SIST-TS CEN/TS 17784-2:2023
(Main)Organo-mineral fertilizers - Identification of complexing agents - Part 2: Method using high-performance liquid chromatography (HPLC)
Organo-mineral fertilizers - Identification of complexing agents - Part 2: Method using high-performance liquid chromatography (HPLC)
This document specifies a chromatographic method which allows the identification of heptagluconic acid (HGA) in organo-mineral fertilizers containing heptagluconic acid metal complexes.
NOTE For the complete names of the chelating agents mentioned in this document, see Annex D.
Organisch-mineralische Düngemittel - Identifizierung von Komplexbildnern - Teil 2: Verfahren mittels Hochleistungs-Flüssigkeitschromatographie (HPLC)
Dieses Dokument legt ein chromatographisches Verfahren fest, das die Identifizierung von Heptaglukon-säure (HGA, en: heptagluconic acid) in organisch-mineralischen Düngemitteln mit Heptaglukonsäure-Metall-Komplexen ermöglicht.
ANMERKUNG Die vollständigen Bezeichnungen der in diesem Dokument genannten Chelatbildner sind in Anhang D aufgeführt.
Engrais organo-minéraux - Identification des agents complexants - Partie 2 : Méthode par chromatographie liquide à haute performance (HPLC)
Le présent document spécifie une méthode chromatographique qui permet l’identification de l’acide heptagluconique (HGA) dans les engrais organo-minéraux contenant des complexes métalliques de l’acide heptagluconique.
NOTE Pour les appellations complètes des agents chélatants mentionnés dans le présent document, voir l’Annexe D.
Organsko-mineralna gnojila - Identifikacija sredstev za kompleksiranje - 2. del: Metoda s tekočinsko kromatografijo visoke ločljivosti (HPLC)
Ta dokument določa kromatografsko metodo, ki omogoča prepoznavanje heptaglukonske kisline (HGA) v organsko-mineralnih gnojilih, ki vsebujejo kovinske komplekse heptaglukonske kisline.
OPOMBA: Za vsa imena sredstev za kelatiranje, omenjenih v tem dokumentu, glej dodatek D.
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
SIST-TS CEN/TS 17784-2:2023
01-februar-2023
Organsko-mineralna gnojila - Identifikacija sredstev za kompleksiranje - 2. del:
Metoda s tekočinsko kromatografijo visoke ločljivosti (HPLC)
Organo-mineral fertilizers - Identification of complexing agents - Part 2: Method using
high-performance liquid chromatography (HPLC)
Organisch-mineralische Düngemittel - Identifizierung von Komplexbildnern - Teil 2:
Verfahren mittels Hochleistungs-Flüssigkeitschromatographie (HPLC)
Engrais organo-minéraux - Identification des agents complexants - Partie 2 : Méthode
par chromatographie liquide à haute performance (HPLC)
Ta slovenski standard je istoveten z: CEN/TS 17784-2:2022
ICS:
65.080 Gnojila Fertilizers
SIST-TS CEN/TS 17784-2:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST-TS CEN/TS 17784-2:2023
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SIST-TS CEN/TS 17784-2:2023
CEN/TS 17784-2
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
April 2022
TECHNISCHE SPEZIFIKATION
ICS 65.080
English Version
Organo-mineral fertilizers - Identification of complexing
agents - Part 2: Method using high-performance liquid
chromatography (HPLC)
Engrais organo-minéraux - Identification des agents Organisch-mineralische Düngemittel - Identifizierung
complexants - Partie 2 : Méthode par chromatographie von Komplexbildnern - Teil 2: Verfahren mittels
liquide à haute performance (HPLC) Hochleistungs-Flüssigkeitschromatographie (HPLC)
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 17784-2:2022 E
worldwide for CEN national Members.
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SIST-TS CEN/TS 17784-2:2023
CEN/TS 17784-2:2022 (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 . 7
9 Procedure . 7
10 Calculation of the heptagluconic acid content and expression of the results . 9
11 Test report . 9
Annex A (informative) Chromatograms of the standard and a typical sample solution . 10
Annex B (informative) Absorption spectra of the HGA . 12
Annex C (informative) Calculation of the molar ratio HGA:Metal . 13
Annex D (informative) Complete names of chelating agents . 14
Bibliography . 15
2
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SIST-TS CEN/TS 17784-2:2023
CEN/TS 17784-2:2022 (E)
European foreword
This document (CEN/TS 17784-2:2022) 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.
