CEN/TS 17706:2022
(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 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 anorganischem Arsen
Dieses Dokument legt ein Verfahren zur Extraktion, Trennung und Bestimmung von anorganischem Arsen in Planzen-Biostimulanzien mit Anionenaustausch Hochleistungs-Flüssigchromatograph (HPLC) oder Ionenchromatographie (IC) gekoppelt mit ICP MS fest.
Dieses Dokument ist auch anzuwenden für die Mischungen von Düngeprodukten, in denen die Planzen-Biostimulanzien der Hauptbestandteil der Mischung sind. Andernfalls ist die Technische Spezifikation für den Hauptbestandteil der Mischung anzuwenden.
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 liquide haute performance (HPLC) ou chromatographie ionique (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
Ta dokument določa metodo za ekstrakcijo, ločevanje in določevanje anorganskega arzena (iAs) v rastlinskih biostimulantih z anionsko izmenjavo HPLC ali IC v povezavi z masno spektrometrijo z induktivno sklopljeno plazmo (ICP-MS).
Dokument je uporaben tudi za mešanice sredstev za gnojenje, pri katerih so rastlinski biostimulanti glavni del mešanice. V nasprotnem primeru se uporablja tehnična specifikacija za glavni del mešanice.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-februar-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: CEN/TS 17706:2022
ICS:
65.080 Gnojila Fertilizers
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
CEN/TS 17706
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
March 2022
TECHNISCHE SPEZIFIKATION
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 Arsen
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 17706:2022 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 . 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
9 Calculation and expression of the results . 10
9.1 Integration of peaks . 10
9.2 Calculation of inorganic arsenic in the samples . 11
10 Test report . 11
Annex A (informative) Examples of typical chromatographic separation . 12
Bibliography . 15
European foreword
This document (CEN/TS 17706:2022) has been prepared by 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.
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
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.
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 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
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
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 (CEN/TS 17701-1 and
CEN/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.
) CO , mass fraction w ≥ 99,999 %, for preparation of the mobile
5.5 Ammonium carbonate, (NH
4 2 3
phase 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
wit
...
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