CEN/TS 17786-1:2022
(Main)Inorganic micronutrient fertilizers - Determination of the chelated micronutrient content and the chelated fraction of micronutrients - Part 1: Treatment with a cation exchange resin
Inorganic micronutrient fertilizers - Determination of the chelated micronutrient content and the chelated fraction of micronutrients - Part 1: Treatment with a cation exchange resin
This document specifies a method for the determination of the chelated iron content and the chelated fraction of iron, in UVCB chelats, EDDHA, EDDHMA, HBED, EDDHSA, in inorganic micronutrient fertilizers by the treatment with a cation exchange resin.
The limit of determination of the chelated iron content highly depends on the specific electrical conductivity of the sample, on the amount of nutrient present, and varies between 0,005 % in simple matrices with high amounts of micronutrient and 0,5 % in more complex cases (see 9.1).
Anorganische Spurennährstoff-Düngemittel - Bestimmung des Gehaltes an chelatisierten Spurennährstoffen und des chelatisierten Anteils an Spurennährstoffen - Teil 1: Behandlung mit einem Kationenaustauscherharz
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 1 : Traitement avec une résine échangeuse de cations
Le présent document spécifie une méthode pour la détermination de la teneur en fer chélaté et de la fraction chélatée de fer, dans les chélates UVCB, l’EDDHA, l’EDDHMA, le HBED, l’EDDHSA, dans les engrais inorganiques à base d’oligo-éléments par traitement avec une résine échangeuse de cations.
La limite de détermination de la teneur en fer chélaté dépend en grande partie de la conductivité électrique spécifique de l’échantillon, de la quantité d’élément nutritif présent, et varie entre 0,005 % dans les matrices simples avec de grandes quantités d’oligo-éléments et 0,5 % dans les cas plus complexes (voir 9.1).
Anorganska gnojila z mikrohranili - Določanje vsebnosti kelatiranih mikrohranil in deleža kelatiranih mikrohranil - 1. del: Obdelava s kationsko izmenjevalno smolo
Ta dokument navaja metodo za določanje vsebnosti kelatiranega železa in kelatiranega deleža železa v UVCB, EDDHA, EDDHMA, HBED, EDDHSA v anorganskih gnojilih z mikrohranili na podlagi obdelave s kationsko izmenjevalno smolo.
Meja določanja vsebnosti kelatiranega železa je močno odvisna od specifične električne prevodnosti vzorca, od količine prisotnega hranila in se giblje med 0,005 % v enostavnih matricah z velikimi količinami mikrohranil in 0,5 % v bolj zapletenih primerih (glej točko 9.1).
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-februar-2023
Anorganska gnojila z mikrohranili - Določanje vsebnosti kelatiranih mikrohranil in
deleža kelatiranih mikrohranil - 1. del: Obdelava s kationsko izmenjevalno smolo
Inorganic micronutrient fertilizers - Determination of the chelated micronutrient content
and the chelated fraction of micronutrients - Part 1: Treatment with a cation exchange
resin
Anorganische Spurennährstoff-Düngemittel - Bestimmung des Gehaltes an chelatisierten
Spurennährstoffen und des chelatisierten Anteils an Spurennährstoffen - Teil 1:
Behandlung mit einem Kationenaustauscherharz
Engrais inorganiques à base d'oligo-éléments - Détermination de la teneur en oligo-
éléments chélatés et de la fraction chélatée des oligo-éléments - Partie 1 : Traitement
avec une résine échangeuse de cations
Ta slovenski standard je istoveten z: CEN/TS 17786-1:2022
ICS:
65.080 Gnojila Fertilizers
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
CEN/TS 17786-1
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 1: Treatment with a cation
exchange resin
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 1 : Spurennährstoffen und des chelatisierten Anteils an
Traitement avec une résine échangeuse de cations Spurennährstoffen - Teil 1: Behandlung mit einem
Kationenaustauscherharz
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 17786-1:2022 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 . 8
9 Procedure . 8
9.1 Extraction of the sample . 8
9.2 pH adjustment . 9
9.3 Ion exchange separation . 9
9.4 Spectrometric determination .10
9.5 Water soluble iron content determination .10
10 Expression of results .10
10.1 Chelated iron content in the fertilizer .10
10.2 Chelated fraction of iron in the fertilizer .10
11 Test report .11
Annex A (informative) Complete names of chelating agents.12
Bibliography .13
European foreword
This document (CEN/TS 17786-1:2022) 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; and
— Group 2: Chelating agents present in UVCB (unknown or variable composition, complex reaction
products or biological materials) chelates including [o,o] EDDHA, [o,p] EDDHA, [o,o] EDDHMA,
HBED and [o,o] EDDHSA.
