Fertilizers - Determination of boron in concentrations > 10 % using acidimetric titration

This European Standard specifies a method for the determination of total and water extractable boron in mineral fertilizers containing more than 10 % boron.
This method is applicable to water and aqua regia fertilizer extracts obtained according to prEN 16962 and/or prEN 16964.
NOTE    A method used for determination of boron in mineral fertilizers containing less than 10 % of boron (spectrophotometric determination by azomethine-H) can be also used for the scope of this method after appropriate dilution of the extracts.

Düngemittel - Bestimmung von Bor in Konzentrationen > 10 % durch azidimetrische Titration

Diese Europäische Norm legt ein Verfahren zur Bestimmung von Gesamt- und aus Wasser extrahierbarem Bor in mineralischen Düngemitteln, die mehr als 10 % Bor enthalten, fest.
Dieses Verfahren ist auf Wasser  und Königswasser Extrakte von Düngemitteln anwendbar, die nach EN 16962 und/oder EN 16964 erhalten wurden.
Das Verfahren kann nach entsprechender Verdünnung der Extrakte auch für die Bestimmung von Bor in mineralischen Düngemitteln, die weniger oder gleich 10 % Bor enthalten (spektrophotometrische Bestimmung mit Azomethin H), verwendet werden.

Engrais - Dosage du bore dans des concentrations > 10 % par titration acidimétrique

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 plus de 10 % de bore.
Cette méthode est applicable aux extraits d’engrais aqueux et à l’eau régale obtenus conformément à l’EN 16962 et/ou à l’EN 16964.
NOTE   Une méthode utilisée pour le dosage du bore dans des engrais minéraux contenant moins de ou égal à 10 % de bore (dosage spectrophotométrique avec l’azométhine H) peut également être utilisée dans le cadre du domaine d’application de la présente méthode après dilution appropriée des extraits.

Gnojila - Določevanje bora v koncentracijah, večjih od 10 %, s kislinsko titracijo

Ta evropski standard določa postopek za določevanje skupne vsebnosti bora in bora, ki ga je mogoče ekstrahirati z vodo, v mineralnih gnojilih, ki vsebujejo več kot 10 % bora.
Ta metoda se uporablja za ekstrakte gnojil v vodi in zlatotopki, pridobljene v skladu s standardom prEN 16962 in/ali prEN 16964.
OPOMBA:    Metodo, ki se uporablja za določevanje vsebnosti bora v mineralnih gnojilih, ki vsebujejo manj kot 10 % bora (spektrofotometrično določevanje z azometinom-H), je mogoče uporabiti tudi za obseg te metode po ustreznem redčenju ekstraktov.

General Information

Status
Published
Public Enquiry End Date
06-Nov-2016
Publication Date
09-Jul-2018
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
22-Jun-2018
Due Date
27-Aug-2018
Completion Date
10-Jul-2018

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Düngemittel - Bestimmung von Bor in Konzentrationen > 10 % durch azidimetrische TitrationEngrais - Dosage du bore dans des concentrations > 10 % par titration acidimétriqueFertilizers - Determination of boron in concentrations > 10 % using acidimetric titration65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 17042:2018SIST EN 17042:2018en,fr,de01-september-2018SIST EN 17042:2018SLOVENSKI

STANDARD
SIST EN 17042:2018
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 17042
June
t r s z ICS
x wä r z r English Version
Fertilizers æ Determination of boron in concentrations
s r
¨ using acidimetric titration Engrais æ Dosage du bore dans des concentrations
s r
¨ par titrage acidimétrique
Düngemittel æ Bestimmung von Bor in Konzentrationen
s r
¨ durch azidimetrische Titration 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 tã t r s z ESIST EN 17042:2018
EN 17042:2018 (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 ........................................................................................................................................................... 6 8 Procedure........................................................................................................................................................... 7 8.1 Test solution ..................................................................................................................................................... 7 8.2 Blank solution .................................................................................................................................................. 7 8.3 Boron (B) value of the sodium hydroxide solution (6.5) .................................................................. 7 9 Calculation and expression of the results .............................................................................................. 8 10 Test report ......................................................................................................................................................... 8 Annex A (informative)

Verification data — Comparison of ICP-AES method and acidimetric titration method .............................................................................................................................................. 9 A.1 Introduction ...................................................................................................................................................... 9 A.2 Validation based on water extraction...................................................................................................... 9 A.2.1 Test materials used in the validation study .......................................................................................... 9 A.2.2 Results of the validation study ................................................................................................................... 9 A.2.3 Conclusions .................................................................................................................................................... 10 A.3 Validation based on aqua regia extraction ......................................................................................... 10 A.3.1 Test materials used in the validation study ....................................................................................... 10 A.3.2 Results of the validation study ................................................................................................................ 11 A.3.3 Conclusions .................................................................................................................................................... 12 Bibliography ................................................................................................................................................................. 13

