Fertilizers - Determination of chelating agents - Determination of iron chelated by o,p-EDDHA by reversed phase HPLC

This European Standard specifies a method for the chromatographic determination of the amount of iron chelated by each of the individual isomers of the chelating agent ortho para EDDHA (o,p-EDDHA) in fertilizers. The method allows the identification of this chelating agent and the determination of the water soluble fraction of iron chelated by this chelating agent. The method is not applicable for the determination of the amount of free chelating agent.
NOTE 1   This method has been shown to be also suitable for the determination of the amount of iron chelated by each of the individual isomers of the chelating agent ortho ortho EDDHA (o,o-EDDHA) in fertilizers.
NOTE 2   o,o-EDDHA and o,p-EDDHA are abbreviations used in this European Standard for the sake of simplicity. For complete names see Annex C.
NOTE 3   The substances o,o-EDDHA and o,p-EDDHA both exist as different stereoisomers. For o,o-EDDHA a meso form and a d/l pair (the racemic isomers) exist, for o,p-EDDHA two different d/l pairs exist. All four stereoisomers are observed separately in this method.
NOTE 4   Currently, an analytically pure standard only exists for o,o-EDDHA. The method for o,p-EDDHA has been developed with an o,p-EDDHA standard containing an uncertain concentration of o,p-EDDHA.

Düngemittel - Bestimmung von Chelatbildnern - Bestimmung von Eisen-chelatisiertem o,p-EDDHA mit Umkehrphasen HPLC

Diese Europäische Norm legt ein Verfahren zur chromatographischen Bestimmung der Menge des von jedem einzelnen der isomeren Formen des Chelatbildners ortho,para-EDDHA (o,p-EDDHA) chelatisierten Eisens in Düngemitteln fest. Das Verfahren erlaubt die Identifikation dieses Chelatbildners und die Bestimmung der wasserlöslichen Fraktion des von diesem Chelatbildner chelatisierten Eisens. Das Verfahren gilt nicht für die Bestimmung der Menge des freien Chelatbildners.
ANMERKUNG 1   Es wurde gezeigt, dass dieses Verfahren auch zur Bestimmung der Menge des von jedem einzelnen der isomeren Formen des Chelatbildners ortho-ortho-EDDHA (o,o-EDDHA) chelatisierten Eisens in Düngemitteln geeignet ist.
ANMERKUNG 2   Der Einfachheit halber wurden die Abkürzungen o,o-EDDHA und o,p-EDDHA in dieser Europäischen Norm verwendet. Für die vollständigen Bezeichnungen siehe Anhang C.
ANMERKUNG 3   Die Substanzen o,o-EDDHA und o,p-EDDHA liegen beide als verschiedene stereoisomere Formen vor. Für o,o-EDDHA gibt es eine Mesoform und ein d/l-Paar (die Racemformen), für o,p-EDDHA gibt es zwei verschiedene d/l-Paare. Alle vier stereoisomeren Formen werden in diesem Verfahren getrennt voneinander betrachtet.
ANMERKUNG 4   Derzeit existiert nur eine Standardlösung mit analytischem Reinheitsgrad für o,o-EDDHA. Das Verfahren für o,p-EDDHA wurde mit einer o,p-EDDHA-Standardlösung mit unbestimmter o,p-EDDHA-Konzentration entwickelt.

