EN 16962-2018 Fertilizers - Extraction of water soluble micro-nutrients in fertilizers and removal of organic compounds from fertilizer extracts.pdf

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1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Fertilizers Extraction of water soluble micro-nutrients in fertilizers and removal of organic compounds from fertilizer extractsBS EN 16962:2018National forewordThis British Standard is the UK implementation of EN 16962

2、:2018.The UK participation 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

3、a contract. Users are responsible for its correct application. The British Standards Institution 2018 Published by BSI Standards Limited 2018ISBN 978 0 580 91785 1ICS 65.080Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the

4、authority of the Standards Policy and Strategy Committee on 31 March 2018.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS EN 16962:2018EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 16962January 2018ICS 65.080EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN D

5、E NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGCEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2018 CEN Ref. No. EN 16962:2018: EAll rights of exploitation in any form and by any means reserved worldwide for CEN national MembersFertilizers - Extraction of water soluble micro-nutrients

6、 in fertilizers and removal of organic compounds from fertilizer extractsEngrais - Extraction des oligo-lments soluble dans leau des engrais et limination des composs organiques dans les extraits dengraisDngemittel - Extraktion wasserlslicher Spurennhrstoffe aus Dngemitteln und Beseitigung organisch

7、er Verbindungen aus DngemittelextraktenThis 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 giving this European Standard the status of a national standard without any alteration. Up

8、-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 (English, French, German). A version in any other language made by transl

9、ation 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, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland,

10、 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 United Kingdom.English VersionEN 16962:2018 (E)E

11、uropean forewordThis document (EN 16962:2018) has been prepared by Technical Committee 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 endo

12、rsement, at the latest by July 2018, and conflicting national standards shall be withdrawn 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 suc

13、h patent rights.This document has been prepared under a mandate given to CEN by the European 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 Stan

14、dard: 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, Slov

15、enia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.2BS EN 16962:2018EN 16962:2018 (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

16、 of analysis of fertilizers in the framework of Regulation (EC) No 2003/2003 1.Water extraction is empirical and in many cases cannot be quantitative. The extraction is dependent on temperature and extraction time, on the ratio of water/sample and intensity of the extraction. To reduce the level of

17、uncertainty of the extraction step to a reasonable level it is necessary to strictly follow the given procedure. The method can be applied to mineral fertilizers with micro-nutrient content of 10 % as well as of 10 %. Removal of organic compounds is not usually necessary if FAAS or ICP-AES method of

18、 determination is used. It is applied only in some cases for determination of boron and molybdenum by spectrophotometric methods, determination of boron by acidimetric titration and gravimetric determination of molybdenum. The method for removal of organic compounds is a part of this standard.WARNIN

19、G Persons using this European Standard 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 en

20、sure compliance with any national regulatory conditions.IMPORTANT It is absolutely essential that tests conducted according to this European Standard are carried out by suitably trained staff.3BS EN 16962:2018EN 16962:2018 (E)European foreword 2Introduction . 3European foreword 5Introduction . 61 Sc

21、ope . 72 Normative references 73 Terms and definitions . 74 Principle 75 Sampling and sample preparation 76 Reagents 77 Apparatus . 88 Procedure. 88.1 Preparation of the test solutions . 88.1.1 Micro-nutrient content 10 % 88.1.2 Micro-nutrient content 10 % 88.2 Extraction 98.3 Removal of organic com

22、pounds . 99 Precision 1010 Test report 10Bibliography .114Contents PageBS EN 16962:2018EN 16962:2018 (E)European forewordThis document (EN 16962:2018) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”, the secretariat of which is held by DIN.This European Standar

23、d 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.Attention is drawn to the possibility that some of the elements of this docum

24、ent 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 Trade Association.According to the CEN-CENELEC Internal Regulations,

25、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 Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Lat

26、via, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.5BS EN 16962:2018EN 16962:2018 (E)IntroductionThe preparation of this document is based on a mandate given to CEN by the European C

27、ommission 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.Water extraction is empirical and in many cases cannot be quantitative. The extraction is dependent on temperature a

28、nd extraction time, on the ratio of water/sample and intensity of the extraction. To reduce the level of uncertainty of the extraction step to a reasonable level it is necessary to strictly follow the given procedure. The method can be applied to mineral fertilizers with micro-nutrient content of 10

29、 % as well as of 10 %. Removal of organic compounds is not usually necessary if FAAS or ICP-AES method of determination is used. It is applied only in some cases for determination of boron and molybdenum by spectrophotometric methods, determination of boron by acidimetric titration and gravimetric d

30、etermination of molybdenum. The method for removal of organic compounds is a part of this standard.WARNING Persons using this European Standard 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

31、 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 according to this European Standard are carried out by suitably trained staff.6BS

