Organo-mineral fertilizers - Identification of chelating agents - Part 1: Determination of EDTA, HEEDTA and DTPA by ion chromatography

This document specifies a method for the determination by ion chromatography of the total amount of each of the individual chelating agents EDTA, HEEDTA, and DTPA in organo-mineral fertilizers, having an organic matrix based on vegetal residues (cocoa shells, grape residue, soybean residue, ...), algae extract, and animal meal (feather, bones, blood, ...) and containing one or more of these substances.
The method allows the identification and the determination of the total water-soluble fraction of each of these chelating agents. It does not allow to distinguish between the free form and the metal bound form of the chelating agents.
This method applies to organo-mineral fertilizers containing chelates of one or more of the following micronutrients: cobalt, copper, iron, manganese, zinc and with a mass fraction of at least 0,1 %.

Organisch-mineralische Düngemittel - Identifizierung von Chelatbildnern - Teil 1: Bestimmung von EDTA, HEEDTA und DTPA mittels Ionenchromatographie

Dieses Dokument legt ein Verfahren zur ionenchromatographischen Bestimmung des Gesamtgehalts der einzelnen Chelatbildner EDTA, HEEDTA und DTPA in organisch-mineralischen Düngemitteln fest, die eine organische Matrix auf Basis von pflanzlichen Reststoffen (Kakaoschalen, Traubenreststoffe, Sojabohnenreststoffe usw.), Algenextrakt und Tiermehl (Federn, Knochen, Blut usw.) aufweisen und einen oder mehrere dieser Stoffe enthalten.
Das Verfahren erlaubt die Identifizierung und die Bestimmung des gesamten wasserlöslichen Anteils jedes einzelnen der genannten Chelatbildner. Es erlaubt nicht die Unterscheidung zwischen der freien und der metallgebundenen Form der Chelatbildner.
Das Verfahren ist auf organisch-mineralische Düngemittel anwendbar, die Chelate eines oder mehrerer der folgenden Spurennährstoffe aufweisen: Kobalt, Kupfer, Eisen, Mangan, Zink mit einem Massenanteil von mindestens 0,1 %.

Engrais organo-minéraux - Identification des agents chélatants - Partie 1 : Détermination de l'EDTA, de l'HEEDTA et du DTPA par chromatographie ionique

Le présent document spécifie une méthode pour la détermination par chromatographie ionique de la quantité totale de chacun des agents chélatants individuels, à savoir EDTA, HEEDTA et DTPA, dans les engrais organo-minéraux ayant une matrice organique basée sur des résidus végétaux (coques de cacao, résidus de raisins, résidus de soja …), des extraits d’algue et des farines animales (plumes, os, sang ...) et contenant une ou plusieurs de ces substances.
La méthode permet l’identification et la détermination de la fraction totale soluble dans l’eau de chacun de ces agents chélatants. Elle ne permet pas de faire la distinction entre la forme libre et la forme métallique de l’agent chélatant.
La présente méthode s’applique aux engrais organo-minéraux contenant des chélates d’au moins un des oligo-éléments suivants : cobalt, cuivre, fer, manganèse, zinc, avec une fraction massique d’au moins 0,1 %.

Organsko-mineralna gnojila - Identifikacija sredstev za kelatiranje - 1. del: Določevanje EDTA, HEEDTA in DTPA z ionsko kromatografijo

Ta dokument navaja metodo za določanje skupne količine vsakega od posameznih sredstev za kelatiranje EDTA, HEEDTA in DTPA z ionsko kromatografijo v organsko-mineralnih gnojilih, ki imajo organsko matrico na osnovi rastlinskih ostankov (kakavovih lupin, ostankov grozdja, soje ...), izvlečkov alg in živalske moke (perje, kosti, kri ...) ter vsebujejo eno ali več teh snovi.
Metoda omogoča opredelitev in določevanje skupnega v vodi topnega deleža vsakega od teh sredstev za kelatiranje. Metoda ne dopušča razlikovanja med prosto obliko sredstva za kelatiranje in obliko sredstva za kelatiranje, vezano na kovino.
Ta metoda se uporablja za organsko-mineralna gnojila, ki vsebujejo kelate enega ali več naslednjih mikrohranil: kobalta, bakra, železa, mangana, cinka, in sicer z masnim deležem najmanj 0,1 %.

