Plant biostimulants - Determination of inorganic arsenic

This document specifies a method for extraction, separation, and determination of inorganic arsenic (iAs) in plant biostimulants using anion-exchange high performance liquid chromatography (HPLC) or ion chromatography (IC) coupled to ICP-MS. This document is applicable to the fertilizing product blends belonging to PFC 7 where the EU fertilising product plant biostimulant contained in the blend represents the highest % by mass in the blend. In case of equal shares, the user can apply either this or the standard(s) applicable to the other component product(s).

Pflanzen-Biostimulanzien - Bestimmung von anorganischem Arsen

Dieses Dokument legt ein Verfahren zur Extraktion, Trennung und Bestimmung von anorganischem Arsen in Pflanzen-Biostimulanzien mit Anionenaustausch-Hochleistungs-Flüssigchromatograph (HPLC) oder Ionen¬chromatographie (IC) gekoppelt mit ICP MS fest. Dieses Dokument ist für Düngeproduktmischungen anwendbar, die zur PFC 7 gehören und bei denen das in der Mischung enthaltene EU Düngeprodukt Pflanzen-Biostimulans den größten Massenanteil in % in der Mischung ausmacht. Im Fall von gleich großen Anteilen kann der Anwender entweder die vorliegende Norm oder die für den/die anderen Bestandteil(e) anwendbare(n) Norm(en) verwenden.

Biostimulants des végétaux - Dosage de l'arsenic inorganique

Le présent document spécifie une méthode d’extraction, de séparation et de dosage de l’arsenic inorganique (iAs) dans les biostimulants des végétaux par chromatographie en phase liquide haute performance (HPLC) avec échange d’anions ou par chromatographie ionique (IC) couplée à une ICP-MS. Le présent document est applicable aux mélanges de fertilisants appartenant à la catégorie PFC 7, dans lesquels le fertilisant UE biostimulant des végétaux contenu dans le mélange représente le % le plus élevé en masse dans le mélange. Dans le cas où les proportions sont égales, l’utilisateur peut appliquer la présente norme ou la ou les normes applicables aux autres produits constituants.

Rastlinski biostimulanti - Določanje anorganskega arzena

General Information

Status
Published
Public Enquiry End Date
02-Jun-2023
Publication Date
06-Jan-2025
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
20-Dec-2024
Due Date
24-Feb-2025
Completion Date
07-Jan-2025

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SLOVENSKI STANDARD
01-februar-2025
Nadomešča:
SIST-TS CEN/TS 17706:2023
Rastlinski biostimulanti - Določanje anorganskega arzena
Plant biostimulants - Determination of inorganic arsenic
Pflanzen-Biostimulanzien - Bestimmung von anorganischem Arsen
Biostimulants des végétaux - Dosage de l'arsenic inorganique
Ta slovenski standard je istoveten z: EN 17706:2024
ICS:
65.080 Gnojila Fertilizers
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN 17706
EUROPEAN STANDARD
NORME EUROPÉENNE
November 2024
EUROPÄISCHE NORM
ICS 65.080 Supersedes CEN/TS 17706:2022
English Version
Plant biostimulants - Determination of inorganic arsenic
Biostimulants des végétaux - Dosage de l'arsenic Pflanzen-Biostimulanzien - Bestimmung von
inorganique anorganischem Arsen
This European Standard was approved by CEN on 26 August 2024.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC 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
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.

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, Türkiye 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
© 2024 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17706:2024 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 Reagents . 6
6 Apparatus . 8
7 Sampling . 9
8 Procedure . 9
8.1 Sample preparation . 9
8.2 Water bath extraction . 9
8.3 Preparation of the calibration solutions . 9
8.4 Measurement . 9
8.4.1 General instrumental conditions . 9
8.4.2 HPLC-ICP/MS measurement of inorganic arsenic . 10
9 Calculation and expression of the results . 12
9.1 Integration of peaks . 12
9.2 Calculation of inorganic arsenic in the samples . 12
10 Test report . 13
Annex A (informative) Examples of typical chromatographic separation . 14
Annex B (informative) Results of the inter-laboratory study . 18
B.1 Inter-laboratory tests . 18
B.2 Statistical results for determination of inorganic arsenic . 18
Annex ZA (informative) Relationship of this European Standard and the essential
requirements of Regulation (EU) 2019/1009 making available on the market of EU
fertilising products aimed to be covered . 20
Bibliography . 21

