EN 16964-2018 en Fertilizers - Extraction of total micro-nutrients in fertilizers using aqua regia.pdf

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1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Fertilizers - Extraction of total micro-nutrients in fertilizers using aqua regiaBS EN 16964:2018National forewordThis British Standard is the UK implementation of EN 16964:2018.The UK participation in its preparation w

2、as 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 responsible for its corre

3、ct application. The British Standards Institution 2018 Published by BSI Standards Limited 2018ISBN 978 0 580 91787 5ICS 65.080Compliance with a British Standard cannot confer immunity from legal obligations. This British Standard was published under the authority of the Standards Policy and Strategy

4、 Committee on 28 February 2018.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS EN 16964:2018EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 16964January 2018ICS 65.080EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMU

5、NGCEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2018 CEN Ref. No. EN 16964:2018: EAll rights of exploitation in any form and by any means reserved worldwide for CEN national MembersFertilizers - Extraction of total micro-nutrients in fertilizers using aqua regiaEngrais - Extractio

6、n des oligo-lments totaux des engrais leau rgaleDngemittel - Extraktion von Gesamtspurennhrstoffen aus Dngemitteln mit KnigswasserThis European Standard was approved by CEN on 15 October 2017.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for

7、 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 three

8、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 bodies

9、 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, Sloven

10、ia, Spain, Sweden, Switzerland, Turkey and United Kingdom.English VersionEN 16964:2018 (E)European foreword 3Introduction . 41 Scope . 52 Normative references 53 Terms and definitions . 54 Principle 55 Sampling and sample preparation 56 Reagents 57 Apparatus . 68 Procedure. 68.1 General . 68.2 Prepa

11、ration of the test solutions . 68.2.1 Micro-nutrient content 10 % 68.2.2 Micro-nutrient content 10 % 68.3 Extraction 69 Precision . 710 Test report . 7Bibliography 82Contents PageBS EN 16964:2018EN 16964:2018 (E)European forewordThis document (EN 16964:2018) has been prepared by Technical Committee

12、CEN/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 withdr

13、awn 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 Eur

14、opean 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, Fi

15、nland, 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.3BS EN 16964:2018EN 169

16、64:2018 (E)IntroductionThe preparation of this document was 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.Aqua re

17、gia is applied for determination of many elements in different matrices. A horizontal standard for aqua regia extraction of soils, sludges and biowaste was prepared by CEN/TC 400. Similar procedure was applied for determination of the aqua regia extractable content of arsenic, mercury, cadmium, chro

18、mium, nickel and lead in fertilizers and liming materials (European Standard prepared by CEN/TC 260). Wide use of the aqua regia extraction and possibility to prepare a suitable horizontal standard was the main reason to develop the given extraction procedure.WARNING Persons using this European Stan

19、dard should be familiar with normal laboratory practice. 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

20、regulatory conditions.IMPORTANT It is absolutely essential that tests conducted according to this European Standard are carried out by suitably trained staff.4BS EN 16964:2018EN 16964:2018 (E)1 ScopeThis European Standard specifies a method for the total extraction of boron, cobalt, copper, iron, ma

21、nganese, molybdenum and zinc with aqua regia from mineral fertilizers containing one or more micro-nutrients.The extracts can be analysed according to EN 16963, EN 16965, prEN 17041, prEN 17042 and prEN 17043.This method is also suitable for the extraction of cadmium, chromium, nickel and lead to be

22、 determined according to EN 16319; the extraction of mercury to be determined according to EN 16320 and the extraction of arsenic to be determined according to EN 16317.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensab

23、le 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 12944-1, Fertilizers and liming materials and soil improvers Vocabulary Part 1: General termsEN 12944-2, Fertilize

24、rs and liming materials and soil improvers Vocabulary Part 2: Terms relating to fertilizersEN 16963, Fertilizers Determination of boron, cobalt, copper, iron, manganese, molybdenum and zinc using ICP-AESEN 16965, Fertilizers Determination of cobalt, copper, iron, manganese and zinc using flame atomi

25、c absorption spectrometry (FAAS)EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696)3 Terms and definitionsFor the purposes of this document, the terms and definitions given in EN 12944-1 and EN 12944-2 apply.4 PrincipleThe micro-nutrients are extracted from the

26、 sample with boiling aqua regia.5 Sampling and sample preparationSampling and sample preparation are not part of this European Standard. A recommended sampling method is given in EN 1482-1 2 and a recommended sample preparation method in EN 1482-2 3.6 ReagentsAll reagents shall be of recognized anal

27、ytical grade and they shall have negligible concentration of the element to be determined if compared to the lowest concentration of that element in the sample solution.6.1 Water for extraction, grade 2 according to EN ISO 3696, free from micro-nutrients.6.2 Hydrochloric acid 37 % HCl, c(HCl) = 12 m

28、ol/l, = 1,18 g/ml.6.3 Nitric acid 65 %, c(HNO3) = 14,3 mol/l; approximately 1,4 g/ml.5BS EN 16964:2018EN 16964:2018 (E)7 Apparatus7.1 Common laboratory glassware.If the boron content is to be determined, it is necessary to minimize the contact of all solutions with borosilicate glassware.Suitable pl

29、astic or silica ware is needed especially for the extraction step. Glass volumetric flasks may be used for making up to volume but not for storage of extracts and solutions.7.2 Apparatus for thermal heating digestion, temperature controlled with reaction vessel and reflux condenser.The capacity of t

