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

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 parameters :
-   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 FAAS (flame 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 to EN 16109 and EN 16847;
-   determination of the concentration of chelated micronutrients by CEN/TS 17786-1 and/or CEN/TS 17786-2;
-   determination of the complexed micronutrients by EN 15962.
To avoid duplication of the analytical methods, CEN/TS 17786-2 describes the determination of micronutrients and the identification and determination of chelating agents.

Anorganische Spurennährstoff-Düngemittel - Bestimmung der Konzentration freier, chelatisierter oder komplexierter Spurennährstoffe sowie der Chelatbildner und/oder Komplexbildner in einem anorganischen Mehrnährstoff-Spurennährstof-Düngemittel

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

Ta dokument določa metodo za določanje deleža kelatiranih in kompleksnih mikrohranil v sestavljenih anorganskih gnojilih z mikrohranili.

General Information

Status
Published
Publication Date
05-Apr-2022
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
06-Apr-2022
Due Date
28-Jan-2023
Completion Date
06-Apr-2022

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SLOVENSKI STANDARD
01-februar-2023
Anorganska gnojila z mikrohranili - Določanje koncentracije prostih, kelatiranih ali
kompleksiranih mikrohranil ter sredstev za kelatiranje in/ali kompleksiranje v
sestavljenih anorganskih gnojilih z mikrohranili
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
Anorganische Spurennährstoff-Düngemittel - Bestimmung der Konzentration freier,
chelatisierter oder komplexierter Spurennährstoffe sowie der Chelatbildner und/oder
Komplexbildner in einem anorganischen Mehrnährstoff-Spurennährstof-Düngemittel
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
Ta slovenski standard je istoveten z: CEN/TS 17764:2022
ICS:
65.080 Gnojila Fertilizers
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

CEN/TS 17764
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
April 2022
TECHNISCHE SPEZIFIKATION
ICS 65.080
English Version
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
Engrais inorganiques - Détermination de la Anorganische Spurennährstoffdüngemittel -
concentration en oligo-éléments libres, chélatés ou Bestimmung der Konzentration freier, chelatisierter
complexés et des agents chélatants et/ou complexants oder komplexgebundener Spurennährstoffe sowie der
présents dans les engrais inorganiques composés à Chelatbildner und/oder Komplexbildner in einem
base d'oligo-éléments anorganischen Mehrnährstoff-
Spurennährstoffdüngemittel
This Technical Specification (CEN/TS) was approved by CEN on 13 March 2022 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, 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.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 17764:2022 E
worldwide for CEN national Members.

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 . 9
8 Sampling and sample preparation. 9
9 Procedure . 9
9.1 General . 9
9.2 Determination of the water-soluble micronutrient content . 10
9.2.1 Extraction . 10
9.2.2 Determination by ICP or FAAS . 10
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 . 11
10.1 Sum of water-soluble micronutrient content . 11
10.2 Sum of chelating agents content . 11
10.3 Chelated fraction (ChF) . 12
10.4 Sum of complexing agents content . 12
10.5 Complexed fraction . 12
10.6 Free micronutrients . 13
11 Test report . 13
Annex A (informative) Complete names of chelating agents . 14
Bibliography . 15

European foreword
This document (CEN/TS 17764:2022) 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 Standardization Request given to CEN by the European
Commission and the European Free Trade Association.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
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, 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 the United Kingdom.
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.
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 parameters :
— 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 FAAS (flame 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 to EN 16109 and EN 16847;
— determination of the concentration of chelated micronutrients by CEN/TS 17786-1 and/or
CEN/TS 17786-2;
— determination of the complexed micronutrients by EN 15962.
To avoid duplication of the analytical methods, CEN/TS 17786-2 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 — Vocabulary — Part 1: General terms
EN 12944-2, Fertilizers and liming materials — Vocabulary — Part 2: Terms relating to fertilizers
EN 13368-1, Fertilizers — Determination of chelating agents in fertilizers by chromatography — Part 1:
Determination of EDTA, HEEDTA and DTPA by ion chromatography

Abbreviated terms are described in Annex A.
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)
CEN/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
CEN/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
CEN/T
...

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