 g/ml. 5.2 Nitric acid solution of 2 % (v/v), to be prepared: pipette 20 ml nitric acid concentrated (5.1) in a 1 000 ml volumetric flask (6.4) and fill to the mark with water. 5.3 Hydrogen peroxide, not less than 30 % (m/m). 5.4 Element stock sol

49、utions Ca, Na, P, Mg, K, S, Fe, Zn, Cu, Mn, Co, Mo, Cd, Pb, As c = 1 000 mg/l. The user should choose a suitable stock solution. Both single-element stock solutions and multi-element stock solutions with adequate specification stating the acid used and the preparation technique are commercially available. It is advisable to use certified stock solutions. NOTE Element stock solutions with concentrations different from 1 000 mg/l are also acceptable. 5.5 Standard solutions Depending on