32、 EN 16962:2018EN 16962:2018 (E)1 ScopeThis European Standard specifies a method for the extraction of water soluble forms of boron, cobalt, copper, iron, manganese, molybdenum and zinc from mineral fertilizers containing one or more micro-nutrients and the procedure for removal of organic compounds

33、from the water extracts.The extracts can be analysed according to EN 16963, EN 16965, prEN 17041, prEN 17042, prEN 17043 and CEN/TS 17060.2 Normative referencesThe following documents in whole or in part, are normatively referenced in this document and are indispensable for its application. For date

34、d 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, Fertilizers and liming materials and soil

35、 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 atomic absorption spectrometry (FAAS)

36、prEN 17043, Fertilizers Determination of molybdenum in concentrations 10 % using spectrometry of a complex with ammonium thiocyanateEN 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 defini

37、tions given in EN 12944-1 and EN 12944-2 apply.4 PrincipleThe micro-nutrients are extracted by shaking the fertilizer sample in water at (20 2) C. Extracts are acidified after the extraction to avoid hydrolysis. Organic matter is removed if necessary by boiling after addition of hydrogen peroxide.5

38、Sampling and sample preparationSampling and sample preparation are not part of this 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 analytical grade and they shall have negligible

39、 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.7BS EN 16962:2018EN 16962:2018 (E)6.2 Nitric acid 65 %, c(HNO3) = 14,3 mol/l; = 1,42 g/m

40、l.6.2.1 Diluted nitric acid solution, c(HNO3) = 5 mol/l.Add 350 ml of nitric acid (6.2) to 650 ml of water (6.1).6.3 Hydrogen peroxide solution 30 % H2O2, = 1,11 g/ml, free from micro-nutrients.6.4 Hydrochloric acid 37 % HCl, c(HCl) = 12 mol/l, = 1,18 g/ml.6.4.1 Diluted hydrochloric acid solution, c

41、(HCl) = 5 mol/l.Add 420 ml of hydrochloric acid (6.4) to 580 ml of water (6.1).7 ApparatusIf the boron content is to be determined it is recommended to minimize contact of all solutions with borosilicate glassware. Use suitable plastic or silica ware especially for extraction step and for removal of

42、 organic compounds. Glass volumetric flasks may be used for making up to volume but shall not be used for storage of extracts and solutions.7.1 Shaker, rotary or horizontal eccentric shaker.Shaking shall prevent any settling of the sample during extraction.7.2 Electric hotplate, equipped with variab

43、le temperature control.7.3 Extraction vessels, capacity 500 ml and 1 000 ml.7.4 Filter paper, ash-free and of recognized and tested quality.7.5 Beaker, capacity 100 ml.7.6 Volumetric flasks, capacity 25 ml and 50 ml.7.7 Watch glass.8 Procedure8.1 Preparation of the test solutions8.1.1 Micro-nutrient

44、 content 10 %For samples with a micro-nutrient content of 10 % weigh (5 0,005) g of the prepared sample, transfer the sample quantitatively to a 500 ml extraction vessel (7.3) and add (250 0,2) ml of water (6.1) at (20 2) C.8.1.2 Micro-nutrient content 10 %For samples with a micro-nutrient content o

45、f 10 % weigh (2 0,002) g of the prepared sample, transfer the sample quantitatively to a 1 000 ml extraction vessel (7.3) and add (500 0,5) ml of water (6.1) at (20 2) C.8 BS EN 16962:2018EN 16962:2018 (E)8.2 ExtractionClose the vessel tightly and shake vigorously by hand to disperse the sample. The

46、n place the vessel on the shaker (7.1) and shake for 60 min. The intensity of shaking shall be adjusted to prevent any settling of the sample during the extraction. The temperature of the extraction solution shall be kept at (20 2) C during the whole extraction time. Filter the extract if necessary

47、immediately after the extraction into a plastic vessel. Use ash-free filter paper of recognized and tested quality (7.4) and discard the first portion of the filtrate (approximately 20 ml). Pipette 20 ml of the extract into a 25 ml volumetric flask, add 2,5 ml of diluted nitric acid solution (6.2.1)

48、, fill to the mark with water (6.1) and mix well. The final concentration of nitric acid is 0,5 mol/l.Account shall be taken of this dilution when taking aliquot portions and calculating the percentage of micro-nutrient in the sample.Prepare a blank test solution following the same procedure as for

49、samples.Acidification of the water extract with nitric acid is not suitable for spectrophotometric determination of molybdenum according to prEN 17043. In this case hydrochloric acid (6.4) shall be added; the final concentration of hydrochloric acid is 0,5 mol/l. Acidification with hydrochloric acid shall be used also if precipitation of Fe(III) is observed after the addition of nitric acid. If boron is not to be determined standard glassware may be used. If the measurement is not carried out immediate