Plant biostimulants - Determination of phosphonates

This document specifies a method for the extraction and determination of phosphonates (P–PO3) in plant biostimulants using ion chromatography and conductivity detection (IC-CD).
This document is also applicable to the blends of fertilizing products where plant biostimulants are the main part of the blend. Otherwise, the Technical Specification for the main part of the blend applies.

Pflanzen-Biostimulanzien - Bestimmung von Phosphonaten

Dieses Dokument legt ein Verfahren zur Extraktion und Bestimmung von Phosphonaten (P PO3) in Pflanzen-Biostimulanzien mit Ionenchromatographie und Leitfähigkeitsnachweis (IC CD) fest.
Dieses Dokument ist auch anzuwenden für die Mischungen von Düngeprodukten, in denen die Pflanzen-Biostimulanzien der Hauptbestandteil der Mischung sind. Andernfalls ist die Technische Spezifikation für den Hauptbestandteil der Mischung anzuwenden.

Biostimulants des végétaux - Dosage des phosphonates

Le présent document spécifie une méthode d’extraction et de dosage des phosphonates (P-PO3) dans les biostimulants des végétaux par chromatographie ionique et détection conductimétrique (IC-CD).
Le présent document est également applicable aux mélanges de fertilisants dans lesquels les biostimulants des végétaux représentent la majorité du mélange. Dans le cas contraire, c’est la Spécification Technique correspondant au fertilisant majoritairement présent dans le mélange qui s’applique.

Rastlinski biostimulanti - Določevanje fosfonatov

General Information

Status
Published
Publication Date
22-Mar-2022
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
23-Mar-2022
Due Date
30-Aug-2022
Completion Date
23-Mar-2022

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SLOVENSKI STANDARD
SIST-TS CEN/TS 17705:2023
01-februar-2023
Rastlinski biostimulanti - Določevanje fosfonatov
Plant biostimulants - Determination of phosphonates
Pflanzen-Biostimulanzien - Bestimmung von Phosphonaten
Biostimulants des végétaux - Dosage des phosphonates
Ta slovenski standard je istoveten z: CEN/TS 17705:2022
ICS:
65.080 Gnojila Fertilizers
SIST-TS CEN/TS 17705:2023 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST-TS CEN/TS 17705:2023
---------------------- Page: 2 ----------------------
SIST-TS CEN/TS 17705:2023
CEN/TS 17705
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
March 2022
TECHNISCHE SPEZIFIKATION
ICS 07.080
English Version
Plant biostimulants - Determination of phosphonates

Biostimulants des végétaux - Dosage des phosphonates Biostimulanzien für die pflanzliche Anwendung -

Bestimmung von Phosphonaten

This Technical Specification (CEN/TS) was approved by CEN on 3 January 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 17705:2022 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST-TS CEN/TS 17705:2023
CEN/TS 17705:2022 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

Introduction .................................................................................................................................................................... 4

1 Scope .................................................................................................................................................................... 5

2 Normative references .................................................................................................................................... 5

3 Terms and definitions ................................................................................................................................... 5

4 Principle ............................................................................................................................................................. 5

5 Reagents ............................................................................................................................................................. 5

6 Apparatus ........................................................................................................................................................... 6

7 Procedure........................................................................................................................................................... 6

7.1 Sample preparation ........................................................................................................................................ 6

7.2 Water extraction.............................................................................................................................................. 6

7.3 Preparation of the calibration solutions ................................................................................................ 7

7.4 Measurement .................................................................................................................................................... 7

8 Calculation and expression of the results .............................................................................................. 9

8.1 Integration of peaks ....................................................................................................................................... 9

8.2 Concentration of phosphonates in test solutions ................................................................................ 9

9 Test report ...................................................................................................................................................... 10

Annex A (informative) Separation of phosphonates from other interfering ions in a mixture

of standards .................................................................................................................................................... 11

Bibliography ................................................................................................................................................................. 12

---------------------- Page: 4 ----------------------
SIST-TS CEN/TS 17705:2023
CEN/TS 17705:2022 (E)
European foreword

This document (CEN/TS 17705:2022) has been prepared by the Technical Committee CEN/TC 455 “Plant

biostimulants”, the secretariat of which is held by AFNOR.

