kSIST-TS FprCEN/TS 17764:2021

Inorganic fertilizers - Determination of the concentration of free, chelated or complexed micronutrients and the chelating and/or complexing agent present in compound inorganic micronutrient fertilizers

This document specifies a method for the determination of the fraction of chelated and complexed micronutrients in compound inorganic micronutrient fertilizers.

Anorganische Spurennährstoffdüngemittel - Bestimmung der Konzentration freier, chelatisierter oder komplexgebundener Spurennährstoffe sowie der Chelatbildner und/oder Komplexbildner in einem anorganischen Mehrnährstoff-Spurennährstoffdüngemittel

Dieses Dokument legt das Verfahren zur Bestimmung von freien, chelatisierten oder komplexierten Spurennährstoffen sowie von Chelat- und/oder Komplexbildnern in anorganischen Mehrnährstoff-Spuren-nährstoff-Düngemitteln fest.
Dieses Verfahren ist bei anorganischen Mehrnährstoff-Spurennährstoff-Düngemitteln anwendbar, wenn Spurennährstoffe chelatisiert und/oder komplexiert sind.
Das Verfahren basiert auf der Bestimmung der folgenden spezifischen Parameter :
—   der Konzentration der wasserlöslichen Spurennährstoffe;
—   des Anteils der chelatisierten Spurennährstoffe im Verhältnis;
—   Identifizierung der Chelatbildner EDTA, DTPA, HEEDTA, IDHA, [S,S] EDDS, [o,o] EDDHA, [o,o] EDDHMA, [o,p] EDDHA, HBED und EDDHSA;
—   des Anteils der komplexierten Spurennährstoffe;
—   Identifizierung der Komplexbildner (Ligninsulfonate, Heptaglukonsäure (HGA, en: heptagluconic acid)).
Das Verfahren basiert auf
—   der ICP- (induktiv gekoppeltes Plasma, en: inductive coupled plasma) oder FAAS- (Flammen-Atomabsorptionsspektrometrie) Messung der Konzentration von wasserlöslichen Spurennährstoffen nach EN 16963 oder EN 16965 im Anschluss an eine Extraktion nach EN 16962;
—   der LC- (Flüssigchromatographie, en: liquid chromatography) Messung der Chelatbildner nach EN 15950, EN 13368 1, EN 13368 2, EN 13368 3, EN 15451, EN 15452;
und/oder der Komplexbildner nach EN 16109 und EN 16847;
—   der Bestimmung der Konzentration von chelatisierten Spurennährstoffen wie in CEN/TS 17786 1 und/oder CEN/TS 17786 2 angegeben;
—   der Bestimmung der komplexierten Spurennährstoffe wie in EN 15962 angegeben.
Um eine Wiederholung der Analyseverfahren zu vermeiden, beschreibt CEN/TS 17786 2 die Bestimmung von Spurennährstoffen und die Identifizierung und Bestimmung von Chelatbildnern.

Engrais inorganiques - Détermination de la concentration en oligo-éléments libres, chélatés ou complexés et des agents chélatants et/ou complexants présents dans les engrais inorganiques composés à base d’oligo-éléments

Le présent document spécifie la méthode de dosage des oligo-éléments libres, chélatés ou complexés et des agents chélatants et/ou complexants présents dans les engrais inorganiques composés à base d’oligo-éléments.
Cette méthode s’applique aux engrais inorganiques composés à base d’oligo-éléments lorsque les oligo-éléments sont chélatés et/ou complexés.
La méthode est basée sur la détermination des paramètres spécifiques suivants   :
-   la concentration en oligo-éléments solubles dans l’eau ;
-   la fraction d’oligo-éléments chélatés correspondante ;
-   l’identification des agents chélatants EDTA, DTPA, HEEDTA, IDHA, [S,S]–EDDS, [o,o] EDDHA, [o,o] EDDHMA, [o,p] EDDHA, HBED et EDDHSA ;
-   la fraction d’oligo-éléments complexés ;
-   l’identification des agents complexants [lignosulfonates, acide heptagluconique (HGA)].
La méthode est basée sur :
-   un dosage par ICP (plasma à couplage inductif) ou par FAAS (spectrométrie d’absorption atomique de flamme) de la concentration en oligo-éléments solubles dans l’eau conformément à l’EN 16963 ou l’EN 16965 après extraction conformément à l’EN 16962 ;
-   un dosage par LC (chromatographie en phase liquide) des agents chélatants conformément à l’EN 15950, l’EN 13368-1, l’EN 13368-2, l’EN 13368-3, l’EN 15451, l’EN 15452 ;
et/ou des agents complexants conformément à l’EN 16109 et l’EN 16847 ;
-   la détermination de la concentration en oligo-éléments chélatés conformément à la CEN/TS 17786-1 et/ou à la CEN/TS 17786-2 ;
-   le dosage des oligo-éléments complexés conformément à l’EN 15962.
Pour éviter la duplication des méthodes analytiques, la CEN/TS 17786-2 décrit le dosage des oligo-éléments et l’identification et le dosage des agents chélatants.

