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

This document specifies a method for the determination of the chelated fraction of micronutrients for fertilizers containing one or many micronutrients chelated by EDTA, DTPA, HEEDTA, IDHA or [S,S]-EDDS in fertilizers.
This method is used for inorganic micronutrient fertilizers when micronutrients are chelated only by EDTA, DTPA, HEEDTA, IDHA or [S,S]-EDDS or for mixtures in which EDTA, DTPA, HEEDTA, IDHA or [S,S]-EDDS is one of the chelating agents.
The method is applicable to all inorganic micronutrient fertilizers containing EDTA, DTPA, HEEDTA, IDHA or [S,S]-EDDS as chelating agent for contents > 0,1 % (w/w).
The method is based on ICP or AAS measurement of the concentration of micronutrients according to EN 16963 or EN 16965 after water extraction according to EN 16962 and LC measurement of the chelating agents according to EN 15950, EN 13368-1 and EN 13368-3.

Anorganische Spurennährstoff-Düngemittel - Bestimmung des Gehaltes an chelatisierten Spurennährstoffen und des chelatisierten Anteils an Spurennährstoffen - Teil 2: Bestimmung von EDTA, DTPA, HEEDTA, IDHA oder EDDS

Dieses Dokument legt ein Verfahren zur Bestimmung des Gehalts an chelatisiertem Eisen sowie des chelatisierten Anteils an Eisen in UVCB-Chelaten, EDDHA, EDDHMA, HBED und EDDHSA in anorganischen Spurennährstoff-Düngemitteln durch Behandlung mit einem Kationenaustauschharz fest.
Die Bestimmungsgrenze des Gehalts an chelatisiertem Eisen hängt stark von der spezifischen elektrischen Leitfähigkeit der Probe und der Menge des vorhandenen Nährstoffs ab und variiert zwischen 0,005 % in einfachen Matrices mit großen Mengen an Spurennährstoffen und 0,5 % in komplexeren Fällen (siehe 9.1).

Engrais inorganiques à base d'oligo-éléments - Détermination de la teneur en oligo-éléments chélatés et de la fraction chélatée des oligo-éléments - Partie 2 : Dosage de l'EDTA, du DTPA, du HEEDTA, de l'IDHA ou de l'EDDS

Le présent document spécifie une méthode pour la détermination de la fraction chélatée des oligo-éléments pour les engrais contenant un ou plusieurs oligo-éléments chélatés par de l’EDTA, du DTPA, du HEEDTA, de l’IDHA ou du [S,S]-EDDS dans les engrais.
Cette méthode est utilisée pour les engrais inorganiques à base d’oligo-éléments lorsque les oligo-éléments sont chélatés uniquement par de l’EDTA, du DTPA, du HEEDTA, de l’IDHA ou du [S,S]-EDDS ou pour des mélanges dans lesquels l’EDTA, le DTPA, le HEEDTA, l’IDHA ou le [S,S]-EDDS est l’un des agents chélatants.
La méthode est applicable à tous les engrais inorganiques à base d’oligo-éléments contenant de l’EDTA, du DTPA, du HEEDTA, de l’IDHA ou du [S,S]-EDDS comme agent chélatant pour des teneurs > 0,1 % (w/w).
La méthode est basée sur un dosage par ICP ou par AAS de la concentration en oligo-éléments conformément à l’EN 16963 ou l’EN 16965 après extraction à l’eau conformément à l’EN 16962, et sur un dosage par LC des agents chélatants conformément à l’EN 15950, l’EN 13368-1 et l’EN 13368-3.

