Fertilizers - Determination of boron in concentrations ≤ 10 % using spectrometry with azomethine-H

This European Standard specifies a method for the determination of total and water extractable boron in mineral fertilizers containing less than or equal to 10 % boron. The method is not suitable for fertilizers with Fe concentrations more than twenty times higher than the concentration of boron.
This method is applicable to water and aqua regia fertilizer extracts obtained according to EN 16962 and/or EN 16964.
The method can also be used for the determination of boron in mineral fertilizers containing more than 10 % boron after appropriate dilution of the extracts.

Düngemittel - Bestimmung von Bor in Konzentrationen ≤ 10 % durch Spektrometrie mit Azomethin-H

Diese Europäische Norm legt ein Verfahren zur Bestimmung von Gesamtbor und aus Wasser extrahierbarem Bor in mineralischen Düngemitteln fest, die weniger oder gleich 10 % Bor enthalten. Das Verfahren eignet sich nicht für Düngemittel mit Fe-Konzentrationen, die mehr als zwanzig Mal höher sind als die Konzentration an Bor.
Die Extraktionsverfahren sind in prEN 16962 und/oder prEN 16964 festgelegt.
Das Verfahren kann auch für die Bestimmung von Bor in mineralischen Düngemitteln, die mehr als 10 % Bor enthalten, nach entsprechender Verdünnung der Extrakte verwendet werden.

Engrais - Dosage du bore dans des concentrations ≤ 10 % par spectrométrie avec l'azomethine-H

La présente Norme européenne spécifie une méthode pour le dosage du bore total et du bore extractible à l’eau dans des engrais minéraux contenant au plus 10 % de bore. La méthode ne convient pas pour les engrais ayant des concentrations en Fe supérieures à vingt fois la concentration en bore.
Cette méthode est applicable aux extraits d’engrais aqueux et à l’eau régale préparés conformément à l’EN 16962 et/ou à l’EN 16964.
La méthode peut également être utilisée pour le dosage du bore dans des engrais minéraux contenant plus de 10 % de bore après une dilution appropriée des extraits.

Gnojila - Določevanje bora v koncentracijah, manjših ali enakih 10 %, s spektrometrijo z azometinom-H

Ta dokument določa postopek za določevanje skupne vsebnosti bora in bora, ki ga je mogoče ekstrahirati z vodo, v mineralnih gnojilih, ki vsebujejo manj kot oziroma 10 % bora, s spektrometrijo z azometinom-H. Metoda ni primerna za gnojila s koncentracijami Fe, ki za več kot 20-krat presegajo koncentracijo bora.

General Information

Status
Published
Publication Date
12-Jun-2018
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
13-Jun-2018
Completion Date
13-Jun-2018

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.$]RPHWKLQ+OD]RPHWKLQH+D]RPHWKLQH+65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 17041:2018SIST EN 17041:2018en,fr,de01-september-2018SIST EN 17041:2018SLOVENSKI

STANDARD
SIST EN 17041:2018
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 17041
June
t r s z ICS
x wä r z r English Version
Fertilizers æ Determination of boron in concentrations ≤
s r

¨ using spectrometry with azomethineæH Engrais æ Dosage du bore dans des concentrations ≤

s r
¨ par spectrométrie avec l 5azomethineæH
Düngemittel æ Bestimmung von Bor in Konzentrationen ≤
s r

¨ durch Spektrometrie mit AzomethinæH This European Standard was approved by CEN on

t x February
t r s zä

egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä

translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä

CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä

EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre:
Rue de la Science 23,
B-1040 Brussels

t r s z CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN

s y r v sã t r s z ESIST EN 17041:2018
EN 17041:2018 (E) 2 Contents Page

European foreword ....................................................................................................................................................... 3 Introduction .................................................................................................................................................................... 4 1 Scope .................................................................................................................................................................... 5 2 Normative references .................................................................................................................................... 5 3 Terms and definitions ................................................................................................................................... 5 4 Principle ............................................................................................................................................................. 5 5 Sampling and sample preparation ............................................................................................................ 5 6 Reagents ............................................................................................................................................................. 6 7 Apparatus ........................................................................................................................................................... 7 8 Procedure........................................................................................................................................................... 7 8.1 General ................................................................................................................................................................ 7 8.2 Preparation of calibration solutions ........................................................................................................ 7 8.3 Preparation of the test solutions ............................................................................................................... 7 8.4 Preparation of the correction solutions ................................................................................................. 8 8.5 Colour development ....................................................................................................................................... 8 8.6 Measurement .................................................................................................................................................... 8 9 Calculation and expression of the result ................................................................................................ 8 10 Test report ......................................................................................................................................................... 9 Annex A (infor– Comparison of ICP-AES method and spectrophotometric method with azomethine-H ............................................................................. 10 A.1 Introduction ................................................................................................................................................... 10 A.2 Validation based on water extraction................................................................................................... 10 A.2.1 Test materials used in the validation study ....................................................................................... 10 A.2.2 Results of the validation study ................................................................................................................ 11 A.2.3 Conclusions .................................................................................................................................................... 12 A.3 Validation based on aqua regia extraction ......................................................................................... 12 A.3.1 Test materials used in the validation study ....................................................................................... 12 A.3.2 Results of the validation study ................................................................................................................ 14 A.3.3 Conclusions .................................................................................................................................................... 15 Bibliography ................................................................................................................................................................. 16