Anorganska gnojila - Določevanje koncentracije prostih, kelatiranih ali kompleksiranih mikrohranil ter sredstev za kelatiranje in/ali kompleksiranje v sestavljenih anorganskih gnojilih z mikrohranili

General Information

• Status: Not Published
• Public Enquiry End Date: 02-Jan-2022
• ICS: 65.080 - Fertilizers
• Technical Committee: KAT - Soil quality
• Current Stage: 5520 - Unique Acceptance Procedure (UAP) (Adopted Project)
• Start Date: 04-Nov-2021
• Due Date: 24-Mar-2022
• Completion Date: 28-Jan-2022
• Directive: 2003/2003 - Regulation (EC) N° 2003/2003 of the European Parlament and of the council of 13 October 2003 relating to fertilisers
• Directive: 2019/1009 - Regulation (EU) 2019/1009 of the European Parliament and of the Council of 5 June 2019 laying down rules on the making available on the market of EU fertilising products and amending Regulations (EC) No 1069/2009 and (EC) No 1107/2009 and repealing Regulation (EC) No 2003/2003
• Mandate: M/564 - Fertilising products in support of Regulation (EU) 2019/1009
• Mandate: M/565 - Medical devices and in vitro diagnostic medical devices in support of Regulation (EU) 2017/745 of the European Parliament and of the Council and Regulation (EU) 2017/746
• Mandate: M/MDR - Medical devices and in vitro diagnostic medical devices in support of Regulation (EU) 2017/745 of the European Parliament and of the Council and Regulation (EU) 2017/746
• Ref Project: CEN/TS 17764:2022 - Inorganic micronutrient fertilizers - Determination of the concentration of free, chelated or complexed micronutrients and the chelating and/or complexing agents present in compound inorganic micronutrient fertilizers

Standards Content (sample)

SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 17764:2021
01-december-2021
[Not translated]

Inorganic fertilizers - Determination of the concentration of free, chelated or complexed

micronutrients and the chelating and/or complexing agent present in compound inorganic

micronutrient fertilizers
Anorganische Spurennährstoffdüngemittel - Bestimmung der Konzentration freier,
chelatisierter oder komplexgebundener Spurennährstoffe sowie der Chelatbildner
und/oder Komplexbildner in einem anorganischen Mehrnährstoff-
Spurennährstoffdüngemittel
Ta slovenski standard je istoveten z: FprCEN/TS 17764
ICS:
65.080 Gnojila Fertilizers
kSIST-TS FprCEN/TS 17764:2021 en,fr,de

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

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kSIST-TS FprCEN/TS 17764:2021
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kSIST-TS FprCEN/TS 17764:2021
FINAL DRAFT
TECHNICAL SPECIFICATION
FprCEN/TS 17764
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
November 2021
ICS 65.080
English Version
Inorganic fertilizers - Determination of the concentration
of free, chelated or complexed micronutrients and the
chelating and/or complexing agent present in compound
inorganic micronutrient fertilizers
Anorganische Spurennährstoffdüngemittel -
Bestimmung der Konzentration freier, chelatisierter
oder komplexgebundener Spurennährstoffe sowie der
Chelatbildner und/oder Komplexbildner in einem
anorganischen Mehrnährstoff-
Spurennährstoffdüngemittel

This draft Technical Specification is submitted to CEN members for Vote. It has been drawn up by the Technical Committee

CEN/TC 260.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.

Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are

aware and to provide supporting documentation.