Anorganska gnojila z mikrohranili - Določanje vsebnosti kelatiranih mikrohranil in deleža kelatiranih mikrohranil - 2. del: Določevanje EDTA, DTPA, HEEDTA, IDHA ali EDDS

Ta dokument navaja metodo za določanje kelatiranega deleža mikrohranil za gnojila, kadar je eno ali več mikrohranil v gnojilih kelatirano z EDTA, DTPA, HEEDTA, IDHA ali [S,S]-EDDS.
Ta metoda se uporablja za anorganska gnojila z mikrohranili, kadar so mikrohranila kelatirana samo z EDTA, DTPA, HEEDTA, IDHA ali [S,S]-EDDS, ali za mešanice, v katerih je EDTA, DTPA, HEEDTA, IDHA ali [S,S]-EDDS eno od sredstev za kelatiranje.
Metoda je uporabna za vsa anorganska gnojila z mikrohranili, ki vsebujejo EDTA, DTPA, HEEDTA, IDHA ali [S,S]-EDDS kot sredstvo za kelatiranje za vsebnosti > 0,1 % (g/100 g).
Metoda temelji na meritvi ICP ali AAS koncentracije mikrohranil v skladu s standardom EN 16963 ali EN 16965 po vodni ekstrakciji v skladu s standardom EN 16962 in meritvi LC sredstev za kelatiranje v skladu s standardi EN 15950, EN 13368-1 in EN 13368-3.

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 vsebnosti kelatiranih mikrohranil in
deleža kelatiranih mikrohranil - 2. del: Določevanje EDTA, DTPA, HEEDTA, IDHA ali
EDDS
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
Anorganische Spurennährstoff-Düngemittel - Bestimmung des Gehaltes an chelatisierten
Spurennährstoffen und des chelatisierten Anteils an Spurennährstoffen - Teil 2:
Bestimmung von EDTA, DTPA, HEEDTA, IDHA oder EDDS
Engrais inorganiques à base d'oligo-éléments - Détermination de la teneur en oligo-
éléments chélatés et de la fraction chélatée des oligo-éléments - Partie 2 : Dosage de
l'EDTA, du DTPA, du HEEDTA, de l'IDHA ou de l'EDDS
Ta slovenski standard je istoveten z: CEN/TS 17786-2:2022
ICS:
65.080 Gnojila Fertilizers
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

CEN/TS 17786-2
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
April 2022
TECHNISCHE SPEZIFIKATION
ICS 65.080
English Version
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
Engrais inorganiques à base d'oligo-éléments - Anorganische Spurennährstoffdüngemittel -
Détermination de la teneur en oligo-éléments chélatés Bestimmung des Gehaltes an chelatisierten
et de la fraction chélatée des oligo-éléments - Partie 2 : Spurennährstoffen und des chelatisierten Anteils an
Dosage de l'EDTA, du DTPA, du HEEDTA, de l'IDHA ou Spurennährstoffen - Teil 2: Bestimmung von EDTA,
de l'EDDS DTPA, HEEDTA, IDHA oder EDDS
This Technical Specification (CEN/TS) was approved by CEN on 21 February 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 17786-2:2022 E
worldwide for CEN national Members.

Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 6
5 Interferences . 6
6 Reagents . 6
7 Apparatus . 7
8 Sampling and sample preparation. 7
9 Procedure . 7
9.1 General . 7
9.2 Water-soluble micronutrient content . 7
9.3 Chelating agent content . 7
10 Expression of results . 8
10.1 Water-soluble micronutrient content . 8
10.2 Chelating agent content . 8
10.3 Chelated fraction (ChF) . 9
11 Test report . 9
Annex A (informative) Complete names of chelating agents . 10
Bibliography . 11