30、he reaction vessel shall be at least 5 times of the volume of the aqua regia used.7.3 Filter paper, ash free and of recognized and tested quality.8 Procedure8.1 GeneralCAUTION Suitable precautions shall be taken to avoid any contact of laboratory staff with acid fumes. It is recommended that the ext

31、raction procedure is carried out in a fume cupboard.8.2 Preparation of the test solutions8.2.1 Micro-nutrient content 10 %For samples with a micro-nutrient content of 10 % weigh (3 0,003) g of the prepared sample, transfer the sample quantitatively to the reaction vessel (7.2).8.2.2 Micro-nutrient c

32、ontent 10 %For samples with a micro-nutrient content of 10 % weigh (1 0,001) g of the prepared sample, transfer the sample quantitatively to the reaction vessel (7.2).8.3 ExtractionMoisten the test portion (8.2.1 or 8.2.2) with about 0,5 ml to 1,0 ml of water (6.1) and add, while mixing, 21 ml of hy

33、drochloric acid (6.2) followed by 7 ml of nitric acid (6.3) drop wise if necessary to reduce foaming. Connect a condenser to the reaction vessel and let the mixture stand at laboratory temperature until any effervescence almost ceases. Transfer to the heating device and slowly raise the temperature

34、of the reaction mixture to reflux conditions and maintain for 2 h ensuring that the condensation zone is lower than 1/3 of the height of the condenser. Then allow to cool and rinse the condenser with 10 ml of water (6.1).For samples with a micro-nutrient content of 10 % transfer quantitatively into

35、a 150 ml volumetric flask and dilute to the mark with water. The test solution corresponds to a 50 times dilution of the sample.For samples with a micro-nutrient content of 10 % transfer quantitatively into a 500 ml volumetric flask and dilute to the mark with water. The test solution corresponds to

36、 a 500 times dilution of the sample.Test solutions may be filtered or centrifuged if necessary. Use ash-free filter paper of recognized and tested quality (7.3) and discard the first portion of the filtrate (approximately 20 ml).6 BS EN 16964:2018EN 16964:2018 (E)Prepare a blank test solution follow

37、ing the same procedure as for samples.Carry out the measurement immediately or store the extracts in tightly closed plastic vessels for up to 15 d.If boron is not to be determined standard glassware may be used. Glass condensers may be used for all elements including boron. If only glassware is avai

38、lable it may be used for boron determination only if the concentration of boron in blank samples is negligible.Procedure using a test portion of (2 0,002) g: 14 ml of hydrochloric acid (6.2), 4,7 ml of nitric acid (6.3) and 100 ml volumetric flask may be used alternatively if 150 ml volumetric flask

39、s are not available.The amount of added aqua regia is sufficient for oxidation of about 0,5 g organic carbon. If there is more than 0,5 g of organic carbon add 1 ml of concentrated nitric acid (6.3) to every 0,1 g of organic carbon above 0,5 g, but not more than 10 ml of nitric acid.Addition of one

40、drop of octanol to the reaction vessel may be used as an antifoaming agent.Erlenmeyer flasks or high beakers covered with watch glasses may be used as an alternative for the extraction step if the laboratory proves that there were no loses of the elements to be determined.9 PrecisionThe precision of

41、 the extraction method specified in this document has been determined in an inter-laboratory test based on the measurement methods specified in EN 16963 and EN 16965. The statistical data obtained by ICP-AES measurement are given in EN 16963. The statistical data obtained by FAAS measurement are giv

42、en in EN 16965.10 Test reportThe test report shall contain at least the following information:a) all information necessary for the complete identification of the sample;b) test method used with reference to this document, EN 16964;c) date of sampling and sampling procedure (if known);d) date when th

43、e extraction was finished;e) all operating details not specified in this document, or regarded as optional, together with details of any incidents that occurred when performing the method, which might have influenced the test result(s).7BS EN 16964:2018EN 16964:2018 (E)Bibliography1 Regulation (EC)

44、No 2003/2003 of the European Parliament and of the Council of 13 October 2003 relating to fertilizers, Official Journal L 304, 21/11/ 2003, Pp. 1-1942 EN 1482-1, Fertilizers and liming materials Sampling and sample preparation Part 1: Sampling3 EN 1482-2, Fertilizers and liming materials Sampling an

45、d sample preparation Part 2: Sample preparation4 EN 16317, Fertilizers and liming materials Determination of arsenic by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution5 EN 16319, Fertilizers and liming materials Determination of cadmium, chromium, lead

46、and nickel by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution6 EN 16320, Fertilizers and liming materials Determination of mercury by vapour generation (VG) after aqua regia dissolution7 prEN 17041, Fertilizers Determination of boron in concentrations 1

47、0 % using spectrometry with azomethine-H8 prEN 17042, Fertilizers Determination of boron in concentrations 10 % using acidimetric titration9 prEN 17043, Fertilizers Determination of molybdenum in concentrations 10 % using spectrometry of a complex with ammonium thiocyanate10 CEN/TS 17060, Fertilizer

48、s Determination of molybdenum in concentrations 10 % using a gravimetric method with 8-hydroxyquinoline8 BS EN 16964:2018This page deliberately left blankThis page deliberately left blankBSI is the national body responsible for preparing British Standards and other standards-related publications, in

49、formation and services.BSI is incorporated by Royal Charter. British Standards and other standardization products are published by BSI Standards Limited.British Standards Institution (BSI)About usWe bring together business, industry, government, consumers, innovators and others to shape their combined experience and expertise into standards -based solutions.The knowledge embodied in our standards has been carefully assembled in a dependable format and refined through our open consulta