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.
---------------------- Page: 5 ----------------------
SIST-TS CEN/TS 17705:2023
CEN/TS 17705:2022 (E)
Introduction

This document was prepared by the experts of CEN/TC 455 “Plant Biostimulants”. The European

Committee for Standardization (CEN) was requested by the European Commission (EC) to draft

European standards or European standardization deliverables to support the implementation of

Regulation (EU) 2019/1009 of 5 June 2019 laying down rules on the making available on the market of

EU fertilizing products (“FPR” or “Fertilising Products Regulation”).

This standardization request, presented as M/564, also contributes to the Communication on “Innovating

for Sustainable Growth: A Bio economy for Europe”. The Working Group 4 “Other safety parameters”, was

created to develop a work program as part of this request. The technical committee CEN/TC 455 “Plant

Biostimulants” was established to carry out the work program that will prepare a series of standards. The

interest in biostimulants has increased significantly in Europe as a valuable tool to use in agriculture.

Standardization was identified as having an important role in order to promote the use of biostimulants.

The work of CEN/TC 455 seeks to improve the reliability of the supply chain, thereby improving the

confidence of farmers, industry, and consumers in biostimulants, and will promote and support

commercialisation of the European biostimulant industry.

The preparation of this document is based on the Fertilising Products Standardization Request (M/564)

to CEN by the European Commission and the European Free Trade Association concerning a development

of the methods for analysis of fertilizers in the framework of Regulation (EC) No 2019/1009.

This document describes the extraction and measurement for the determination of phosphonate

(phosphite) in plant biostimulants. It is based on a water extraction of the phosphonate (phosphite)

followed by ion chromatography with conductivity detection (IC-CD).

The ion chromatography with a conductivity detector (IC-CD) method can be used in well-equipped

analytical laboratories for the determination of different ions. In the field of fertilizing products, the

method is used and standardized for the determination of perchlorates in mineral fertilizers. The IC-CD

method can determine more ions simultaneously.

The legislative limit for phosphonate content is 0,5 % (mass fraction) and the method described in this

document was adapted to achieve this requirement and simultaneously to reduce interferences from

other co-extracted anions as much as possible.

The definition of phosphonates is not clearly stated in the Regulation 2019/1009 and to avoid any

misunderstanding the results are expressed as a content of phosphorus (P) bound in the form of free

water-soluble phosphonates (P-PO3).
---------------------- Page: 6 ----------------------
SIST-TS CEN/TS 17705:2023
CEN/TS 17705:2022 (E)
1 Scope

This document specifies a method for the extraction and determination of phosphonates (P–PO ) in plant

biostimulants using ion chromatography and conductivity detection (IC-CD).

This document is also applicable to the blends of fertilizing products where plant biostimulants are the

main part of the blend. Otherwise, the Technical Specification for the main part of the blend applies.

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.

CEN/TS 17704, Plant biostimulants — Determination of dry matter
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
phosphonates
salts derived from phosphonic acid (H PO )
3 3
4 Principle

A representative test portion of the sample is extracted with water. Phosphonate in the extract is

selectively separated from other compounds using ion chromatography (IC) and determined by a

conductivity detector (CD). External calibration is used for quantification of the amount of the

phosphonate.
5 Reagents

All reagents shall be of recognized analytical grade. The concentration of phosphonate in the reagents

and deionized water used shall be low enough not to affect the results of the determination.

5.1 Water with a specific conductivity not higher than 0,2 mS/m at 25 °C.

5.2 Phosphonate standard stock solution r(P-PO3) = 1 000 mg/l is prepared by dissolving

commercially available sodium phosphite dibasic pentahydrate salt (Mw = 216,04 mol/l, purity ≥ 98 %).

For preparation the phosphonate standard stock solution 0,697 ± 0,001 g is weighed, transferred to

100 ml volumetric flask, fill with deionized water (5.1) to final volume and mix thoroughly.