SIST EN 17042:2018

EN 17042:2018 (E) 3 European foreword This document (EN 17042:2018) 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 endorsement, at the latest by December 2018, and conflicting national standards shall be withdrawn at the latest by December 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 European Commission and the European Free Trade Association. 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, 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. SIST EN 17042:2018

EN 17042:2018 (E) 4 Introduction The preparation of this document by CEN is based on a mandate 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 European Standard 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 measurement. The determination of boron in fertilizers can be executed by inductively coupled plasma-atomic emission spectrometry (ICP-AES). Acidimetric determination after addition of mannitol is more labour intensive but it is an option when ICP-AES is not available. 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 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. SIST EN 17042:2018

EN 17042:2018 (E) 5 1 Scope This European Standard specifies a method for the determination of total and water extractable boron in mineral fertilizers containing more than 10 % boron. This method is applicable to water and aqua regia fertilizer extracts obtained according to EN 16962 and/or EN 16964. NOTE A method used for the determination of boron in mineral fertilizers containing less than or equal to 10 % of boron (spectrophotometric determination by azomethine-H) can be also used for the scope of this method after appropriate dilution of the extracts. 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 applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 1482-2, Fertilizers and liming materials - Sampling and sample preparation - Part 2: Sample preparation EN 12944-1, Fertilizers and liming materials and soil improvers - Vocabulary - Part 1: General terms EN 12944-2, Fertilizers and liming materials and soil improvers - Vocabulary - Part 2: Terms relating to fertilizers EN 16962, Fertilizers - Extraction of water soluble micro-nutrients in fertilizers and removal of organic compounds from fertilizer extracts EN 16964, Fertilizers - Extraction of total micro-nutrients in fertilizers using aqua regia EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696) 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 12944-1 and EN 12944-2 apply. 4 Principle Boric acid forms a complex with mannitol: H3BO3 + C6H14O6 \ C6H15O8B + H2O. This complex acid is titrated with sodium hydroxide solution to a pH of 6,3. 5 Sampling and sample preparation Sampling is not part of this European Standard. A recommended sampling method is specified in EN 1482-1 [2]. Sample preparation shall be carried out in accordance with EN 1482-2. The sample extracts shall be prepared in accordance with EN 16962 and/or EN 16964. SIST EN 17042:2018

EN 17042:2018 (E) 6 6 Reagents All reagents shall be of recognized analytical grade. All reagents including water shall have negligible concentration of boron if compared to the lowest concentration of that element in the sample solution. 6.1 Water, grade 2 according to EN ISO 3696 and free from boron. 6.2 Methyl red indicator solution. Dissolve 0,1 g of methyl red (C15H15N3O2) in 50 ml of ethanol (95 %) in a 100 ml volumetric flask (7.5). Make up the volume to 100 ml with water (6.1). Mix thoroughly. 6.3 Diluted hydrochloric acid solution, with a concentration of about c = 0,5 mol/l. Mix 1 volume of hydrochloric acid HCl ( = 1,18 g/ml) with 20 volumes of water (6.1). 6.4 Sodium hydroxide solution, with a concentration of about c = 0,5 mol/l. The solution shall be free from carbon dioxide. Dissolve 20 g of sodium hydroxide (NaOH) in pellet form in a 1 000 ml volumetric flask (7.6) containing about 800 ml of boiled water (6.1). After dissolution and cooling make up to 1 000 ml with boiled water (6.1) and mix thoroughly. 6.5 Standard sodium hydroxide solution, with a concentration of about c = 0,025 mol/l. The solution shall be free from carbon dioxide. Dilute 0,5 mol/l sodium hydroxide solution (6.4) 20 times with boiled water and mix thoroughly. The value of the solution expressed as boron (B) is to be determined (8.3). 6.6 Boron calibration solution,

= 100 mg/l. Weigh to the nearest 0,1 mg 0,571 9 g of boric acid (H3BO3), dissolve in water (6.1), transfer quantitatively into a 1 000 ml volumetric flask (7.6), make up to volume with water (6.1) and mix thoroughly. Transfer to a plastic bottle for storage in a refrigerator at 4 °C to 8 °C. Commercially available stock solution with adequate specification may be used. The solution is generally considered to be stable for one year, but in reference to guaranteed stability, the recommendations of the manufacturer shall be considered. 6.7 D-mannitol, (C6H14O6) powder. 6.8 Sodium chloride (NaCl). 7 Apparatus 7.1 pH meter, with glass electrode. 7.2 Magnetic stirrer. 7.3 Beaker, capacity 400 ml. 7.4 Polytetrafluoroethylene (PTFE) (Teflon®)1) rod. 7.5 Volumetric flasks, capacity 100 ml.

1) This information is given for the convenience of users of this document and does not constitute an endorsement by CEN of the product named. Equivalent products may be used if they can be shown to lead to the same results. SIST EN 17042:2018

EN 17042:2018 (E) 7 7.6 Volumetric flasks, capacity 1 000 ml. 8 Procedure 8.1 Test solution Place an aliquot (a) of the extract containing 2 mg to 4 mg boron into a 400 ml beaker (7.3). Add 150 ml of water (

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