EN 17050-2017 en Animal feeding stuffs Methods of sampling and analysis - Determination of iodine in animal feed by ICP-MS.pdf

1、Animal feeding stuffs: Methods of sampling and analysis - Determination of iodine in animal feed by ICP-MSBS EN 17050:2017BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 17050 September 2017 ICS 65.120 English Vers

2、ion Animal feeding stuffs: Methods of sampling and analysis - Determination of iodine in animal feed by ICP-MS Aliments pour animaux - Mthodes dchantillonnage et danalyse - Dosage de liode dans les aliments pour animaux par spectromtrie de masse plasma induit par haute frquence (ICP-MS) Futtermittel

3、 - Probenahme- und Untersuchungs-verfahren - Bestimmung von Iod in Futtermitteln mittels Anionenaustausch ICP-MS This European Standard was approved by CEN on 28 June 2017. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this Europe

4、an 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 three official versions

5、(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 bodies of Austria, Belg

6、ium, 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, Slovenia, Spain, Sweden

7、, 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 reserved worldwide for CEN

8、national Members. Ref. No. EN 17050:2017 ENational forewordThis British Standard is the UK implementation of EN 17050:2017.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 o

9、n 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 0 580 94204 4ICS 65.120Compliance with a Briti

10、sh Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 September 2017.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS EN 17050:2017EUROPEAN STANDARD NORM

11、E EUROPENNE EUROPISCHE NORM EN 17050 September 2017 ICS 65.120 English Version Animal feeding stuffs: Methods of sampling and analysis - Determination of iodine in animal feed by ICP-MS Aliments pour animaux - Mthodes dchantillonnage et danalyse - Dosage de liode dans les aliments pour animaux par s

12、pectromtrie de masse plasma induit par haute frquence (ICP-MS) Futtermittel - Probenahme- und Untersuchungs-verfahren - Bestimmung von Iod in Futtermitteln mittels Anionenaustausch ICP-MS This European Standard was approved by CEN on 28 June 2017. CEN members are bound to comply with the CEN/CENELEC

13、 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 may be obtained on application to the CEN-CENELEC Management Centre or t

14、o 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 offici

15、al 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, N

16、orway, 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 righ

17、ts of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 17050:2017 EBS EN 17050:2017EN 17050:2017 (E) 2 Contents Page European foreword . 4 1 Scope 5 2 Normative references 5 3 Principle . 5 4 Reagents . 5 4.1 General 5 4.2 Tetra methyl ammonium hydro

18、xide (TMAH (CH3)4N+OH) solution . 5 4.3 Diluted tetra methyl ammonium hydroxide (TMAH) solution . 6 4.4 Stock solutions . 6 4.4.1 General 6 4.4.2 Iodine stock solution (KIO3); = 1 000 mg/l, purity: mass fraction w 99,5 % 6 4.4.3 Tellurium stock solution, = 1 000 mg/l . 6 4.5 Standard solutions 6 4.5

19、.1 Iodine standard solution, = 10 mg/l . 6 4.5.2 Tellurium standard solution (internal standard) . 6 4.6 Iodine calibration solutions 6 4.6.1 General 6 4.6.2 Calibration solution 1 - = 5 g/l 7 4.6.3 Calibration solution 2 - = 20 g/l . 7 4.6.4 Calibration solution 3 - = 50 g/l . 7 4.7 Zero member com

20、pensation solution 7 5 Apparatus and equipment . 7 5.1 General 7 5.2 Containers 7 5.3 Plastic syringes 7 5.4 Membrane filters . 7 5.5 Ultracentrifuge . 8 5.6 Drying oven . 8 5.7 Inductively coupled plasma mass spectrometer (ICP-MS). 8 5.8 Tubes . 8 6 Sampling . 8 6.1 General 8 6.2 Sampling procedure

21、 . 8 7 Procedure. 8 7.1 Sample preparation 8 7.2 Iodine extraction . 8 7.3 Preparation of sample and blank solutions 9 7.4 Determination of iodine by ICP-MS 9 7.4.1 General 9 7.4.2 Preparation of apparatus . 9 7.4.3 Calibration . 9 7.4.4 Determination . 10 8 Calculation 10 BS EN 17050:2017EN 17050:2

22、017 (E) 3 9 Limit of quantification (LOQ) . 10 10 Precision 10 10.1 Inter-laboratory test 10 10.2 Repeatability 10 10.3 Reproducibility 11 11 Test report 11 Annex A (informative) Results of the inter-laboratory test . 12 Bibliography . 15 BS EN 17050:2017EN 17050:2017 (E) 4 European foreword This do

23、cument (EN 17050:2017) 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 text or by endorsement, at the latest by March 2

24、018, and conflicting national standards shall be withdrawn at the latest by March 2018. 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

25、. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association, and supports essential requirements of EU Directive(s). WARNING The method described in this standard implies the use of reagents that pose a hazard to health. The stand

26、ard 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 prior to use of the standard and to ensure that regulatory and legal requirements are complied with.

