1、Animal feeding stuffs - Methods of sampling and analysis - Determination of calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead by ICP-AESBS EN 15510:2017BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06EUROPEA
2、N STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15510 August 2017 ICS 65.120 Supersedes EN 15510:2007English Version Animal feeding stuffs: Methods of sampling and analysis - Determination of calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead
3、by ICP-AES Aliments des animaux - Mthodes dchantillonnage et danalyse - Dtermination des teneurs en calcium, sodium, phosphore, magnsium, potassium, fer, zinc, cuivre, manganse, cobalt, molybdne et plomb par ICP-AES Futtermittel - Probenahme- und Untersuchungsverfahren - Bestimmung von Calcium, Natr
4、ium, Phosphor, Magnesium, Kalium, Eisen, Zink, Kupfer, Mangan, Cobalt, Molybdn und Blei mittels ICP-AES 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 Sta
5、ndard 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 exists in three official versions (Engli
6、sh, 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 national standards bodies of Austria, Belgium, B
7、ulgaria, 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, Sweden, Swit
8、zerland, 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 any means reserved worldwide for CEN nation
9、al Members. Ref. No. EN 15510:2017 ENational forewordThis British Standard is the UK implementation of EN 15510:2017. It supersedes BS EN 15510:2007, which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee AW/10, Animal feeding stuffs.A list of organizations r
10、epresented 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 British Standards Institution 2017 Published by BSI Standards Limited 2017ISBN 978
11、0 580 94541 0ICS 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 2017.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STA
12、NDARDBS EN 15510:2017EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15510 August 2017 ICS 65.120 Supersedes EN 15510:2007English Version Animal feeding stuffs: Methods of sampling and analysis - Determination of calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese,
13、cobalt, molybdenum and lead by ICP-AES Aliments des animaux - Mthodes dchantillonnage et danalyse - Dtermination des teneurs en calcium, sodium, phosphore, magnsium, potassium, fer, zinc, cuivre, manganse, cobalt, molybdne et plomb par ICP-AES Futtermittel - Probenahme- und Untersuchungsverfahren -
14、Bestimmung von Calcium, Natrium, Phosphor, Magnesium, Kalium, Eisen, Zink, Kupfer, Mangan, Cobalt, Molybdn und Blei mittels ICP-AES 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
15、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 exists in th
16、ree 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 national standards b
17、odies 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, Slovakia, S
18、lovenia, 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 any means reser
19、ved worldwide for CEN national Members. Ref. No. EN 15510:2017 EBS EN 15510:2017EN 15510:2017 (E) 2 Contents Page European foreword . 4 1 Scope 5 2 Normative references 5 3 Terms and definitions . 5 4 Principle . 6 5 Reagents . 6 6 Apparatus . 8 7 Sampling . 8 8 Sample preparation 9 8.1 General 9 8.
20、2 Animal feeding stuffs, which can be ground as such 9 8.3 Liquid animal feeding stuffs 9 8.3.1 General 9 8.3.2 Pre-drying 9 8.3.3 Freeze-drying . 9 8.4 Mineral matrices . 9 9 Procedure. 9 9.1 Digestion 9 9.1.1 Selection of the procedure . 9 9.1.2 Extraction with HCl . 10 9.1.3 Dry ashing and extrac
21、tion with HCl 10 9.1.4 Wet digestion with HNO3. 11 9.2 Calibration 11 9.2.1 General . 11 9.2.2 External calibration 11 9.2.3 Standard addition technique . 11 9.2.4 Example of calibration with one addition after dry ashing HCl 11 9.2.5 Example of calibration with one addition after wet digestion 1 %
22、HCl 12 9.2.6 Example of calibration with one addition after wet digestion with HNO3. 12 9.3 Determination . 12 9.3.1 General . 12 9.3.2 Determination by inductively coupled plasma atomic emission spectrometry 12 10 Calculation and expression of the result . 13 10.1 General . 13 10.2 External calibra
23、tion 14 10.3 Standard addition method with only one addition 14 10.4 Standard addition method with several additions 14 10.5 Calculation of the element content in the sample 15 10.6 Example of calculation after standard addition technique with one addition 16 11 Precision 16 11.1 Inter-laboratory te
24、st . 16 11.2 Repeatability 16 11.3 Reproducibility . 16 BS EN 15510:2017EN 15510:2017 (E) 3 12 Test report 20 Annex A (informative) Results of the inter-laboratory test . 21 Annex B (informative) Notes on the detection technique, interferences and quantification 27 B.1 General . 27 B.2 Interferences
25、 27 B.2.1 General . 27 B.2.2 Spectral interferences . 27 B.2.3 Ionization interferences . 27 B.2.4 Physical interferences 27 B.3 Quantification and matrix matching 27 B.3.1 General . 27 B.3.2 Calibration curve 28 B.3.3 Matrix matching 28 B.3.4 Standard addition . 28 Bibliography . 29 BS EN 15510:201
26、7EN 15510:2017 (E) 4 European foreword This document (EN 15510:2017) has been prepared by Technical Committee CEN/TC 327 “Animal feeding stuffs”, 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 te