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
SIST-TS CEN/TS 17789-1:2023
01-februar-2023
Organsko-mineralna gnojila - Identifikacija sredstev za kelatiranje - 1. del:
Določevanje EDTA, HEEDTA in DTPA z ionsko kromatografijo
Organo-mineral fertilizers - Identification of chelating agents - Part 1: Determination of
EDTA, HEEDTA and DTPA by ion chromatography
Organisch-mineralische Düngemittel - Identifizierung von Chelatbildnern - Teil 1:
Bestimmung von EDTA, HEEDTA und DTPA mittels Ionenchromatographie
Engrais organo-minéraux - Identification des agents chélatants - Partie 1 : Détermination
de l'EDTA, de l'HEEDTA et du DTPA par chromatographie ionique
Ta slovenski standard je istoveten z: CEN/TS 17789-1:2022
ICS:
65.080 Gnojila Fertilizers
SIST-TS CEN/TS 17789-1:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST-TS CEN/TS 17789-1:2023

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SIST-TS CEN/TS 17789-1:2023


CEN/TS 17789-1
TECHNICAL SPECIFICATION

SPÉCIFICATION TECHNIQUE

April 2022
TECHNISCHE SPEZIFIKATION
ICS 65.080
English Version

Organo-mineral fertilizers - Identification of chelating
agents - Part 1: Determination of EDTA, HEEDTA and
DTPA by ion chromatography
Engrais organo-minéraux - Identification des agents Organisch-mineralische Düngemittel - Identifizierung
chélatants - Partie 1 : Détermination de l'EDTA, de von Chelatbildnern - Teil 1: Bestimmung von EDTA,
l'HEEDTA et du DTPA par chromatographie ionique HEEDTA und DTPA mittels Ionenchromatographie
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 17789-1:2022 E
worldwide for CEN national Members.

---------------------- Page: 3 ----------------------
SIST-TS CEN/TS 17789-1:2023
CEN/TS 17789-1:2022 (E)
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 5
5 Interferences . 5
6 Reagents . 6
7 Apparatus . 7
8 Sampling and sample preparation . 8
9 Procedure . 8
9.1 Preparation of the test solution . 8
9.2 Preparation of the standard solutions . 8
9.3 Chromatographic analysis . 8
10 Expression of results . 9
11 Test report . 9
Annex A (informative) Complete names of chelating agents . 10
Annex B (informative) Chromatogram . 11
Bibliography . 12

2

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SIST-TS CEN/TS 17789-1:2023
CEN/TS 17789-1:2022 (E)
European foreword
This document (CEN/TS 17789-1:2022) 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.

3

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SIST-TS CEN/TS 17789-1:2023
CEN/TS 17789-1:2022 (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 organo-mineral 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.
1
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 or biological materials) chelates including [o,o] EDDHA, [o,p] EDDHA, [o,o] EDDHMA, HBED
and EDDHSA.
This document specifies the test method to be used in order to determine the content of certain chelating
agents (EDTA, DTPA and HEEDTA) in organo-mineral fertilizers (product function category (PFC) 1(B)
according to Regulation (EU) 2019/1009 [4]).


