Fertilizers - Determination of molybdenum in concentrations > 10 % using a gravimetric method with 8-hydroxyquinoline

This Technical Specification specifies the procedure for determination of total and water extractable molybdenum in mineral fertilizers containing more than 10 % molybdenum. This method is applicable to water and aqua regia fertilizer extracts obtained according to EN 260172 and/or EN 260176.

Düngemittel - Bestimmung von Molybdän in Konzentrationen > 10 % durch Gravimetrie mit 8-Hydroxychinolin

Diese Technische Spezifikation legt ein Verfahren zur Bestimmung von Gesamt-Molybdän und wasserextrahierbarem Molybdän in mineralischen Düngemitteln, die mehr als 10 % Molybdän enthalten, fest.
Dieses Verfahren ist auf Wasser- und Königswasser-Extrakte von Düngemitteln anwendbar, die nach prEN 16962:2016 und/oder prEN 16964:2016 erhalten wurden.

Engrais - Dosage du molybdène dans des concentrations > 10 % en utilisant une méthode gravimétrique à la 8-hydroxyquinoléine

La présente Spécification technique spécifie une méthode pour le dosage du molybdène total et du molybdène extractible à l’eau dans des engrais minéraux contenant plus de 10 % de molybdène.
Cette méthode est applicable aux extraits d’engrais aqueux et à l’eau régale obtenus conformément au prEN 16962:2016 et/ou au prEN 16964:2016.

Gnojila - Določevanje molibdena v koncentracijah do 10 % z gravimetrično metodo z 8-hidroksikinolinom

Ta tehnična specifikacija določa postopek za določevanje skupne vsebnosti molibdena in molibdena, ki ga je mogoče ekstrahirati z vodo, v mineralnih gnojilih, ki vsebujejo več kot 10 % molibdena. Ta metoda se uporablja za ekstrakte gnojil v vodi in zlatotopki, pridobljene v skladu s standardom EN 260172 in/ali EN 260176.

General Information

Status
Published
Public Enquiry End Date
09-Jan-2016
Publication Date
07-Nov-2017
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
17-Oct-2017
Due Date
22-Dec-2017
Completion Date
08-Nov-2017

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SLOVENSKI STANDARD
SIST-TS CEN/TS 17060:2017
01-december-2017
*QRMLOD'RORþHYDQMHPROLEGHQDYNRQFHQWUDFLMDKGR]JUDYLPHWULþQRPHWRGR
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Fertilizers - Determination of molybdenum in concentrations > 10 % using a gravimetric

method with 8-hydroxyquinoline

Düngemittel - Bestimmung von Molybdän in Konzentrationen > 10 % durch Gravimetrie

mit 8-Hydroxychinolin
Engrais - Dosage du molybdène dans des concentrations > 10 % en utilisant une
méthode gravimétrique à la 8-hydroxyquinoléine
Ta slovenski standard je istoveten z: CEN/TS 17060:2017
ICS:
65.080 Gnojila Fertilizers
SIST-TS CEN/TS 17060:2017 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TS CEN/TS 17060:2017
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SIST-TS CEN/TS 17060:2017
CEN/TS 17060
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
May 2017
TECHNISCHE SPEZIFIKATION
ICS 65.080
English Version
Fertilizers - Determination of molybdenum in
concentrations > 10 % using a gravimetric method with 8-
hydroxyquinoline
Engrais - Dosage du molybdène dans des Düngemittel - Bestimmung von Molybdän in

concentrations > 10 % en utilisant une méthode Konzentrationen > 10 % durch Gravimetrie mit 8-

gravimétrique à la 8-hydroxyquinoléine Hydroxychinolin

This Technical Specification (CEN/TS) was approved by CEN on 3 March 2017 for provisional application.

The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to

submit their comments, particularly on the question whether the CEN/TS can be converted into a European Standard.

CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS

available promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in

parallel to the CEN/TS) until the final decision about the possible conversion of the CEN/TS into an EN is reached.

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,

Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,

Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels

© 2017 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 17060:2017 E

worldwide for CEN national Members.
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SIST-TS CEN/TS 17060:2017
CEN/TS 17060:2017 (E)
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 Preparation of the test solution ................................................................................................................. 7

8.2 Precipitation ..................................................................................................................................................... 7

8.3 Filtration and washing .................................................................................................................................. 7

8.4 Weighing the precipitate .............................................................................................................................. 7

9 Calculation and expression of the results .............................................................................................. 7

10 Test report ......................................................................................................................................................... 8

Annex A (informative) Verification gravimetric method to ICP-AES method ........................................ 9

Bibliography ................................................................................................................................................................. 12

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CEN/TS 17060:2017 (E)
European foreword

This document (CEN/TS 17060:2017) has been prepared by Technical Committee CEN/TC 260

“Fertilizers and liming materials”, the secretariat of which is held by DIN.

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 announce this Technical Specification: 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.
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CEN/TS 17060:2017 (E)
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 on fertilizers in the framework of Regulation (EC) No 2003/2003 [1].

This document 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.

Determination of molybdenum in fertilizers can be executed by inductively coupled plasma-atomic

emission spectrometry (ICP-AES) according to prEN 16963:2016. The gravimetric determination as

molybdenyl oxinate is more labour intensive and skill demanding but it is an option when ICP-AES is

not available.

WARNING — Persons using this European Technical Specification should be familiar with

normal laboratory practice. This European Technical Specification 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

Technical Specification are carried out by suitably trained staff.
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SIST-TS CEN/TS 17060:2017
CEN/TS 17060:2017 (E)
1 Scope

This Technical Specification specifies a method for the determination of total and water extractable

molybdenum in mineral fertilizers containing more than 10 % molybdenum.

This method is applicable to water and aqua regia fertilizer extracts obtained according to

prEN 16962:2016 and/or prEN 16964:2016.
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

prEN 16962:2016, Fertilizers — Extraction of water soluble micro-nutrients in fertilizers and removal of

organic compounds from fertilizer extracts

prEN 16964:2016, Fertilizers — Extraction of total micro-nutrients in fertilizers and removal of organic

compounds from fertilizer extracts

EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696)

ISO 4793, Laboratory sintered (fritted) filters — Porosity grading, classification and designation

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

The molybdenum content is determined by precipitation as molybdenyl oxinate under specific

conditions.
5 Sampling and sample preparation

Sampling is not part of the method specified in this document. A recommended sampling method is

given in EN 1482-1.

Sample preparation shall be carried out in accordance with EN 1482-2. The sample extracts shall be

prepared in accordance with prEN 16962:2016 and/or prEN 16964:2016.
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CEN/TS 17060:2017 (E)
6 Reagents

All reagents shall be of recognized analytical grade and shall have negligible concentrations of

molybdenum if compared to the lowest concentration of that element in the sample solution.

6.1 Water, according to EN ISO 3696 grade 2.
6.2 Sulfuric acid, H SO , ρ = 1,84 g/ml.
2 4
6.3 Sulfuric acid solution, approximately 1 mol/l.

Carefully pour 55 ml of sulfuric acid (6.2) into a 1 l volumetric flask (7.5) containing 800 ml water (6.1).

Mix. After cooling, make up to 1 l. Mix again.
6.4 Concentrated ammonia solution, NH OH, ρ = 0,9 g/ml.
6.5 Diluted ammonia solution, volume fraction ratio = 1:3.

Mix 1 volume of concentrated ammonia solution (6.4) with 3 volumes of water (6.1).

6.6 Concentrated acetic acid, 99,7 % CH COOH, ρ = 1,049 g/ml.
6.7 Diluted acetic acid solutio
...

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