5.3 Phosphonate standard solution, r(P-PO3) = 100 mg/l is prepared from a standard stock solution

(5.2) by appropriate dilution with deionized water (5.1). Pipette 10 ml of stock solution (5.2) to a 100ml

volumetric flask, fill with deionized water (5.1) to final volume and mix thoroughly.

5.4 Mobile phase, KOH cartridge for ion chromatography (commercially supplied). Concentration of

the KOH mobile phase is e
...

SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 17705:2021
01-november-2021
Rastlinski biostimulansi - Določevanje fosfonatov
Plant biostimulants - Determination of phosphonates
Biostimulanzien für die pflanzliche Anwendung - Bestimmung von Phosphonaten
Biostimulants des végétaux - Dosage des phosphonates
Ta slovenski standard je istoveten z: FprCEN/TS 17705
ICS:
65.080 Gnojila Fertilizers
kSIST-TS FprCEN/TS 17705:2021 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
kSIST-TS FprCEN/TS 17705:2021
---------------------- Page: 2 ----------------------
kSIST-TS FprCEN/TS 17705:2021
FINAL DRAFT
TECHNICAL SPECIFICATION
FprCEN/TS 17705
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
September 2021
ICS 07.080
English Version
Plant biostimulants - Determination of phosphonates

Biostimulants des végétaux - Dosage des phosphonates Biostimulanzien für die pflanzliche Anwendung -

Bestimmung von Phosphonaten

This draft Technical Specification is submitted to CEN members for Vote. It has been drawn up by the Technical Committee

CEN/TC 455.

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 17705:2021 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
kSIST-TS FprCEN/TS 17705:2021
FprCEN/TS 17705:2021 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

Introduction .................................................................................................................................................................... 4

1 Scope .................................................................................................................................................................... 5

2 Normative references .................................................................................................................................... 5

3 Terms and definitions ................................................................................................................................... 5

4 Principle ............................................................................................................................................................. 5

5 Reagents ............................................................................................................................................................. 5

6 Apparatus ........................................................................................................................................................... 6

7 Procedure........................................................................................................................................................... 6

7.1 Sample preparation ........................................................................................................................................ 6

7.2 Water extraction.............................................................................................................................................. 6

7.3 Preparation of the calibration solutions ................................................................................................ 7

7.4 Measurement .................................................................................................................................................... 7

7.4.1 Instrument conditions ................................................................................................................................... 7

7.4.2 IC-CD measurement ........................................................................................................................................ 8

8 Calculation and expression of the results .............................................................................................. 9

8.1 Integration of peaks ....................................................................................................................................... 9

8.2 Concentration of phosphonates in test solutions ................................................................................ 9

9 Test report ...................................................................................................................................................... 10

Annex A (informative) Separation of phosphonates from other interfering ions in a mixture

of standards .................................................................................................................................................... 11

Bibliography ................................................................................................................................................................. 12

---------------------- Page: 4 ----------------------
kSIST-TS FprCEN/TS 17705:2021
FprCEN/TS 17705:2021 (E)
European foreword

This document (FprCEN/TS 17705:2021) has been prepared by the Technical Committee CEN/TC 455

“Plant biostimulants”, the secretariat of which is held by AFNOR.
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.
---------------------- Page: 5 ----------------------
kSIST-TS FprCEN/TS 17705:2021
FprCEN/TS 17705:2021 (E)
Introduction

This document was prepared by the experts of CEN/TC 455 ‘Plant Biostimulants’. The European

Committee for Standardization (CEN) was requested by the European Commission (EC) to draft

European standards or European standardization deliverables to support the implementation of

Regulation (EU) 2019/1009 of 5 June 2019 laying down rules on the making available on the market of

EU fertilising products (“FPR” or “Fertilising Products Regulation”).

This request, presented as SR M/564, also contributes to the Communication on “Innovating for

Sustainable Growth: A Bio economy for Europe”. The Working Group 4 “Other safety parameters”, was

created to develop a work program as part of this Request. The technical committee CEN/TC 455 ‘Plant

Biostimulants’ was established to carry out the work program that will prepare a series of standards. The

interest in biostimulants has increased significantly in Europe as a valuable tool to use in agriculture.