Engrais - Dosage des agents chélatants - Dosage du fer chélaté par o,p-EDDHA par chromatographie liquide à haute performance á polarité de phase inversée

La présente Norme européenne prescrit une méthode de détermination par chromatographie de la quantité de fer chélaté par chacun des isomères de l’agent chélatant ortho para EDDHA (o,p-EDDHA) présent dans les engrais. Cette méthode permet d’identifier cet agent chélatant et de doser la fraction soluble dans l’eau du fer chélaté par cet agent chélatant. Elle ne permet pas de déterminer la quantité d’agent chélatant libre.
NOTE 1   Il s’est avéré que cette méthode permettait également de déterminer la quantité de fer chélaté par chacun des isomères de l’agent chélatant ortho ortho EDDHA (o,o-EDDHA) présent dans les engrais.
NOTE 2   o,o-EDDHA et o,p-EDDHA sont des abréviations utilisées dans la présente Norme européenne par souci de simplicité. Les dénominations complètes sont données dans l’Annexe C.
NOTE 3   Les substances o,o-EDDHA et o,p-EDDHA existent en tant que stéréo-isomères distincts. Pour o,o-EDDHA, il existe une forme méso et une paire d/l (les isomères racémiques), pour o,p-EDDHA il existe deux paires d/l différentes. La présente méthode permet d’observer les quatre stéréo-isomères séparément.
NOTE 4   Actuellement, il n'existe d’étalon de pureté analytique que pour o,o-EDDHA. La méthode concernant o,p EDDHA a été mise au point avec un étalon de o,p-EDDHA dont la concentration en o,p-EDDHA est incertaine.

Gnojila - Določevanje sredstev za kelatiziranje - Določevanje železovih kelatov z o,p-EDDHA s tekočinsko kromatografijo visoke ločljivosti (HPLC) z obrnjeno fazo

General Information

Status
Published
Publication Date
10-Jun-2009
ICS
65.080 - Fertilizers
Technical Committee
KAT - Soil quality
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
03-Jun-2009
Due Date
08-Aug-2009
Completion Date
11-Jun-2009
Mandate
M/335 - Standardization Mandate assigned to the CEN concerning the modernisation of the methods of anylysis of Fertilizers
Ref Project
EN 15452:2008 - Fertilizers - Determination of chelating agents - Determination of iron chelated by o,p-EDDHA by reversed phase HPLC

Relations

Replaces
SIST-TS CEN/TS 15452:2008 - Fertilizers - Determination of chelating agents - Determination of iron chelated by o,p-EDDHA by reversed phase HPLC
Effective Date
01-Jul-2009

Overview

EN 15452:2008 is a CEN European Standard that specifies a validated chromatographic method for the determination of iron chelated by o,p-EDDHA in fertilizers using reversed‑phase HPLC. The method identifies the chelating agent (o,p‑EDDHA), quantifies the water‑soluble fraction of Fe‑EDDHA, and resolves the individual stereoisomer peaks. It is not intended for measuring free (uncomplexed) chelating agent.

Key topics and technical requirements

  • Analytical technique: reversed‑phase high performance liquid chromatography (RP‑HPLC) with UV detection at 277 nm.
  • Column & conditions: C18 (ODS‑2) column, typically 250 × 4.6 mm, 5 µm; isocratic eluent composed of sodium formate (pH 3.0) and acetonitrile; typical flow 1.0 mL/min; 20 µL injection loop.
  • Calibration & quantification: external standard method using an Fe‑complexed o,p‑EDDHA standard; separate calibration lines are prepared for each stereoisomer peak (d/l‑1 and d/l‑2).
  • Scope & limitations: determines Fe chelated by o,p‑EDDHA (and-per NOTE-also applicable to o,o‑EDDHA Fe chelates); does not determine free chelating agent. Resolves multiple stereoisomers (four peaks observed for combined materials).
  • Sample preparation: water extraction of fertilizers and filtration (0.45 µm) prior to injection; sampling/sample preparation should follow EN 1482‑2.
  • Quality & precision: method validated via an inter‑laboratory study; repeatability and reproducibility figures are reported in the standard (see Annex B).
  • Reagents & standards: analytical‑grade reagents, Fe(III) nitrate standard, sodium formate eluent; water compliant with EN ISO 3696.

