EN 16963-2018 en Fertilizers - Determination of boron cobalt copper iron manganese molybdenum and zinc using ICP-AES.pdf

1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Fertilizers Determination of boron, cobalt, copper, iron, manganese, molybdenum and zinc using ICP-AESBS EN 16963:2018National forewordThis British Standard is the UK implementation of EN 16963:2018.The UK participation

2、 in its preparation was entrusted to Technical Committee CII/37, Fertilisers and related chemicals.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 resp

3、onsible for its correct application. The British Standards Institution 2018 Published by BSI Standards Limited 2018ISBN 978 0 580 91786 8ICS 65.080Compliance with a British Standard cannot confer immunity from legal obligations. This British Standard was published under the authority of the Standard

4、s Policy and Strategy Committee on 28 February 2018.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS EN 16963:2018EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 16963January 2018ICS 65.080EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPIS

5、CHES KOMITEE FR NORMUNGCEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2018 CEN Ref. No. EN 16963:2018: EAll rights of exploitation in any form and by any means reserved worldwide for CEN national MembersFertilizers Determination of boron, cobalt, copper, iron, manganese, molybdenum

6、 and zinc using ICP-AESEngrais Dosage du bore, du cobalt, du cuivre, du fer, du manganse, du molybdne et du zinc par ICP-AESDngemittel Bestimmung von Bor, Cobalt, Kupfer, Eisen, Mangan, Molybdn und Zink mit ICP-AESThis European Standard was approved by CEN on 15 October 2017.CEN members are bound to

7、 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 standards may be obtained on application to the CEN-CE

8、NELEC 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 notified to the CEN-CENELEC Management Centre has th

9、e 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, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembo

10、urg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.English VersionEN 16963:2018 (E)European forewordThis document (EN 16963:2018) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming mat

11、erials”, the secretariat of which is held by DIN.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 latest by July 2018.Attenti

12、on 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 Commission and the European Free

13、 Trade Association.According to the CEN-CENELEC Internal Regulations, the national standards organizations 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 Mac

14、edonia, France, Germany, 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.2BS EN 16963:2018EN 16963:2018 (E)IntroductionThe preparation

15、 of this document is based on a mandate given to CEN by the European Commission and the European Free Trade Association (Mandate M/335) concerning the modernization of methods of analysis of fertilizers in the framework of Regulation (EC) No 2003/2003 1.This document is part of a modular approach an

16、d concerns the analytical measurement step. “Modular” means that a test standard concerns a specific step in assessing a property and not the whole chain of measurements. Inductively coupled plasma atomic emission spectrometry (ICP-AES) is nowadays widely used and well established in many laboratori

17、es. The European Standard can be used for determination of boron, cobalt, copper, iron, manganese, molybdenum and zinc in all extracts prepared according to EN 16962 and EN 16964. The method can be applied to mineral fertilizers with micro-nutrient contents of 10 % as well as contents of 10 %.The in

18、ter-laboratory study reflects the final properties of the method for determination of individual micro-nutrients in water and aqua regia extracts including extraction steps.WARNING Persons using this European Standard should be familiar with normal laboratory practice. This European Standard does no

19、t purport to address all of the safety issues, if any, associated with its use. It is the responsibility of the user to establish appropriate health and safety practices and to ensure compliance with any national regulatory conditions.IMPORTANT It is absolutely essential that tests conducted accordi

20、ng to this European Standard are carried out by suitably trained staff.3BS EN 16963:2018EN 16963:2018 (E)European foreword 2Introduction . 3European foreword 5Introduction . 61 Scope . 72 Normative references 73 Terms and definitions . 74 Principle 75 Interferences 75.1 General . 75.2 Spectral inter

21、ferences . 75.3 Transport interferences 85.4 Excitation interferences 85.5 Chemical interferences 85.6 Memory interferences 86 Reagents 87 Apparatus . 97.1 Common laboratory glassware. 97.2 Inductively coupled plasma optical emission spectrometer. 98 Procedure. 98.1 Preparation of test and blank sol

22、ution . 98.2 Preparation of the calibration solutions 108.3 Measurement . 108.3.1 Instrument conditions .108.3.2 Optimization of the instrument conditions .108.3.3 Interferences 118.3.4 Matrix effects118.3.5 Spiking . 119 Calculation and expression of the results .1210 Precision 1310.1 Inter-laborat

23、ory tests . 1310.2 Repeatability 1310.3 Reproducibility 1311 Test report 16Annex A (informative) Statistical results of the inter-laboratory test 17Bibliography .264Contents PageBS EN 16963:2018EN 16963:2018 (E)European forewordThis document (EN 16963:2018) has been prepared by Technical Committee C

24、EN/TC 260 “Fertilizers and liming materials”, the secretariat of which is held by DIN.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 withdra

25、wn at the latest 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 Euro

26、pean Commission and the European Free Trade Association.According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Fin

27、land, 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 and the United Kingdom.5BS EN 16963:2018EN 1696

28、3:2018 (E)IntroductionThe preparation of this document is based on a mandate given to CEN by the European Commission and the European Free Trade Association (Mandate M/335) concerning the modernization of methods of analysis of fertilizers in the framework of Regulation (EC) No 2003/2003 1.This docu