SIST EN 17041:2018

EN 17041:2018 (E) 3 European foreword EN 17041:2018 260 “Fertilizers and liming materialsóá the secretariat of which is held by DINä This European Standard shall be given the status of a national standardá either by publication of an identical text or by endorsementá at the latest by December

t r s zá and conflicting national standards shall be withdrawn at the latest by December

t r s zä Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rightsä CEN shall not be held responsible for identifying any or all such patent rightsä This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Associationä According to the CEN-CENELEC Internal Regulationsá the national standards organisations of the following countries are bound to implement this European Standardã Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and the United Kingdomä SIST EN 17041:2018

EN 17041:2018 (E) 4 Introduction The preparation of this document by CEN is based on a mandate by the European Commission and the tion of methods of

1 This European Standard is part of a modular approach and concerns the analytical measurement stepä òModularó means that a test standard concerns a specific step in assessing a property and not the whole chain of measurementsä The determination of boron in fertilizers can be executed by inductively coupled plasma-atomic --H is more labour intensive than ICP-EN

s x { x uand it is an option when ICP-AES is not availableä The spectrophotometric determination can be influenced by iron and more attention is necessary also to organic matter removal and interferences from extract colourä The procedure for removal of organic matter from the extracts is given in EN 16962ä WARNING — Persons using this European Standard should be familiar with normal laboratory practiceä This European Standard does not purport to address all of the safety issuesá if anyá associated with its useä It is the responsibility of the user to establish appropriate health and safety practices and to ensure compliance with any national regulatory conditionsä IMPORTANT — It is absolutely essential that tests conducted according to this European Standard are carried out by suitably trained staffä SIST EN 17041:2018

EN 17041:2018 (E) 5 1 Scope This European Standard specifies a method for the determination of total and water extractable boron in mineral fertilizers containing less than or equal to

s r

¨ boronä The method is not suitable for fertilizers with Fe concentrations more than twenty times higher than the concentration of boronä This method is applicable to water and aqua regia fertilizer extracts obtained according to EN 16962 EN 16964ä The method can also be used for the determination of boron in mineral fertilizers containing more than 10

¨ boron after appropriate dilution of the extractsä 2 Normative references The following documentsá in whole or in partá are normatively referenced in this document and are indispensable for its applicationä For dated referencesá only the edition cited appliesä For undated ppliesä EN 1482-2á Fertilizers and liming materials - Sampling and sample preparation - Part 2: Sample preparation EN 12944-1á Fertilizers and liming materials and soil improvers - Vocabulary - Part 1: General terms EN 12944-2á Fertilizers and liming materials and soil improvers - Vocabulary - Part 2: Terms relating to fertilizers EN 16962á Fertilizers - Extraction of water soluble micro-nutrients in fertilizers and removal of organic compounds from fertilizer extracts EN 16964á Fertilizers - Extraction of total micro-nutrients in fertilizers using aqua regia EN ISO

u x { xá Water for analytical laboratory use - Specification and test methods (ISO 3696) 3 Terms and definitions For the purposes of this documentá the terms and definitions given in EN 12944-1 and EN 12944-2 applyä 4 Principle Boron reacts with azomethine-H and the yellow complex produced is determined spectrophotometrically at

v s r nmä Interfering ions are masked with ethylenediaminetetraacetic acid -EDTA complex is removed by

5 Sampling and sample preparation Sampling is not part of the method specified in this documentä A recommended sampling method is specified in EN 1482-1 2 Sample preparation shall be carried out in accordance with EN 1482-2ä The sample extracts shall be prepared in accordance with EN 16962 EN 16964ä SIST EN 17041:2018

EN 17041:2018 (E) 6 6 Reagents All reagents shall be of recognized analytical grade and shall have negligible concentration of boron if compared to the lowest concentration of that element in the sample solutionä All reagents including water shall be tested for presence of boronä 6.1 Water for extractioná grade

t according to EN ISO
u x { x and free from boronä 6.2 EDTA buffer solutionä 6.2.1 Ammonium acetate

uCOONH4 6.2.2 Disodium salt of ethylenediaminetetraacetic acid 2 6.2.3 Acetic acidá

sá s s
Place in a
w r r
yä v
xä s g ammonium acetate
xä tä s
xä tä t ml
xä tä u xä s yä { ±

yä x 6.3 Azomethine-H solutionä 6.3.1 Azomethine-H 17H12NNaO8S2 6.3.2 Ascorbic acid 6H8O6 Place in a 200

yä u): 10
xä t mg of azomethine-H
xä uä s

xä uä t xä ssolution is stable for three daysä 6.4 Boron calibration solutionsä 6.4.1 Boron stock solutioná

s r r
Dissolve
rá w y s 9
uBO u xä s) in a 1 000
yä w xä s yä x to 8)

¹Cä Commercially available stock solutions with adequate specification may be usedä The solution is considered to be stable for more than one yeará but in reference to guaranteed

...

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