Applications and users

  • Fertilizer manufacturers: quality control of micronutrient formulations containing Fe‑EDDHA to verify declared chelated iron content.
  • Analytical laboratories: routine testing for regulatory compliance, product specification, and batch release.
  • Regulatory bodies and certification labs: verification of micronutrient content against labeling and legal requirements (Regulation (EC) No 2003/2003 referenced).
  • R&D groups: method for comparing formulation performance, stability studies, and isomer profiling.

Practical benefits include reliable separation of stereoisomers, robust quantification of water‑soluble Fe‑EDDHA, and documented precision from inter‑laboratory testing.

Related standards

  • EN 1482‑2 - Sampling and sample preparation for fertilizers
  • EN ISO 3696 - Water for analytical laboratory use
  • ISO 5725‑2 - Methodology for repeatability and reproducibility assessment
  • Regulation (EC) No 2003/2003 - Fertiliser regulation referenced for context

Keywords: EN 15452:2008, o,p‑EDDHA, Fe‑EDDHA, reversed‑phase HPLC, fertilizers, chelating agents, iron chelate determination, RP‑HPLC method.

Frequently Asked Questions

SIST EN 15452:2009 is a standard published by the Slovenian Institute for Standardization (SIST). Its full title is "Fertilizers - Determination of chelating agents - Determination of iron chelated by o,p-EDDHA by reversed phase HPLC". This standard covers: This European Standard specifies a method for the chromatographic determination of the amount of iron chelated by each of the individual isomers of the chelating agent ortho para EDDHA (o,p-EDDHA) in fertilizers. The method allows the identification of this chelating agent and the determination of the water soluble fraction of iron chelated by this chelating agent. The method is not applicable for the determination of the amount of free chelating agent. NOTE 1 This method has been shown to be also suitable for the determination of the amount of iron chelated by each of the individual isomers of the chelating agent ortho ortho EDDHA (o,o-EDDHA) in fertilizers. NOTE 2 o,o-EDDHA and o,p-EDDHA are abbreviations used in this European Standard for the sake of simplicity. For complete names see Annex C. NOTE 3 The substances o,o-EDDHA and o,p-EDDHA both exist as different stereoisomers. For o,o-EDDHA a meso form and a d/l pair (the racemic isomers) exist, for o,p-EDDHA two different d/l pairs exist. All four stereoisomers are observed separately in this method. NOTE 4 Currently, an analytically pure standard only exists for o,o-EDDHA. The method for o,p-EDDHA has been developed with an o,p-EDDHA standard containing an uncertain concentration of o,p-EDDHA.

This European Standard specifies a method for the chromatographic determination of the amount of iron chelated by each of the individual isomers of the chelating agent ortho para EDDHA (o,p-EDDHA) in fertilizers. The method allows the identification of this chelating agent and the determination of the water soluble fraction of iron chelated by this chelating agent. The method is not applicable for the determination of the amount of free chelating agent. NOTE 1 This method has been shown to be also suitable for the determination of the amount of iron chelated by each of the individual isomers of the chelating agent ortho ortho EDDHA (o,o-EDDHA) in fertilizers. NOTE 2 o,o-EDDHA and o,p-EDDHA are abbreviations used in this European Standard for the sake of simplicity. For complete names see Annex C. NOTE 3 The substances o,o-EDDHA and o,p-EDDHA both exist as different stereoisomers. For o,o-EDDHA a meso form and a d/l pair (the racemic isomers) exist, for o,p-EDDHA two different d/l pairs exist. All four stereoisomers are observed separately in this method. NOTE 4 Currently, an analytically pure standard only exists for o,o-EDDHA. The method for o,p-EDDHA has been developed with an o,p-EDDHA standard containing an uncertain concentration of o,p-EDDHA.

SIST EN 15452:2009 is classified under the following ICS (International Classification for Standards) categories: 65.080 - Fertilizers. The ICS classification helps identify the subject area and facilitates finding related standards.

SIST EN 15452:2009 has the following relationships with other standards: It is inter standard links to SIST-TS CEN/TS 15452:2008. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.