27、xt 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 be held responsible for iden
28、tifying any or all such patent rights. This document supersedes EN 15510:2007. 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 s
29、tandard 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 organisations of the following cou
30、ntries 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, Netherlands, Norway, P
31、oland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 15510:2017EN 15510:2017 (E) 5 1 Scope This European Standard specifies the inductively coupled plasma atomic emission spectroscopy (ICP-AES) method for the determination of the elem
32、ents calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead. The elements calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum and lead are extracted either in feeds mainly consisting of organic ma
33、tter after dry ashing and dissolving in hydrochloric acid or in feeds mainly consisting of inorganic matter after wet digestion with hydrochloric acid. For the determination of extractable lead in minerals and feeds containing phyllosilicates (e.g. kaolinite clay) wet digestion with diluted nitric a
34、cid should be used. The method was successfully tested for: calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt and molybdenum in the following animal feeding stuffs: 2 complete feeds (pig feed, sheep feed), 1 feed material (phosphate), 1 mineral premixture and 2
35、 complementary feeds (2 mineral feeds), lead in 2 feed materials (phosphate, CaCO3), 2 feed additives (Bentonite, CuSO4), 1 complementary feed (mineral feed) For elements with a HORRAT value higher than 2 (see Annex A) the method is more applicable as a screening method and not for confirmatory purp
36、oses. The method detection limit for each element is dependent on the sample matrix and the instrument. The method is not applicable for the determination of a low concentration of elements. The limit of quantification should be 3 mg/kg or lower. This method also applies for the determination in pro
37、ducts with high element content (5 %). For this purpose the accuracy of the method has to be checked individually. NOTE 1 Results using EN 15550 may be lower than those obtained when applying EN 15621 as pressure digestion is used in EN 15621. 2 Normative references The following documents, in whole
38、 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 labora
39、tory use - Specification and test methods (ISO 3696) EN ISO 6498, Animal feeding stuffs - Guidelines 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) smallest measured content from whi
40、ch it is possible to deduce the presence of the analyte with reasonable statistical certainty Note 1 to entry: The limit of detection is numerically equal to three times the standard deviation of the mean of blank determinations (n 10, were n = number of measures) performed under reproducibility con
41、ditions. BS EN 15510:2017EN 15510:2017 (E) 6 3.2 limit of quantification (LOQ) lowest content of the analyte that can be measured with reasonable statistical certainty Note 1 to entry: If both trueness and precision are constant over a concentration range around the limit of detection, then the limi
42、t of quantification is numerically equal to ten times the standard deviation of the mean of blank determinations (n 10, were n = number of measures) performed under reproducibility conditions. 3.3 feed additives substances that comply with the definition of feed additives given in the Regulation (EC
43、) 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 animal 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 t
44、he elements calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, manganese, cobalt, molybdenum, lead, a test portion of the sample is dry ashed and dissolved in hydrochloric acid for feeds mainly consisting of organic matter or wet digested with hydrochloric acid for feeds mainly c
45、onsisting of inorganic matter. 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 calcium, sodium, phosphorus, magnesium, potassium, iron, zinc, copper, man
46、ganese, cobalt, molybdenum and lead is determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) using external calibration or standard addition technique. 5 Reagents Use only reagents of recognized analytical grade, unless otherwise specified. WARNING Use of this European Stan
47、dard 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 applicabili
48、ty of regulatory limitations prior to use. 5.1 Water, complying with grade 2 as defined in EN ISO 3696. 5.2 Nitric acid, concentrated, not less than 65 % (m/m), having a density of approximately (HNO3) 1,42 g/ml. 5.3 Dilute nitric acid, to be prepared by mixing 1 volume of nitric acid (5.2) with 1 v
49、olume of water. 5.4 Nitric acid solution of 5 % (m/v), to be prepared: pipette 160 ml of dilute nitric acid (5.3) into a 1 000 ml volumetric flask (6.7) and fill to the mark with water. 5.5 Nitric acid solution of 2 % (v/v), to be prepared: pipette 20 ml of nitric acid (5.2) into a 1 000 ml volumetric flask (6.7) and fill to the mark with water. BS EN 15510:2017EN 15510:2017 (E) 7 5.6 Hydrochloric acid, concentrated, not less than 30 % (mass fraction), having a density of approximately (HCl) 1,15 g/ml. 5.7 Dilute hydrochloric acid, t