3
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SIST-TS CEN/TS 17784-2:2023
CEN/TS 17784-2:2022 (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 can be either a chelating agent or a complexing agent.
The incorporation of heptagluconic acid as complexing agent in organo-mineral fertilizers is intended to
enhance the long term availability to plants of micronutrients in such EU fertilizing products.
4
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SIST-TS CEN/TS 17784-2:2023
CEN/TS 17784-2:2022 (E)
1 Scope
This document specifies a chromatographic method which allows the identification of heptagluconic
acid (HGA) in organo-mineral fertilizers containing heptagluconic acid metal complexes.
NOTE For the complete names of the chelating agents mentioned in this document, see Annex D.
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 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
complexing agent
organic substance forming a flat or steric structure with one di- or tri-valent transition metal cation
(zinc (Zn), copper (Cu), iron (Fe), manganese (Mn) or cobalt (Co))
4 Principle
The method is based on demetallation with phosphoric acid of the micronutrient HGA complex present
in an aqueous solution of the sample.
The complexing agent is then identified and determined by high-performance liquid chromatography.
The separation is carried out on an NH phase bonded to silica column and an aqueous solution of
2
phosphoric acid and acetonitrile as eluent.
The detection is based on UV photometry at 210 nm.
WARNING — Users of this document should be familiar with normal laboratory practice. This
document does not purport to address all of the safety issues, if any, associated with its use. It is the
responsibility of the user to establish appropriate health and safety practices and to ensure compliance
with any national regulatory conditions.
IMPORTANT — It is absolutely essential that tests conducted according to this document are carried
out by suitably trained staff.
5 Interferences
Current knowledge on eventual interferences from other substances is summarized in the list below:
5
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SIST-TS CEN/TS 17784-2:2023
CEN/TS 17784-2:2022 (E)
a) High concentrations of phosphate in the sample solution can create a large peak preventing the
identification/determination of HGA.
b) High concentrations of chloride, sulfate and nitrate do not interfere in the
identification/determination of the complexing agent.
c) The presence of the chelates of EDDHSA, [o,o] EDDHA, [o,o] EDDHMA, EDTA, DTPA, CDTA, HEEDTA,
IDHA as well as the corresponding chelating agent do not interfere since they are separated from
HGA.
These substances can be detected in the chromatogram by the appearance of a peak at larger
retention times. Therefore, the presence of these kinds of substances shall be taken into account
when successive injections are scheduled.
d) The presence of gluconic acid does interfere in the determination of the complexing agent.
e) The presence of aspartic acid, humic substances and lignosulfonic acid can interfere with the
identification/determination of HGA.
6 Reagents
All reagents sha
...
SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 17784-2:2021
01-december-2021
Organsko-mineralna gnojila - Identifikacija kompleksirajočih agensov - 2. del:
Metoda s tekočinsko kromatografijo visoke ločljivosti (HPLC)
Organo-mineral fertilizers - Identification of complexing agents - Part 2: Method using
high-performance liquid chromatography (HPLC)
Organisch-mineralische Düngemittel - Identifizierung von Komplexbildnern - Teil 2:
Verfahren mittels Hochleistungs-Flüssigkeitschromatographie (HPLC)
Ta slovenski standard je istoveten z: FprCEN/TS 17784-2
ICS:
65.080 Gnojila Fertilizers
kSIST-TS FprCEN/TS 17784-2:2021 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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kSIST-TS FprCEN/TS 17784-2:2021
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kSIST-TS FprCEN/TS 17784-2:2021
FINAL DRAFT
TECHNICAL SPECIFICATION
FprCEN/TS 17784-2
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
October 2021
ICS 65.080
English Version
Organo-mineral fertilizers - Identification of complexing
agents - Part 2: Method using high-performance liquid
chromatography (HPLC)
Organisch-mineralische Düngemittel - Identifizierung
von Komplexbildnern - Teil 2: Verfahren mittels
Hochleistungs-Flüssigkeitschromatographie (HPLC)
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 17784-2:2021 E
worldwide for CEN national Members.