European foreword
This document (EN 17706:2024) has been prepared by Technical Committee CEN/TC 455 “Plant
Biostimulants”, the secretariat of which is held by AFNOR.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by May 2025, and conflicting national standards shall be
withdrawn at the latest by May 2025.
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 supersedes CEN TS 17706:2022.
In comparison with the previous edition no technical changes were applied in this document. The
following main editorial changes have been made:
— Introduction;
— Scope – text regarding blends changed;
— Annex B – results of the interlaboratory study added;
— Annex ZA added;
— Bibliography reordered.
This document has been prepared under a Standardization Request addressed to CEN by the European
Commission. The Standing Committee of the EFTA States subsequently approves these requests for its
Member States.
For relationship with EU Legislation, see informative Annex ZA, which is an integral part of this document.
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 implement this European Standard: 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, Türkiye and the United
Kingdom.
Introduction
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 [1] laying down rules on the making available on the market
of EU fertilising products (“FPR” or “Fertilising Products Regulation”).
This standardization request, presented as SR M/564 and relevant amendments, also contributes to the
Communication on “Innovating for Sustainable Growth: A Bio economy for Europe”. The interest in plant
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 standard is based on a mild acid oxidative extraction of the arsenic species followed by liquid
chromatography (HPLC or IC) coupled to the element-specific detector ICP-MS for the determination of
the mass fraction of inorganic arsenic.
The other standards developed for determination of inorganic arsenic content in animal feedingstuffs
and foodstuffs were studied as a basis of the described method [2], [3], [4], [5].
The inter-laboratory study reflects the final statistical characteristics of the method for the determination
of inorganic arsenic content in plant biostimulants. The results are given in Annex B (informative).
WARNING — Persons using this document should be familiar with usual 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.
1 Scope
This document specifies a method for extraction, separation, and determination of inorganic arsenic (iAs)
in plant biostimulants using anion-exchange high performance liquid chromatography (HPLC) or ion
chromatography (IC) coupled to ICP-MS.
This document is applicable to the blends of fertilizing products where a blend is a mix of at least two of
the following component EU fertilising products categories: Fertilizers, Liming Materials, Soil Improvers,
Growing Media, Inhibitors, Plant Biostimulants, and where the following category Plant Biostimulants is
the highest percentage in the blend by mass or volume, or in the case of liquid form by dry mass. If Plant
Biostimulants is not the highest percentage in the blend, the European Standard for the highest
percentage of the blend applies. In case a blend of fertilizing products is composed of components in equal
quantity or in case the component EU fertilising products used for the blend have identical formulations ,
the user decides which standard to 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.
EN 17702-1:2024, Plant biostimulants — Sampling and sample preparation — Part 1: Sampling
EN 17702-2:2024, Plant biostimulants — Sampling and sample preparation — Part 2: Sample preparation
EN 17704:2024, 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 terminology 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
analyte
parameter to be determined
3.2
blank calibration solution
solution prepared in the same way as the calibration solution but leaving out the analytes
3.3
blank test solution
solution prepared in the same way as the test sample solution but omitting the test portion

An example of such a blend is a product with two claimed functions consisting of a non-microbial plant
biostimulant and an organic fertilizer composed of 1kg/kg of plant biostimulant from seaweed.
3.4
calibration solution
solution used to calibrate the instrument, prepared from stock solutions by adding acids, buffer, reference
element and salts as needed
3.5
stock solution
solution with accurately known analyte concentration(s), prepared from pure chemicals
4 Principle
This document specifies a method for the determination of inorganic arsenic in plant biostimulants.
Inorganic arsenic consists of arsenite As (III) and arsenate As(V). A representative test portion of the
sample is treated with a diluted nitric acid and hydrogen peroxide solution in a heated water bath. By this
means the sample is solubilised, arsenic species are extracted into solution and As (III) is oxidized to
As(V). The inorganic arsenic is selectively separated from other arsenic compounds using anion exchange
HPLC (High Performance Liquid Chromatography) coupled online to the element-specific detector ICP-
MS (Inductively Coupled Plasma Mass Spectrometer) for the determination of the mass fraction of the
inorganic arsenic. External calibration with solvent matrix-matched standards is used for the
quantification of the amount of the inorganic arsenic. Alternatively, IC (ion chromatography) coupled to
ICP-MS can be used.
A preliminary determination of the total arsenic in aqua regia ex
...

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