Warning : This document is not a Technical Specification. It is distributed for review and comments. It is subject to change

without notice and shall not be referred to as a Technical Specification.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. FprCEN/TS 17764:2021 E

worldwide for CEN national Members.
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kSIST-TS FprCEN/TS 17764:2021
FprCEN/TS 17764:2021 (E)
Contents Page

European foreword ....................................................................................................................................... 3

Introduction ..................................................................................................................................................... 4

1 Scope ..................................................................................................................................................... 5

2 Normative references ..................................................................................................................... 5

3 Terms and definitions .................................................................................................................... 7

4 Principle .............................................................................................................................................. 7

5 Interferences ..................................................................................................................................... 8

6 Reagents .............................................................................................................................................. 8

7 Apparatus ............................................................................................................................................ 8

8 Sampling and sample preparation............................................................................................. 9

9 Procedure ........................................................................................................................................... 9

9.1 General ................................................................................................................................................. 9

9.2 Determination of the water-soluble micronutrient content ............................................ 9

9.2.1 Extraction ............................................................................................................................................ 9

9.2.2 Determination by ICP or AAS ....................................................................................................... 9

9.3 Determination of the chelating and/or complexing agents ........................................... 10

9.3.1 General ............................................................................................................................................... 10

9.3.2 Determination of the chelated or complexed micronutrient......................................... 10

10 Expression of results ..................................................................................................................... 10

10.1 Introduction ..................................................................................................................................... 10

10.2 Sum of water soluble micronutrient content ....................................................................... 10

10.3 Sum of chelating agents content ............................................................................................... 11

10.4 Chelated fraction (ChF) ................................................................................................................ 11

10.5 Sum of complexing agents content .......................................................................................... 12

10.6 Complexed fraction ....................................................................................................................... 12

10.7 Free micronutrients ...................................................................................................................... 12

11 Test report ........................................................................................................................................ 13

Annex A (Informative) Complete names of chelating agents ...................................................... 14

Bibliography ................................................................................................................................................... 15

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kSIST-TS FprCEN/TS 17764:2021
FprCEN/TS 17764:2021 (E)
European foreword

This document (FprCEN/TS 17764:2021) has been prepared by Technical Committee CEN/TC 260

“Fertilizers and liming materials” the secretariat of which is held by DIN.
This document is currently submitted to the Vote on TS.

This document has been prepared under a standardization request given to CEN by the European

Commission and the European Free Trade Association.
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kSIST-TS FprCEN/TS 17764:2021
FprCEN/TS 17764:2021 (E)
Introduction

Micronutrients are considered to be, in plant nutrition, a number of elements known to be needed in

small amounts for proper plant growth and development. The most common are Iron (Fe), Manganese

(Mn), Molybdenum (Mo), Copper (Cu), Zinc (Zn) and Boron (B).

If an inorganic micronutrient fertilizer contains a substance, or one of the substances in the mixture,

which is intended to enhance the long term availability to plants of micronutrients in the EU fertilizing

products, that substance is either a chelating agent or a complexing agent.

In this document the test method is defined to be used in order to determine free, chelated or

complexed micronutrients and chelating and/or complexing agents present in compound inorganic

micronutrient fertilizers (classified as product function category (PFC) 1(C)(II)(b) according to

Regulation (EU) 2019/1009 [7]).

This method allows the determination of the content of Co, Cu, Fe, Mn, Zn as free and/or chelated

and/or complexed micronutrients.
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kSIST-TS FprCEN/TS 17764:2021
FprCEN/TS 17764:2021 (E)
1 Scope

This document specifies the method for the determination of free, chelated or complexed

micronutrients and chelating and/or complexing agents present in compound inorganic micronutrient

fertilizers.

This method applies to compound inorganic micronutrient fertilizers when micronutrients are

chelated and/or complexed.

The method is based on the determination of the following specific determinations :

— the water-soluble micronutrient concentration;
— the fraction of chelated micronutrients in relation;

— identification of chelating agents EDTA, DTPA, HEEDTA, IDHA, [S,S]–EDDS, [o,o] EDDHA,

[o,o] EDDHMA, [o,p] EDDHA, HBED and EDDHSA;
— the fraction of complexed micronutrients;

— identification of complexing agents (lignosulfonates, heptagluconic acid (HGA)).

