kSIST-TS FprCEN/TS 17706:2021
(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 HPLC or IC coupled to ICP-MS.
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.
Biostimulanzien für die pflanzliche Anwendung - Bestimmung von anorganischem Arsen
Dieses Dokument legt ein Verfahren zur Extraktion, Trennung und Bestimmung von anorganischem Arsen in Biostimulanzien für die pflanzliche Anwendung mit Anionenaustausch HPLC oder IC gekoppelt mit ICP MS fest.
Dieses Dokument gilt auch für die Mischungen von Düngeprodukten, in denen die Biostimulanzien für die pflanzliche Anwendung der Hauptbestandteil der Mischung sind. Andernfalls gilt die Technische Spezifikation für den Hauptbestandteil der Mischung.
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 HPLC échangeuse d’anions ou par IC couplée à une ICP-MS.
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 anorganskega arzena
General Information
Standards Content (sample)
SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 17706:2021
01-november-2021
Rastlinski biostimulansi - Določevanje anorganskega arzena
Plant biostimulants - Determination of inorganic arsenic
Biostimulanzien für die pflanzliche Anwendung - Bestimmung von anorganischem Arsen
Biostimulants des végétaux - Dosage de l'arsenic inorganiqueTa slovenski standard je istoveten z: FprCEN/TS 17706
ICS:
65.080 Gnojila Fertilizers
kSIST-TS FprCEN/TS 17706:2021 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 17706:2021
FINAL DRAFT
TECHNICAL SPECIFICATION
FprCEN/TS 17706
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
September 2021
ICS 07.080
English Version
Plant biostimulants - Determination of inorganic arsenic
Biostimulants des végétaux - Dosage de l'arsenic Biostimulanzien für die pflanzliche Anwendung -
inorganique Bestimmung von anorganischem ArsenThis 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 17706:2021 E
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kSIST-TS FprCEN/TS 17706:2021
FprCEN/TS 17706:2021 (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 ............................................................................................................................................................. 6
6 Apparatus ........................................................................................................................................................... 7
7 Sampling ............................................................................................................................................................. 8
8 Procedure........................................................................................................................................................... 8
8.1 Sample preparation ........................................................................................................................................ 8
8.2 Water bath extraction ................................................................................................................................... 8
8.3 Preparation of the calibration solutions ................................................................................................ 8
8.4 Measurement .................................................................................................................................................... 9
8.4.1 General instrumental conditions .............................................................................................................. 9
8.4.2 HPLC-ICP/MS measurement of inorganic arsenic ............................................................................... 9
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 ...................................................................................................................................................... 11
Annex A (informative) Examples of typical chromatographic separation ............................................. 13
Bibliography ................................................................................................................................................................. 16
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FprCEN/TS 17706:2021 (E)
European foreword
This document (FprCEN/TS 17706:2021) 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 Vote on TS.
This document has been prepared under a Standardization Request given to CEN by the European
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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
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 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.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.
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.---------------------- Page: 6 ----------------------
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1 Scope
This document specifies a method for extraction, separation, and determination of inorganic arsenic (iAs)
in plant biostimulants using anion-exchange HPLC or IC coupled to ICP-MS.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 referencesThe 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, Plant biostimulants — Determination of dry matter3 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
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
3.3blank test solution
solution prepared in the same way as the test sample solution but omitting the test portion
3.4calibration solution
solution used to calibrate the instrument, prepared from stock solutions by adding acids, buffer, reference
element and salts as needed3.5
stock solution
solution with accurately known analyte concentration(s), prepared from pure chemicals
4 PrincipleThis 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-
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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 extracts by ICP-AES (FprCEN/TS 17701-1
and FprCEN/TS 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.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 1 000 ml volumetric flask. Fill the flask to the mark with water (5.1.). This solution is prepared on the
day of use.It is recommended that the total volume needed for the analysis is estimated and only this amount is
produced in the day of use.5.5 Ammonium carbonate, (NH ) CO , mass fraction w ≥ 99,999 %, for preparation of the mobile
4 2 3phase solution.
5.6 Aqueous ammonia, (NH (aq).) w ≥ 25 %, for adjustment of pH in the mobile phase.
5.7 Methanol, (CH OH), HPLC grade, for preparation of the mobile phase solution.5.8 Mobile phase, e.g. 50 mmol/l ammonium carbonate in 3 % methanol at pH 10,3
Dissolve 4,80 g of ammonium carbonate (5.5) in approximately 800 ml water (5.1). Adjust the pH to 10,3
with aqueous ammonia (5.6) and add 30 ml of methanol (5.7) and then fill up to 1 000 ml with water
(5.1). Prior to use filter the mobile phase solution through a 0,45 µm filter using a filtering device (6.4).
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The optimal concentration of ammonium carbonate in the mobile phase depends on the analytical column
used (e.g. brand, particle size and dimensions) and should be verified in advance. The appropriate
concentration of ammonium carbonate (usually between 10 and 50 mmol/l) is highly dependent on the
column used and is up to the discretion of the analyst. It should fulfil the criteria for sufficient resolution
of the arsenate peak.Methanol is added to the mobile phase in order to enhance the signal intensity for arsenic. The
concentration of methanol to achieve the highest signal to noise ratio depends on the instrument used
and should be identified by the analyst.Different mobile phase may be also used according to the instructions of the manufacturer of th
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