Standardization was identified as having an important role in order to promote the use of biostimulants.

The work of CEN/TC 455 seeks to improve the reliability of the supply chain, thereby improving the

confidence of farmers, industry, and consumers in biostimulants, and will promote and support

commercialisation of the European biostimulant industry.

The preparation of this document is based on the Fertilising Products Standardization Request (M/564)

to CEN by the European Commission and the European Free Trade Association concerning a development

of the methods for analysis of fertilizers in the framework of Regulation (EC) No 2019/1009.

This document describes the extraction and measurement for the determination of phosphonate

(phosphite) in plant biostimulants. It is based on a water extraction of the phosphonate (phosphite)

followed by ion chromatography with conductivity detection (IC-CD).

The ion chromatography with a conductivity detector (IC-CD) method can be used in well-equipped

analytical laboratories for the determination of different ions. In the field of fertilizing products, the

method is used and standardized for the determination of perchlorates in mineral fertilizers. The IC-CD

method can determine more ions simultaneously.

The legislative limit for phosphonate content is 0,5 % (mass fraction) and the method described in this

document was adapted to achieve this requirement and simultaneously to reduce interferences from

other co-extracted anions as much as possible.

The definition of phosphonates is not clearly stated in the Regulation 2019/1009 and to avoid any

misunderstanding the results are expressed as a content of phosphorus (P) bound in the form of free

water-soluble phosphonates (P-PO3).

This document is also applicable to the blends of fertilizing products where plant biostimulants are the

main part of the blend. Otherwise, the Technical Specification for the main part of the blend apply.

---------------------- Page: 6 ----------------------
kSIST-TS FprCEN/TS 17705:2021
FprCEN/TS 17705:2021 (E)
1 Scope

This document specifies a method for the extraction and determination of phosphonates (P–PO ) in plant

biostimulants using ion chromatography and conductivity detection (IC-CD).

This document is also applicable to the blends of fertilizing products where plant biostimulants are the

main part of the blend. Otherwise, the Technical Specification for the main part of the blend apply.

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.

FprCEN/TS 17704:2021, Plant biostimulants — Determination of dry matter
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

• IEC Electropedia: available at https://www.electropedia.org/
• ISO Online browsing platform: available at https://www.iso.org/obp
3.1
phosphonates
salts derived from phosphonic acid (H PO )
3 3
4 Principle

A representative test portion of the sample is extracted with water. Phosphonate in the extract is

selectively separated from other compounds using ion chromatography (IC) and determined by a

conductivity detector (CD). External calibration is used for quantification of the amount of the

phosphonate.
5 Reagents

All reagents shall be of recognized analytical grade. The concentration of phosphonate in the reagents

and deionized water used shall be low enough not to affect the results of the determination.

5.1 Water with a specific conductivity not higher than 0,2 mS/m at 25 °C.

5.2 Phosphonate standard stock solution r(P-PO3) = 1 000 mg/l is prepared by dissolving

commercially available sodium phosphite dibasic pentahydrate salt (Mw = 216,04 mol/l, purity ≥ 98 %).

For preparation the phosphonate standard stock solution 0,697 ± 0,001 g is weighed, transferred to

100 ml volumetric flask, fill with deionized water (5.1) to final volume and mix thoroughly.

5.3 Phosphonate standard solution, r(P-PO3) = 100 mg/l is prepared from a standard stock solution

(5.2) by appropriate dilution with deionized water (5.1). Pipette 10 ml of stock solution (5.2) to a 100ml

volumetric flask, fill with deionized water (5.1) to final volume and mix thoroughly.

5.4 Mobile phase, KOH cartridge for ion chromatography (commercially supplied). Concentration of

the KOH mobile phase is electrolytically generated in externally supplied deionized water (5.1).

---------------------- Page: 7 ----------------------
kSIST-TS FprC
...

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