27、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, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Ger

28、many, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 17050:2017EN 17050:2017 (E) 5 1 Scope This European standard specifies a

29、method for the determination of iodine in animal feeding stuffs by inductively coupled plasma mass spectrometry (ICP-MS) following extraction with an alkaline solution. This method was successfully tested in the range of 0,70 to 631 mg/kg in following animal feeds: seaweed meal, mineral premixture,

30、fish meal, plant based ingredient, marine based compound feed and a synthetic iodine solution. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited appl

31、ies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 15111, Foodstuffs - Determination of trace elements - Determination of iodine by ICP-MS (inductively coupled plasma mass spectrometry) EN ISO 3696, Water for analytical laboratory use -

32、Specification and test methods (ISO 3696) EN ISO 6497, Animal feeding stuffs - Sampling (ISO 6497) EN ISO 6498, Animal feeding stuffs - Guidelines for sample preparation (ISO 6498) 3 Principle This standard describes a method for the determination of iodine in animal feeding stuffs. A representative

33、 test portion of the sample is treated with a strong alkaline solution of tetra methyl ammonium hydroxide (TMAH) and incubated at 90C for three hours. Hereby iodine is extracted into solution and is determined by use of inductively coupled plasma mass spectrometry (ICP-MS). The method principles are

34、 the same as used in EN 15111. WARNING The 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. It is the responsibility of the user of this European Standard to establish a

35、ppropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 4 Reagents Use only reagents of recognized analytical grade and water conforming to grade 2 of EN ISO 3696. 4.1 General The concentration of iodine in the reagents and water used shall be l

36、ow enough not to affect the results of the determination. NOTE Different qualities of tetra methyl ammonium hydroxide (TMAH) are available and it is important to check that the iodine content is sufficiently low and does not affect the analysis. 4.2 Tetra methyl ammonium hydroxide (TMAH (CH3)4N+OH)

37、solution Use mass concentration = 250 g/l, (mass fraction w = 25 %), suitable for trace analysis with an iodine content of less than 1 g/l. BS EN 17050:2017EN 17050:2017 (E) 6 4.3 Diluted tetra methyl ammonium hydroxide (TMAH) solution Dilute TMAH solution for preparing the zero member compensation

38、and calibration solutions with a concentration to suit that of the sample solution (see 7.3). Prepare a 0,5 % TMAH solution by diluting e.g. 1,0 ml of TMAH solution (4.2) to 50 ml with water. 4.4 Stock solutions 4.4.1 General Commercially available standard stock solutions of iodine and tellurium ar

39、e recommended. As an alternative the solutions described below may be used. 4.4.2 Iodine stock solution (KIO3); = 1 000 mg/l, purity: mass fraction w 99,5 % Dissolve 1,686 4 g of potassium iodate in water and dilute to 1 000 ml with water. 4.4.3 Tellurium stock solution, = 1 000 mg/l Dissolve 1,250

40、8 g of tellurium dioxide (TeO2) in 4 mol/l hydrochloric acid (HCl) and dilute to 1 000 ml with water. 4.5 Standard solutions 4.5.1 Iodine standard solution, = 10 mg/l Pipette 1 ml of the iodine stock solution (4.4.2) into a 100 ml volumetric flask and dilute to the mark with water. This solution is

41、stable for about four weeks and is used to prepare the calibration solutions in 4.6. 4.5.2 Tellurium standard solution (internal standard) Prepare e.g. a 10 mg/l standard tellurium solution by pipetting 1 ml of the tellurium stock solution (4.4.3) into a 100 ml volumetric flask and dilute to the mar

42、k with water. This solution is stable for about four weeks. Tellurium is satisfactory as an internal standard for determining iodine since it has a mass in a comparable range and ionization energy similar to that of iodine. The original tellurium content in the sample to be analysed shall be negligi

43、ble. If that is not the case, another suitable internal standard shall be used (e.g. rhodium (Rh). 4.6 Iodine calibration solutions 4.6.1 General The concentrations of the calibration solutions specified below are given as example and may be modified to suit the sensitivity of the apparatus and the

44、concentration range to be covered for the analysis in question. The linear range of the detector system should not be exceeded. The internal standard added to the calibration solutions shall have a concentration high enough to reach a stable detector count rate. The calibration, zero member compensa

45、tion and sample solutions shall contain exactly the same amount of internal standard. The internal standard may be added online. The TMAH concentrations in the calibration solutions shall be approximately equal to that of the sample solutions. The calibration solutions shall be prepared freshly ever

46、y working day. BS EN 17050:2017EN 17050:2017 (E) 7 4.6.2 Calibration solution 1 - = 5 g/l Fill a 50 ml volumetric flask with about 30 ml of diluted TMAH solution (4.3). Pipette 2,5 ml of tellurium standard solution (4.5.2) into the flask and mix. Add 25 l of iodine standard solution (4.5.1) to this

47、mixture and fill to the mark with diluted TMAH solution (4.3). 4.6.3 Calibration solution 2 - = 20 g/l Fill a 50 ml volumetric flask with about 30 ml of diluted TMAH solution (4.3). Pipette 2,5 ml of tellurium standard solution (4.5.2) into the flask and mix. Add 100 l of iodine standard solution (4

48、.5.1) to this mixture and fill to the mark with diluted TMAH solution (4.3). 4.6.4 Calibration solution 3 - = 50 g/l Fill a 50 ml volumetric flask with about 30 ml of diluted TMAH solution (4.3). Pipette 2,5 ml of tellurium standard solution (4.5.2) into the flask and mix. Add 250 l of iodine standa

49、rd solution (4.5.1) to this mixture and fill to the mark with diluted TMAH solution (4.3). 4.7 Zero member compensation solution The zero member compensation solution contains water and the same amount of TMAH and internal standard as the sample solution. Fill a 50 ml volumetric flask with about 30 ml of diluted TMAH solution (4.3). Pipette 2,5 ml of tellurium standard solution (4.5.2) into the flask, mix and fill to the mark with diluted TMAH solution (4.3). 5 Apparatus and equipment 5.1 General To minimize the