EN 17706:2024
(Main)Plant biostimulants - Determination of inorganic arsenic
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 die Mischungen von Düngeprodukten anwendbar, in denen eine Mischung aus mindestens zwei der folgenden Kategorien von Komponenten-EU Düngeprodukten besteht: Düngemittel, Kalkdünger, Bodenverbesserungsmittel, Kultursubstrate, Hemmstoffe, Pflanzen-Biostimulanzien und wenn die folgende Kategorie Pflanzen-Biostimulanzien prozentual den höchsten Massen- oder Volumenanteil in der Mischung bzw., bei flüssiger Form, den höchsten Trockenmasseanteil aufweist. Wenn Pflanzen-Biostimulanzien nicht den höchsten prozentualen Anteil in der Mischung ausmachen, ist die für den höchsten prozentualen Anteil geltende Europäische Norm anwendbar. Falls eine Düngemittelmischung aus Komponenten gleicher Menge besteht oder falls die für die Mischung verwendeten Komponenten-EU Düngeprodukte identische Formulierungen haben, entscheidet der Anwender, welche Norm angewendet wird.
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 également applicable aux mélanges de fertilisants constitués d’au moins deux composants appartenant aux catégories de fertilisants UE suivantes : engrais, amendements minéraux basiques, amendements du sol, supports de culture, inhibiteurs, biostimulants des végétaux et, dans lesquels la catégorie Biostimulants des végétaux représente le pourcentage le plus élevé du mélange en masse ou en volume, ou dans le cas d’un liquide, en masse sèche. Si les biostimulants des végétaux ne représentent pas le pourcentage le plus élevé du mélange, la Norme européenne relative au composant représentant le pourcentage le plus élevé du mélange s’applique. Dans le cas où un mélange de fertilisants contient des composants en quantité égale ou dans le cas où les composants des fertilisants UE utilisés pour le mélange ont des formulations identiques, l’utilisateur décide quelle norme appliquer.
Rastlinski biostimulanti - Določanje anorganskega arzena
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
oSIST prEN 17706:2023
01-maj-2023
Rastlinski biostimulanti - Določevanje 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: prEN 17706
ICS:
65.080 Gnojila Fertilizers
oSIST prEN 17706:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
oSIST prEN 17706:2023
oSIST prEN 17706:2023
DRAFT
EUROPEAN STANDARD
prEN 17706
NORME EUROPÉENNE
EUROPÄISCHE NORM
May 2023
ICS 65.080 Will supersede 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 draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 455.
If this draft becomes a European Standard, 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.
This draft European Standard was established by CEN 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.
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 European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 17706:2023 E
worldwide for CEN national Members.
oSIST prEN 17706:2023
prEN 17706:2023 (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 . 6
6 Apparatus . 8
7 Sampling . 8
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 . 11
9.1 Integration of peaks . 11
9.2 Calculation of inorganic arsenic in the samples . 11
10 Test report . 12
Annex A (informative) Examples of typical chromatographic separation . 13
Annex B (informative) Results of the inter-laboratory study . 17
B.1 Inter-laboratory tests . 17
B.2 Statistical results for determination of inorganic arsenic . 17
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 . 19
Bibliography . 20
oSIST prEN 17706:2023
prEN 17706:2023 (E)
European foreword
This document (prEN 17706:2023) has been prepared by Technical Committee CEN/TC 455 “Plant
Biostimulants”, the secretariat of which is held by AFNOR.
This document is currently submitted to the CEN enquiry.
This document will supersede CEN/TS 17706:2022.
This document has been prepared under a Standardization Request given to CEN by the European
Commission and the European Free Trade Association, and supports essential requirements of EU
Directive(s) / Regulation(s).
For relationship with EU Directive(s) / Regulation(s), see informative Annex ZA, which is an integral part
of this document.
oSIST prEN 17706:2023
prEN 17706:2023 (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 and M/564 Amd1, also contributes to the
Communication on “Innovating for Sustainable Growth: A Bio economy for Europe”. Working Group 4
“Other safety parameters” was created to develop a work programme as part of this request. Technical
committee CEN/TC 455 “Plant Biostimulants” was established to carry out the work programme 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 boosting 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 a standardization request to CEN by the European Commission and the European
Free Trade Association (Mandate M/564) concerning the modernization of methods of analysis of
fertilizers in the framework of Regulation (EU) 2019/1009 of the European Parliament and of the Council.
This document describes a procedure of extraction and measurement for the determination of inorganic
arsenic in plant biostimulants. 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 iAs.
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.
oSIST prEN 17706:2023
prEN 17706:2023 (E)
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 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).
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 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
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
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 describes 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
Under preparation
oSIST prEN 17706:2023
prEN 17706:2023 (E)
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 extracts by ICP-AES (EN 17701-1 and
EN 17701-2 ) could reduce the number of the samples where the determination of iAs is necessary
because if the content of aqua regia (total) extractable arsenic is lower than the legislative limit for iAs
then the determination of iAs is not necessary.
5 Reagents
When using a method of high sensitivity like ICP-MS and HPLC the control of the blank levels of water,
acid and other reagents is very important. The reagents shall be of adequate purity and of recognized
analytical grade. The concentration of arsenic species in the reagents and water used shall be negligible
and low enough not to affect the results of the determination. Generally ultra-pure water from
a purification system and nitric acid of minimum p.a. quality is recommended.
5.1 Water with an electrical conductivity not higher than 0,1 mS/m at 25 °C, having a resistivity
greater than 18,2 MΩ⋅cm.
5.2 Nitric acid (HNO ), concentrated, ≥ 65 % (mass fraction), mass concentration of approximately ρ
(HNO ) 1,4 g/ml.
Use only nitric acid available with high purity (minimum p.a. quality) in order to avoid potential
contamination.
5.3 Hydrogen peroxide, H O not less than 30 % (mass fraction).
2 2
High purity is essential to avoid potential contamination. Commercially available hydrogen peroxide for
analysis should be tested for contamination of arsenic prior to use. It is necessary to prevent peroxide
degradation and ensure the stability of the solution, this is in the discretion of the analyst to use only H O
2 2
of adequate quality
5.4 Extraction solution, 0,1 mol/l HNO in 3 %(V/V) H O .
3 2 2
Add 6,5 ml of HNO (5.2) and thereafter 100 ml of hydrogen peroxide (5.3) into 800 ml water (5.1) in
a 1
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.