29、ment is part of a modular approach and concerns the analytical measurement step. “Modular” means that a test standard concerns a specific step in assessing a property and not the whole chain of measurements. Inductively coupled plasma atomic emission spectrometry (ICP-AES) is nowadays widely used an

30、d well established in many laboratories. The European Standard can be used for determination of boron, cobalt, copper, iron, manganese, molybdenum and zinc in all extracts prepared according to EN 16962 and EN 16964. The method can be applied to mineral fertilizers with micro-nutrient contents of 10

31、 % as well as contents of 10 %.The inter-laboratory study reflects the final properties of the method for determination of individual micro-nutrients in water and aqua regia extracts including extraction steps.WARNING Persons using this European Standard should be familiar with normal laboratory pra

32、ctice. This European Standard does not purport to address all of the safety issues, if any, associated with its use. It is the responsibility of the user to establish appropriate health and safety practices and to ensure compliance with any national regulatory conditions.IMPORTANT It is absolutely e

33、ssential that tests conducted according to this European Standard are carried out by suitably trained staff.6BS EN 16963:2018EN 16963:2018 (E)1 ScopeThis European Standard specifies a method for the determination of boron, cobalt, copper, iron, manganese, molybdenum and zinc in fertilizer extracts u

34、sing inductively coupled plasma-atomic emission spectrometry (ICP-AES).This method is applicable to water and aqua regia fertilizer extracts prepared according to EN 16962 and/or EN 16964.NOTE In most cases, the presence of small quantities of organic matter will not affect determinations by ICP-AES

35、 and it is not necessary to apply organic matter removal.2 Normative referencesThe 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 applies. For undated references, the latest

36、 edition of the referenced document (including any amendments) applies.EN 12944-1, Fertilizers and liming materials and soil improvers Vocabulary Part 1: General termsEN 12944-2, Fertilizers and liming materials and soil improvers Vocabulary Part 2: Terms relating to fertilizersEN 16962, Fertilizers

37、 Extraction of water soluble micro-nutrients in fertilizers and removal of organic compounds from fertilizer extractsEN 16964, Fertilizers Extraction of total micro-nutrients in fertilizers using aqua regiaEN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696)3 Te

38、rms and definitionsFor the purposes of this document, the terms and definitions given in EN 12944-1 and EN 12944-2 apply.4 PrincipleThe method is based on the ICP-AES measurement of the concentration of boron, cobalt, copper, iron, manganese, molybdenum and zinc in fertilizer extracts prepared accor

39、ding to EN 16962 or EN 16964. The elements are determined after appropriate dilution of the extract. The solution is dispersed by a nebulizer of the ICP-AES instrument and the resulting aerosol is transported into the plasma. Element specific emission spectra are produced by a radio-frequency induct

40、ively coupled argon plasma where atoms or ions are excited at high temperature. The emission spectra are dispersed by a spectrometer, and the intensities of the emission lines are monitored by photosensitive devices. Multi-element determinations using sequential or simultaneous optical systems and a

41、xial or radial viewing of the plasma may be used.5 Interferences5.1 GeneralInterferences and matrix effects shall be recognized and appropriate measures to minimize them shall be made. There are several types of interferences see 5.2 to 5.6.5.2 Spectral interferencesSpectral interferences are due to

42、 incomplete isolation of the radiation emitted by the analyte from other detected radiation sources. Spectral interferences are caused by background emission from continuous 7BS EN 16963:2018EN 16963:2018 (E)or recombination phenomena, by stray light which causes background increase or overlap of a

43、spectral line from another element, or unresolved overlap of molecular band spectra. Background emission and stray light can usually be compensated for by subtracting the background emission measured adjacent to the analyte wavelength peak. To correct a sloping background shift two background correc

44、tion points on each side of the peak are used. Increase of background is more intensive with axial-view instruments. Background correction is not required in cases of line broadening where a background correction measurement would actually degrade the analytical result. A spectral line overlap usual

45、ly leads to the choice of an alternative line. If this is not possible, mathematical correction procedures (e.g. inter-element correction technique, multi-component spectral fitting) can be used to compensate for the interference. These correction procedures are usually a part of the instrument soft

46、ware.5.3 Transport interferencesTransport interferences are caused by differences in the properties between the sample solutions and the calibration solutions (viscosity, surface tension, density, dissolved solid content, type and concentration of acids). As a consequence, the supply of solution to

47、the nebulizer, the efficiency of nebulization and the droplet size distribution of the aerosol is altered, resulting in a change of sensitivity. Errors due to these interferences can be overcome by dilution of the solutions, by matrix matching, by standard addition or by internal standard.5.4 Excita

48、tion interferencesExcitation interferences are attributed to a change in the excitation conditions in the plasma especially by the presence of easily ionisable elements. The interference depends on the operating conditions of the plasma (e.g. power, sample introduction, gas flow-rate, observation he

49、ight) and differ from element to element. Improvement of the plasma conditions can therefore reduce excitation interferences. Other possibilities are dilution of the solutions, matrix matching or the standard addition technique.5.5 Chemical interferencesChemical interferences are not significant with the ICP-AES technique, but if observed, they can be minimized by careful selection of operating conditions (e.g. radio frequency power, observation position, gas flow rate and so forth).5.6 Memory interferencesMemory interferences result when a