SIST EN 15452:2009 is associated with the following European legislation: Standardization Mandates: M/335. When a standard is cited in the Official Journal of the European Union, products manufactured in conformity with it benefit from a presumption of conformity with the essential requirements of the corresponding EU directive or regulation.

SIST EN 15452:2009 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.

Standards Content (Sample)


2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Düngemittel - Bestimmung von Chelatbildnern - Bestimmung von Eisen-chelatisiertem o,p-EDDHA mit Umkehrphasen HPLCEngrais - Dosage des agents chélatants - Dosage du fer chélaté par o,p-EDDHA par chromatographie liquide à haute performance á polarité de phase inverséeFertilizers - Determination of chelating agents - Determination of iron chelated by o,p-EDDHA by reversed phase HPLC65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 15452:2008SIST EN 15452:2009en,fr,de01-julij-2009SIST EN 15452:2009SLOVENSKI
STANDARDSIST-TS CEN/TS 15452:20081DGRPHãþD

EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 15452July 2008ICS 65.080Supersedes CEN/TS 15452:2006
English VersionFertilizers - Determination of chelating agents - Determination ofiron chelated by o,p-EDDHA by reversed phase HPLCEngrais - Dosage des agents chélatants - Dosage du ferchélaté par o,p-EDDHA par chromatographie liquide àhaute performance à polarité de phase inverséeDüngemittel - Bestimmung von Chelatbildnern -Bestimmung von Eisen-chelatisiertem o,p-EDDHA mitUmkehrphasen HPLCThis European Standard was approved by CEN on 30 May 2008.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2008 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15452:2008: ESIST EN 15452:2009

Typical chromatogram.10 Annex B (informative)
Statistical results of the inter-laboratory test.11 Annex C (informative)
Complete names of chelating agents.12 Bibliography.13
1 Scope This European Standard specifies a method for the chromatographic determination of the amount of iron chelated by each of the individual isomers of the chelating agent ortho-para EDDHA (o,p-EDDHA) in fertilizers. The method allows the identification of this chelating agent and the determination of the water soluble fraction of iron chelated by this chelating agent. The method is not applicable for the determination of the amount of free chelating agent. NOTE 1 This method has been shown to be also suitable for the determination of the amount of iron chelated by each of the individual isomers of the chelating agent ortho-ortho EDDHA (o,o-EDDHA) in fertilizers. NOTE 2 o,o-EDDHA and o,p-EDDHA are abbreviations used in this European Standard for the sake of simplicity. For complete names see Annex C. NOTE 3 The substances o,o-EDDHA and o,p-EDDHA both exist as different stereoisomers. For o,o-EDDHA a meso form and a d/l pair (the racemic isomers) exist, for o,p-EDDHA two different d/l pairs exist. All four stereoisomers are observed separately in this method. NOTE 4 Currently, an analytically pure standard only exists for o,o-EDDHA. The method for o,p-EDDHA has been developed with an o,p-EDDHA standard containing an uncertain concentration of o,p-EDDHA. 2 Normative references The following referenced documents are indispensable for the application 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 1482-2, Fertilizers and liming materials — Sampling and sample preparation — Part 2: Sample preparation 3 Principle The technique used is reversed phase HPLC with UV detection at 277 nm. The sample is separated on a silica-based reversed phase column using sodium formate, c = 0,015 mol/l, pH = 3,0, and acetonitrile as mobile phase. For both o,p-EDDHA and o,o-EDDHA, two stereoisomer peaks are observed. The concentration of iron chelated by o,p-EDDHA (o,p-Fe) is determined according to the external standard method. 4 Interferences No interferences have been detected. Iron chelates with EDTA, HEDTA, DTPA and EDDHMA do not interfere. 5 Reagents 5.1 General a) All reagents shall be of recognized analytical grade. SIST EN 15452:2009
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