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kSIST-TS FprCEN/TS 17784-2:2021
FprCEN/TS 17784-2:2021 (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 . 6
8 Sampling and sample preparation . 7
9 Procedure . 7
10 Calculation of the heptagluconic acid content and expression of the results . 9
11 Test report . 9
Annex A (informative) Chromatograms of the standard and a typical sample solution . 10
Annex B (informative) Absorption spectra of the HGA . 12
Annex C (informative) Calculation of the molar ratio HGA:Metal . 13
Annex D (informative) Complete names of chelating agents . 14
Bibliography . 15
2
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kSIST-TS FprCEN/TS 17784-2:2021
FprCEN/TS 17784-2:2021 (E)
European foreword
This document (FprCEN/TS 17784-2:2021) 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
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kSIST-TS FprCEN/TS 17784-2:2021
FprCEN/TS 17784-2:2021 (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 can be either a chelating agent or a complexing agent.
The incorporation of heptagluconic acid as complexing agent in organo-mineral fertilizers is intended to
enhance the long term availability to plants of micronutrients in such EU fertilizing products.
WARNING — Users of this document should be familiar with normal laboratory practice. This
document does not purport to address all of the safety issues, if any, associated with its use. It is the
responsibility of the user to establish appropriate health and safety practices and to ensure compliance
with any national regulatory conditions.
IMPORTANT — It is absolutely essential that tests conducted according to this document are carried
out by suitably trained staff.
4
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kSIST-TS FprCEN/TS 17784-2:2021
FprCEN/TS 17784-2:2021 (E)
1 Scope
This document specifies a chromatographic method which allows the identification of heptagluconic
acid (HGA) in organo-mineral fertilizers containing heptagluconic acid metal complexes.
NOTE For the complete names of the chelating agents mentioned in this document, see Annex D.
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 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
complexing agent
organic substance forming a flat or steric structure with one di- or tri-valent transition metal cation
(zinc (Zn), copper (Cu), iron (Fe), manganese (Mn) or cobalt (Co))
4 Principle
The method is based on demetallation with phosphoric acid of the micronutrient HGA complex present
in an aqueous solution of the sample.
The complexing agent is then identified and determined by high-performance liquid chromatography.
The separation is carried out on an NH phase bonded to silica column and an aqueous solution of
2
phosphoric acid and acetonitrile as eluent.
The detection is based on UV photometry at 210 nm.
5 Interferences
Current knowledge on eventual interferences from other substances is summarized in the list below:
a) High concentrations of phosphate in the sample solution can create a large peak preventing the
identification/determination of HGA.
b) High concentrations of chloride, sulfate and nitrate do not interfere in the
identification/determination of the complexing agent.
5
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kSIST-TS FprCEN/TS 17784-2:2021
FprCEN/TS 17784-2:2021 (E)
c) The presence of the chelates of EDDHSA, [o,o] EDDHA, [o,o] EDDHMA, EDTA, DTPA, CDTA, HEEDTA,
IDHA as well as the corresponding chelating agent do not interfere since they are separated from
HGA.
These substances can be detected in the chromatogram by the appearance of a peak at larger
retention times. Therefore, the presence of these kinds of substances shall be taken into account
when successive injections are scheduled.
d) The presence of gluconic acid does interfere in the determination of the complexing agent.
e) The presence of aspartic acid, humic substances and lignosulfonic acid can interfere with the
identification/determination of HGA.
6 Reagents
All reagents shall be of recognized analytical grade.
6.1 Water
All water used should conform to EN ISO 3696, be degassed and be free of organic contaminants.
6.2 Sample preparation solvent.
Add to 800 ml of water, 2 ml of ortho-phosphoric acid 85 % and 25 ml of methanol in a 1 l volumetric
flask. Dilute to the mark with water and homogenize.
6.3 HGA stock solution.
The mass concentration (ρ) of this solution is ρ(HGA) = 19 893 mg/l.
This solution shall be freshly prepa
...
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