European foreword
This document (CEN/TS 17786-2:2022) 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
product, that substance is either a chelating agent or a complexing agent.
The chelating agents are divided into two groups :
— Group 1: EDTA, DTPA, HEEDTA, IDHA and [S,S]-EDDS;
— Group 2: Chelating agents present in UVCB (unknown or variable composition, complex reaction
products and biological materials) chelates including [o,o] EDDHA , [o,p] EDDHA , [o,o] EDDHMA,
HBED and EDDHSA.
This document defines the test method to be used in order to measure the compliance with the
chelated fraction of micronutrients in product function category (PFC) 1(C) (II) (classified according
to Regulation (EU) 2019/1009 [7]) as inorganic micronutrient fertilizer containing one or more
chelating agents of Group 1.
Abbreviated terms are described in Annex A.
1 Scope
This document specifies a method for the determination of the chelated fraction of micronutrients for
fertilizers containing one or many micronutrients chelated by EDTA, DTPA, HEEDTA, IDHA or [S,S]-
EDDS in fertilizers.
This method is used for inorganic micronutrient fertilizers when micronutrients are chelated only by
EDTA, DTPA, HEEDTA, IDHA or [S,S]-EDDS or for mixtures in which EDTA, DTPA, HEEDTA, IDHA or
[S,S]-EDDS is one of the chelating agents.
The method is applicable to all inorganic micronutrient fertilizers containing EDTA, DTPA, HEEDTA,
IDHA or [S,S]-EDDS as chelating agent for contents > 0,1 % (w/w).
The method is based on ICP or AAS measurement of the concentration of micronutrients according to
EN 16963 or EN 16965 after water extraction according to EN 16962 and LC measurement of the
chelating agents according to EN 15950, EN 13368-1 and EN 13368-3.
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
EN 13368-3, Fertilizers — Determination of chelating agents in fertilizers by chromatography — Part 3:
Determination of [S,S]-EDDS by ion pair chromatography
EN 15950, Fertilizers — Determination of N-(1,2-dicarboxyethyl)-D,L-aspartic acid (Iminodisuccinic
acid, IDHA) using high-performance liquid chromatography (HPLC)
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)
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:
— ISO Online browsing platform: available at https://www.iso.org/obp
— IEC Electropedia: available at https://www.electropedia.org/
3.1
chelated fraction
ChF
chelating agent content divided by the water-soluble micronutrient content
Note 1 to entry: The chelated fraction (ChF) is expressed as a percentage.
4 Principle
The principle of the method is to determine the content of micronutrients and the content of one or
more chelating agents declared in the fertilizer followed by calculating the chelated fraction.
The content of micronutrients is determined using ICP-AES (inductive coupled plasma atomic
emission spectrometry) or FAAS (flame atomic absorption spectrometry) methods using EN 16963 or
EN 16965 standards after previous extraction using the EN 16962 method.
The content of the declared chelating agent is determined using one of the following methods:
— for EDTA, DTPA and HEEDTA, EN 13368-1 shall be used;
— for [S,S]-EDDS, EN 13368-3 shall be used;
— for IDHA, EN 15950 shall be used.
The chelated fraction is calculated by comparing the water soluble micronutrient content with the
chelating agent content.
5 Interferences
Other chelating agents such as DTPA, [o,o] EDDHA or [o,p] EDDHA do not interfere the determination
of IDHA. EDTA may interfere with the determination of IDHA with some equipment, especially with
certain columns in the HPLC-equipment.
In case of [S,S]-EDDS no interferences have been detected. Metal chelates with [o,o] EDDHA,
[o,o] EDDHMA, HBED, EDDHSA, EDTA, DTPA, HEEDTA, IDHA, [o,p] EDDHA, lignosulfonates and
heptagluconates as well as the chelating agents do not interfere since after Cu derivatization they are
separate from Cu-[S,S]-EDDS. Since retention times depend on the column type, interferences should
be checked if a mixture with other chelating or complexing agents is suspected.
6 Reagents
6.1 Water
All water used should conform to EN ISO 3696 and be degassed.
6.2 Reagents of recognized analytical grade.
Those included in the following standards shall be used:
— EN 16962, when extracting boron, cobalt, copper, iron, manganese, molybdenum and zinc;
— EN 16963, when determining the content of boron, cobalt, copper, iron, manganese, molybdenum
and zinc by ICP-AES;
— EN 16965, when determining the content of cobalt, copper, iron, manganese and zinc by FAAS;
— EN 13368-1, when determining the content of EDTA, HEEDTA and DTPA;
— EN 13368-3, when determining the content of [S,S]-EDDS;
— EN 15950, when determining the content of IDHA.
7 Apparatu
...

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