EN 17053-2018 en Animal feeding stuffs Methods of sampling and analysis - Determination of trace elements heavy metals and other elements in feed by ICP-MS (multi-method).pdf

1、BSI Standards Publication WB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06 Animal feeding stuffs: Methods of sampling and analysis - Determination of trace elements, heavy metals and other elements in feed by ICP-MS (multi-method) BS EN 17053:2018 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE

2、 NORM EN 17053 January 2018 ICS 65.120 English Version Animal feeding stuffs: Methods of sampling and analysis - Determination of trace elements, heavy metals and other elements in feed by ICP-MS (multi-method) Aliments des animaux - Mthodes dchantillonnage et danalyse - Dosage par ICP-MS (multimtho

3、de) des lments traces, mtaux lourds et autres lments inorganiques prsents dans les aliments Futtermittel - Probenahme- und Untersuchungsverfahren - Bestimmung von Spurenelementen, Schwermetallen und anderen Elementen in Futtermitteln mittels ICP-MS (Multimethode) This European Standard was approved

4、by CEN on 27 November 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 national st

5、andards 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

6、 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, Greece, Hungar

7、y, 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 NORMUNG CE

8、N-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels 2018 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 17053:2018 E National foreword This British Standard is the UK implementation of EN 17053:2018. The UK particip

9、ation 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. This publication does not purport to include all the necessary provisions of a contract. Users are responsibl

10、e for its correct application. The British Standards Institution 2018 Published by BSI Standards Limited 2018 ISBN 978 0 580 94471 0 ICS 65.120 Compliance with a British Standard cannot confer immunity from legal obligations. This British Standard was published under the authority of the Standards P

11、olicy and Strategy Committee on 28 February 2018. Amendments/corrigenda issued since publication Date Text affected BRITISH STANDARD BS EN 17053:2018 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 17053 January 2018 ICS 65.120 English Version Animal feeding stuffs: Methods of sampling and anal

12、ysis - Determination of trace elements, heavy metals and other elements in feed by ICP-MS (multi-method) Aliments des animaux - Mthodes dchantillonnage et danalyse - Dosage par ICP-MS (multimthode) des lments traces, mtaux lourds et autres lments inorganiques prsents dans les aliments Futtermittel -

13、 Probenahme- und Untersuchungsverfahren - Bestimmung von Spurenelementen, Schwermetallen und anderen Elementen in Futtermitteln mittels ICP-MS (Multimethode) This European Standard was approved by CEN on 27 November 2017. CEN members are bound to comply with the CEN/CENELEC Internal Regulations whic

14、h 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 any CEN member. This Eur

15、opean 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 versions. CEN members a

16、re 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, Norway, Poland, Portugal, R

17、omania, 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: Rue de la Science 23, B-1040 Brussels 2018 CEN All rights of exploitation in

18、any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 17053:2018 E BS EN 17053:2018EN 17053:2018 (E) 2 Contents Page 1 Scope 4 2 Normative references 4 3 Principle . 4 4 Reagents . 5 5 Apparatus . 6 6 Sampling . 6 7 Preparation and preservation of test samples . 6 7.1 Ge

19、neral 6 7.2 Animal feeding stuff, which can be ground as such 7 7.3 Mineral animal feeding stuffs . 7 8 Procedure. 7 8.1 Pressure digestion 7 8.2 Extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay) extraction with diluted nitric acid . 7 8.3 Calibration . 8 8.4 Pr

20、eparation of measurement solutions 8 8.5 Determination 9 8.6 Quality assurance . 12 9 Calculation 12 10 Precision 13 10.1 General . 13 10.2 Repeatability 13 10.3 Reproducibility . 13 11 Test report 13 Annex A (informative) Statistical results of interlaboratory tests (listed by element) . 14 Annex B

21、 (informative) Interferences . 27 B.1 Interferences in ICP-MS . 27 B.2 Technical solutions to overcome interferences 28 Bibliography . 29 BS EN 17053:2018EN 17053:2018 (E) 3 European foreword This document (EN 17053:2018) has been prepared by Technical Committee CEN/TC 327 “Animal feeding stuffs - M

22、ethods 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 July 2018, and conflicting national standards shall be withdrawn at the l

23、atest by July 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 has been prepared under a mandate given to CEN by the European Comm

24、ission and the European Free Trade Association. 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 responsibility of the user of this standard to take appropriate mea

25、sures 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 organisations of the following countries are bound to implement t

26、his 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, Netherlands, Norway, Poland, Portugal, Romania, Serbi

27、a, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 17053:2018EN 17053:2018 (E) 4 1 Scope This European Standard specifies a method for the determination of trace elements, heavy metals and other elements in animal feed by inductively coupled plasma mass spectrome

28、try (ICP-MS). The method is used to determine As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn in the extraction solution after pressurized digestion. For the determination of extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay) wet digestion with nitric acid s

29、hould be used. The method described is suitable for use in quadrupole instruments equipped either with or without additional technology to reduce molecular ion interferences (e.g. collision or reaction technologies) as well as in high-resolution sector-field systems. The method was fully statistical

30、ly tested and evaluated in a collaborative trial comprising eight animal feeding stuff samples for the elements As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn. For elements with a HORRAT value higher than 2 (e.g. mercury, see Annex A) the method is more applicable as a screening method and not