1
Abbreviated terms are described in Annex A.
4

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SIST-TS CEN/TS 17789-1:2023
CEN/TS 17789-1:2022 (E)
1 Scope
This document specifies a method for the determination by ion chromatography of the total amount of
each of the individual chelating agents EDTA, HEEDTA, and DTPA in organo-mineral fertilizers, having an
organic matrix based on vegetal residues (cocoa shells, grape residue, soybean residue, …), algae extract,
and animal meal (feather, bones, blood, .) and containing one or more of these substances.
The method allows the identification and the determination of the total water-soluble fraction of each of
these chelating agents. It does not allow to distinguish between the free form and the metal bound form
of the chelating agents.
This method applies to organo-mineral fertilizers containing chelates of one or more of the following
micronutrients: cobalt, copper, iron, manganese, zinc and with a mass fraction of at least 0,1 %.
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 — Vocabulary — Part 1: General terms
EN 12944-2, Fertilizers and liming materials — Vocabulary — Part 2: Terms relating to fertilizers
3 Terms and definitions
For the purposes of this document, the terms and definitions given in EN 12944-1 and EN 12944-2 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/
4 Principle
The micronutrients associated with the chelating agents present in an aqueous extract of the sample are
replaced by iron(III). The iron chelates are separated and determined by ion chromatography. The
separation is based on anion exchange, by elution with a nitrate acetate solution. The detection is based
on UV photometry at 330 nm, after post-column reaction with diluted perchloric acid.
5 Interferences
Several substances can interfere, to a degree largely dependent on the type of column used. With the
column described in 7.2, the following phenomena have been observed.
a) Injection of solutions having high concentrations of salts can cause shifts in the retention times,
mostly decreasing the retention when compared to the standard solutions. In these cases, the identity
of the peaks can be confirmed by standard addition.
b) Solutions having high concentrations of salts can also create a large signal at the void volume, poorly
resolved from the HEEDTA peak.
c) High concentrations of nitrate, carbonate, sulfate, and phosphate do not interfere. However, large
amounts of chloride create a negative fronting peak poorly resolved from the DTPA peak and altering
its peak shape.
5

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SIST-TS CEN/TS 17789-1:2023
CEN/TS 17789-1:2022 (E)
d) Compounds, related to the group of polyamino polycarboxylic acids can interfere. While signals for
[o,o] EDDHA, [o,o] EDDHMA, and EDDHSA are not detected, relatively weak signals are observed for
NTA and CDTA. Under some conditions NTA can coelute with HEEDTA or EDTA.
e) No signals have been detected for the following complexing agents: citrate, oxalate, tartrate,
phthalate, and 20 naturally occurring amino acids.
6 Reagents
All reagents shall be of recognized analytical grade.
6.1 Water
All water used should conform t
...

SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 17789-1:2021
01-december-2021
[Not translated]
Organo-mineral fertilizers - Identification of chelating agents - Part 1: Determination of
EDTA, HEEDTA and DTPA by ion chromatography
Organisch-mineralische Düngemittel - Identifizierung von Chelatbildnern - Teil 1:
Bestimmung von EDTA, HEEDTA und DTPA mittels Ionenchromatographie
Ta slovenski standard je istoveten z: FprCEN/TS 17789-1
ICS:
65.080 Gnojila Fertilizers
kSIST-TS FprCEN/TS 17789-1:2021 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
kSIST-TS FprCEN/TS 17789-1:2021

---------------------- Page: 2 ----------------------
kSIST-TS FprCEN/TS 17789-1:2021


FINAL DRAFT
TECHNICAL SPECIFICATION
FprCEN/TS 17789-1
SPÉCIFICATION TECHNIQUE

TECHNISCHE SPEZIFIKATION

October 2021
ICS 65.080
English Version

Organo-mineral fertilizers - Identification of chelating
agents - Part 1: Determination of EDTA, HEEDTA and
DTPA by ion chromatography
 Organisch-mineralische Düngemittel - Identifizierung
von Chelatbildnern - Teil 1: Bestimmung von EDTA,
HEEDTA und DTPA mittels Ionenchromatographie


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 17789-1:2021 E
worldwide for CEN national Members.

---------------------- Page: 3 ----------------------
kSIST-TS FprCEN/TS 17789-1:2021
FprCEN/TS 17789-1:2021 (E)
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 5
5 Interferences . 5
6 Reagents . 6
7 Apparatus . 7
8 Sampling and sample preparation . 8
9 Procedure . 8
9.1 Preparation of the test solution . 8
9.2 Preparation of the standard solutions . 8
9.3 Chromatographic analysis . 9
10 Expression of results . 9
11 Test report . 9
Annex A (informative) Complete names of chelating agents . 10
Annex B (informative) Chromatogram . 11
Bibliography . 12