The method is based on

— ICP (inductive coupled plasma) or AAS (atomic absorption spectrometry) measurement of the

concentration of water-soluble micronutrients according to EN 16963 or EN 16965 after

extraction according to EN 16962;

— LC (liquid chromatography) measurement of the chelating agents according to EN 15950,

EN 13368-1, EN 13368-2, EN 13368-3, EN 15451, EN 15452;
and/or complexing agents according EN 16109 and EN 16847;

— determination of the concentration of chelated micronutrients by FprCEN/TS 00260286 and/or

FprCEN/TS 00260287;
— determination of the complexed micronutrients by EN 15962.

To avoid duplication of the analytical methods, FprCEN/TS 00260287 describes the determination of

micronutrients and the identification and determination of chelating agents.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. 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 terms

EN 12944-2, Fertilizers and liming materials and soil improvers - Vocabulary - Part 2: Terms relating to

fertilizers
Abbreviated terms are described in Annex A.
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EN 13368-1, Fertilizers - Determination of chelating agents in fertilizers by chromatography - Part 1:

Determination of EDTA, HEEDTA and DTPA by ion chromatography

EN 13368-2, Fertilizers - Determination of chelating agents in fertilizers by chromatography - Part 2:

Determination of Fe chelated by [o,o] EDDHA, [o,o] EDDHMA and HBED, or the amount of chelating

agents, by ion pair chromatography

EN 13368-3, Fertilizers - Determination of chelating agents in fertilizers by chromatography - Part 3:

Determination of [S,S]-EDDS by ion pair chromatography

EN 15451, Fertilizers - Determination of chelating agents - Determination of iron chelated by EDDHSA

by ion pair chromatography

EN 15452, Fertilizers - Determination of chelating agents - Determination of iron chelated by o,p-EDDHA

by reversed phase HPLC

EN 15950, Fertilizers - Determination of N-(1,2-dicarboxyethyl)-D,L-aspartic acid (Iminodisuccinic acid,

IDHA) using high-performance liquid chromatography (HPLC)

EN 15962, Fertilizers - Determination of the complexed micro-nutrient content and of the complexed

fraction of micro-nutrients

EN 16109, Fertilizers - Determination of complexed micro-nutrient ions in fertilizers - Identification of

lignosulfonates

EN 16847, Fertilizers - Determination of complexing agents in fertilizers - Identification of heptagluconic

acid by chromatography

EN 16962, Fertilizers - Extraction of water soluble micro-nutrients in fertilizers and removal of organic

compounds from fertilizer extracts

EN 16963, Fertilizers - Determination of boron, cobalt, copper, iron, manganese, molybdenum and zinc

using ICP-AES

EN 16965, Fertilizers - Determination of cobalt, copper, iron, manganese and zinc using flame atomic

absorption spectrometry (FAAS)

FprCEN/TS 17786-1, Inorganic micronutrient fertilizers — Determination of the chelated micronutrient

content and the chelated fraction of micronutrients — Part 1: Treatment with a cation exchange resin

FprCEN/TS 17786-2, Inorganic micronutrient fertilizers — Determination of the chelated micronutrient

content and the chelated fraction of micronutrients — Part 2: Determination of EDTA, DTPA, HEEDTA,

IDHA or EDDS
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kSIST-TS FprCEN/TS 17764:2021
FprCEN/TS 17764:2021 (E)
3 Terms and definitions

For the purposes of this document, the terms and definitions given in EN 12944-1 and EN 12944-2 and

the following apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— IEC Electropedia: available at https://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
3.1
free micronutrient concentration

difference between the water-soluble micronutrient concentration and the sum of the chelating and

complexing agents concentration
4 Principle

The principle of the method is to determine the concentration of micronutrients and the chelating

and/or complexing agents present in compound inorganic micronutrient fertilizer.

The content of the water-soluble micronutrient is determined using ICP or AAS methods using

EN 16963 or EN 16965 standards after previous extraction using the EN 16962:2018.

The content of the chelating agent is determined using one of the following methods:

— EN 13368-1 for EDTA, DTPA and HEEDTA;
— EN 13368-2 for [o,o] EDDHA, [o,o] EDDHMA, [o,p] EDDHMA and HBED;
— EN 13368-3 for [S,S]–E
...