31、 for confirmatory purposes. High-resolution sector-field ICP-MS was not tested in the validation ring trial. The limit of quantification for each element is dependent on the sample matrix as well as the instrument. For the elements Co, Mn, Mo, Pb, Tl, U a limit of quantification of 0,10 mg/kg should

32、 normally be obtained, for the elements Fe and Zn 5,0 mg/kg, while for Cd 0,03 mg/kg, Hg 0,04 mg/kg and As 0,05 mg/kg should normally be quantifiable. Details on the successfully tested working range for each element are described in this standard. 2 Normative references The following documents, in

33、whole or in part, are normatively referenced in this document and are 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 l

34、aboratory use Specification and test methods (ISO 3696) EN ISO 6498, Animal feeding stuffs Guidelines for sample preparation (ISO 6498) 3 Principle For the determination of As, Cd, Co, Cu, Fe, Hg, Mn, Mo, Pb, Se, Tl, U and Zn a test portion of the sample is digested with concentrated nitric acid und

35、er pressure. For the determination of extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay) wet digestion with nitric acid should be used. The concentration of the elements is determined by inductively coupled plasma mass spectrometry (ICP-MS) using external calibra

36、tion or standard addition technique. To reduce occurring mass interferences mathematical correction equations, physical or chemical technical solutions (see B.2) or high-resolution sector-field ICP-MS may be applied. BS EN 17053:2018EN 17053:2018 (E) 5 4 Reagents WARNING The use of this European Sta

37、ndard can involve hazardous materials, operations and equipment. This standard does not purport to address all the 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 applicabil

38、ity of regulatory limitations prior to use. Use only reagents of recognized analytical grade and water conforming to grade 2 of EN ISO 3696. 4.1 Nitric acid concentrated, not less than 65 % (mass fraction), c(HNO 3) = 14,4 mol/l, having a density of approximately (HNO 3) = 1,40 g/ml. 4.2 Nitric acid

39、 solution of 5 % (mass fraction), Pipette 54 ml of nitric acid (4.1) into a 1 000 ml volumetric flask (5.4) and fill to the mark with water. 4.3 Nitric acid solution (rinsing solution), Pipette 20 ml nitric acid (4.1) in a 1 000 ml volumetric flask (5.4). Fill up to the mark with water. 4.4 Hydrochl

40、oric acid concentrated, 30 % (mass fraction), c(HCl) = 9,5 mol/l, having a density of approximately (HCl) = 1,15 g/ml. 4.5 Hydrogen peroxide, not less than 30 % (mass fraction), c(H 2O 2) = 9,7 mol/l, having a density of approximately (H 2O 2) = 1,12 g/ml. 4.6 Single-element and multi-element stock

41、solutions for ICP-MS, = 1 000 mg/l, It is advisable to use certified multi-element stock solutions. Stock solutions with concentrations different from 1 000 mg/l may be used as well. Stock solutions are considered to be stable for several months. 4.7 Calibration solutions, The concentrations of the

42、calibration solutions depend on the element and the estimated concentration levels in the samples. When preparing calibration solutions care should be taken to pipette suitable volumes, intermediate dilution steps are recommended. If calibration solutions are prepared from single-element stock solut

43、ions, it should be checked whether they are chemically compatible and sufficiently pure (specification). Calibration solutions shall be prepared daily. 4.8 Internal standard stock solution, = 1000 mg/l; As internal standard rhodium is recommended. NOTE Alternatively, for low mass elements germanium,

44、 it is advised to use indium or scandium as internal standards. Rhenium, thulium and lutetium are beneficial for the quantification of high mass elements. 4.9 Internal standard working solution, = 1 mg/l, Dilute 1 ml of the internal standard stock solution (4.8) to 1 000 ml with water. 4.10 Gold chl

45、oride stock solution, AuCl 3 (in 10 % HCl), = 10 g Au/l. 4.11 Gold stability solution, = 200 mg Au/l, Place 200 ml of water into a 500 ml volumetric flask (5.4), pipette 250 ml conc. HCl (4.4) and 10,0 ml gold chloride stock solution (4.10) and fill to the mark with water. BS EN 17053:2018EN 17053:2

46、018 (E) 6 5 Apparatus Usual laboratory apparatus and, in particular, the following: 5.1 Laboratory grinder 5.1.1 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. 5.1.2 Laboratory grinder, capable of grinding to a particle si

47、ze of less than or equal to 0,1 mm, e.g. a ball mill or equivalent. Check that the mill used does not influence the concentration of elements in the sample (e.g. adsorption, contamination) which shall be analysed. 5.2 Analytical balance, capable of weighing to an accuracy of 1 mg. 5.3 Pressure diges

48、tion apparatus, capable to reach temperatures above 210 C. The apparatus shall be tested for safety pressure vessels made of acid-resistant materials and having vials for the sample of acid-resistant material with low level of contamination by elements to be determined. Instead of polytetrafluoroeth

49、ylene (PTFE) vials, it is better to use graduated quartz vials, fluorinated ethylene propylene (FEP) vials or perfluoroalkoxy (PFA) vials. Quartz is advisable to be used for decomposition temperatures above 230 C. NOTE The use of a microwave heated pressure digestion apparatus is an option. 5.4 One-mark volumetric flasks; 5.5 Inductively Coupled Plasma Mass Spectrometer (ICP-MS); 5.6 Freeze-drying equipment, capable of freeze-drying liquid animal feeding stuffs; 5.7 Oven for pre-drying, capable to hold a temperature of 70 C 5