This document defines the test method to be used in order to measure the compliance with the
chelated fraction of iron in product function category (PFC) 1(C) (II)(a) (classified according to
Regulation (EU) 2019/1009 [9]) for fertilizers containing one or more chelating agents of Group 2.
Abbreviated terms are described in Annex A.
1 Scope
This document specifies a method for the determination of the chelated iron content and the chelated
fraction of iron, in UVCB chelates, EDDHA, EDDHMA, HBED, EDDHSA, in inorganic micronutrient
fertilizers by the treatment with a cation exchange resin.
The limit of determination of the chelated iron content highly depends on the specific electrical
conductivity of the sample, on the amount of nutrient present, and varies between 0,005 % in simple
matrices with high amounts of micronutrient and 0,5 % in more complex cases (see 9.1).
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
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 of a micronutrient
ratio of the chelated micronutrient content and the water-soluble micronutrient content
Note 1 to entry: The chelated fraction of a micronutrient is expressed as a percentage.
4 Principle
The sample is extracted with water and the extract adjusted to a neutral pH. The chelated forms of an
element thus having a negative and/or neutral charge are not retained by an ion exchange resin of the
strong sulfonated cationic type, and are separated from the non-chelated forms, having a cationic
nature. The chelated forms are collected and their content determined by spectrometry, as well as the
water soluble content.
5 Interferences
Any substance combining with a micronutrient to form a stable, negative or uncharged compound
(chelate or complex) at neutral pH, will prevent the retention by the resin, and account for a certain
degree of chelation. This is the case for many complexing agents, e.g. amino acids, citrate, and for
chelating agents other than EDTA, HEEDTA, DTPA, [o,o] EDDHA and [o,o] EDDHMA.
In order to determine the presence of the statutory chelating agents in the sample, EN 13368-1 and
EN 13368-2 should be applied.
In some cases, especially where complex fertilizer matrices with high amounts of phosphate are
handled, or where micronutrients with a low chelated fraction are present, slow precipitation
reactions can occur during the contact with the resin, causing equilibrium shifts, adsorption,
decreasing the exchange capacity and leading to inaccurate and imprecise results. It is advised to
proceed as soon as possible with all steps. Highly unstable solutions cannot be considered.
6 Reagents
All reagents shall be of recognized analytical grade.
6.1 Water
All water used should conform to EN ISO 3696 and be degassed.
6.2 Sulfonated cationic exchange resin
6.2.1 General
Polystyrene divinylbenzene (PS-DVB) copolymer, slightly crosslinked (mass fraction of DVB less than
or equal to 8 %), in sodic or protonic form, free from Co, Cu, Fe, Mn, and Zn .
6.2.2 Preparation and determination of cationic exchange capacity
Protonate the resin prior to use, transform to the sodic form, to eliminate any contamination and
measure the cationic exchange capacity (CEC) of the sodic resin in wet form as follows:
Transfer 50 g of resin to a 500 ml beaker and add 250 ml of hydrochloric acid solution (6.4).
Place on a magnetic stirrer. After one hour of moderate stirring, the suspension is transferred onto the
sieve (7.1). The resin is recovered and transferred back to the beaker. The acidification and separation
operations are repeated as described. At the end of the second operation, the protonated resin present
on the sieve is washed thoroughly with water until the rinsing water is free from chloride when tested
with silver nitrate.
Dowex® 50 x 4-400, Amberlite® IR 120 or equivalent are examples of suitable products available
commercially. This information is given for the convenience of users of this document and does not constitute
an endorsement by CEN of these products.
Transfer the wet protonated resin int
...
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