2

---------------------- Page: 4 ----------------------
kSIST-TS FprCEN/TS 17789-1:2021
FprCEN/TS 17789-1:2021 (E)
European foreword
This document (FprCEN/TS 17789-1:2021) 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.
3

---------------------- Page: 5 ----------------------
kSIST-TS FprCEN/TS 17789-1:2021
FprCEN/TS 17789-1:2021 (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 organo-mineral 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.
1
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 or biological materials) chelates including [o,o] EDDHA, [o,p] EDDHA, [o,o] EDDHMA, HBED
and EDDHSA.
This document specifies the test method to be used in order to determine the content of certain chelating
agents (EDTA, DTPA and HEEDTA) in organo-mineral fertilizers (product function category (PFC) 1 (B)
according to Regulation (EU) 2019/1009 [4]).

1
Abbreviated terms are described in Annex A.
4

---------------------- Page: 6 ----------------------
kSIST-TS FprCEN/TS 17789-1:2021
FprCEN/TS 17789-1:2021 (E)
1 Scope
This document specifies a method for the determination by ion chromatography of the total amount of
each of the individual chelating agents EDTA, HEEDTA, and DTPA in organo-mineral fertilizers, having an
organic matrix based on vegetal residues (cocoa shells, grape residue, soybean residue, …), algae extract,
and animal meal (feather, bones, blood, .) and containing one or more of these substances.
The method allows the identification and the determination of the total water-soluble fraction of each of
these chelating agents. It does not allow to distinguish between the free form and the metal bound form
of the chelating agents.
This method applies to organo-mineral fertilizers containing chelates of one or more of the following
micronutrients: cobalt, copper, iron, manganese, zinc and with a mass fraction of at least 0,1 %.
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
3 Terms and definitions
For the purposes of this document, the terms and definitions given in EN 12944-1 and EN 12944-2 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/
4 Principle
The micronutrients associated with the chelating agents present in an aqueous extract of the sample are
replaced by iron(III). The iron chelates are separated and determined by ion chromatography. The
separation is based on anion exchange, by elution with a nitrate acetate solution. The detection is based
on UV photometry at 330 nm, after post-column reaction with diluted perchloric acid.
5 Interferences
Several substances can interfere, to a degree largely dependent on the type of column used. With the
column described in 7.2, the following phenomena have been observed.
a) Injection of solutions having high concentrations of salts can cause shifts in the retention times,
mostly decreasing the retention when compared to the standard solutions. In these cases, the identity
of the peaks can be confirmed by standard addition.
b) Solutions having high concentrations of salts can also create a large signal at the void volume, poorly
resolved from the HEEDTA peak.
5

---------------------- Page: 7 ----------------------
kSIST-TS FprCEN/TS 17789-1:2021
FprCEN/TS 17789-1:2021 (E)
c) High concentrations of nitrate, carbonate, sulfate, and phosphate do not interfere. However, large
amounts of chloride create a negative fronting peak poorly resolved from the DTPA peak and altering
its peak shape.
d) Compounds, related to the group of polyamino polycarboxylic acids can interfere. While signals for
[o,o] EDDHA, [o,o] EDDHMA, and EDDHSA are not detected, relatively weak signals are observed for
NTA and CDTA. Under some conditions NTA can coelute with HEEDTA or EDTA.
e) No signals have been detected for the following complexing agents: citrate, oxalate, tartrate,
phthalate, and 20 naturally occurring amino acids.
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 Nitric acid, substance concentration c(HNO ) = 7,2 mol/l.
3
Nitric acid, diluted 1 + 1 with water.
6.3 Sodium hydroxide solution, c(NaOH) = 0,5 mol/l.
Dissolve 20 g of NaOH in pellet form in a 1 000 ml volumetric flask with water. Dilute to the mark and
homogenize.
6.4 EDTA stock solution, c(EDTA) = 2 mmol/l.
Dissolve 372 mg of the disodium dihydrogen salt of ethylene diamine tetraacetic acid dihydrate in 400 ml
of water in a 500 ml volumetric flask. After dissolution, dilute to the mark with water and homogenize.
Store the solution in a plastic bottle.
6.5 HEE
...

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