Plant biostimulants - Determination of specific elements - Part 1: Digestion by aqua regia for subsequent determination of elements

This document specifies the method for the digestion of different plant biostimulants with aqua regia to enable a subsequent determination of arsenic (As), cadmium (Cd), copper (Cu), chromium (Cr), mercury (Hg), nickel (Ni), lead (Pb) and zinc (Zn). The method can be also applied for determination of other elements. The method is applicable for all solid and/or liquid plant biostimulants.
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.
The extracts are suitable for analysis using CEN/TS 17701-2 (ICP-AES) and CEN/TS 17701-3 (Hg analysis).
NOTE   Alternatively, inductively coupled plasma mass spectrometry (ICP-MS) can be used for the measurement if the user proves that the method gives the same results.

Pflanzen-Biostimulanzien - Bestimmung spezifischer Elemente - Teil 1: Aufschluss durch Königswasser zur anschließenden Bestimmung der Elemente

Dieses Dokument legt das Verfahren für den Aufschluss verschiedener Pflanzen-Biostimulanzien mit Königswasser fest, um eine anschließende Bestimmung von Arsen (As), Cadmium (Cd), Kupfer (Cu), Chrom (Cr), Quecksilber (Hg), Nickel (Ni), Blei (Pb) und Zink (Zn) zu ermöglichen. Das Verfahren kann auch für die Bestimmung anderer Elemente verwendet werden. Das Verfahren ist für alle festen und/oder flüssigen Pflanzen-Biostimulanzien anwendbar.
Dieses Dokument ist auch für die Mischungen von Düngeprodukten, in denen die Pflanzen-Biostimulanzien der Hauptbestandteil der Mischung sind, anwendbar. Andernfalls gilt die Technische Spezifikation für den Hauptbestandteil der Mischung.
Die Extrakte sind für die Analyse nach CEN/TS 17701 2 (ICP AES) und CEN/TS 17701 3 (Quecksilber-Analyse) geeignet.
ANMERKUNG   Alternativ kann die Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP MS) für die Messung genutzt werden, sofern der Anwender nachweist, dass das Verfahren zu den gleichen Ergebnissen führt.

Biostimulants des végétaux - Dosage des éléments spécifiques - Partie 1 : Digestion à l'eau régale pour le dosage ultérieur des éléments

Le présent document spécifie la méthode pour la digestion de différents biostimulants des végétaux à l’eau régale pour permettre le dosage ultérieur de l’arsenic (As), du cadmium (Cd), du cuivre (Cu), du chrome (Cr), du mercure (Hg), du nickel (Ni), du plomb (Pb) et du zinc (Zn). Cette méthode peut aussi être appliquée pour le dosage d’autres éléments. Cette méthode est applicable à tous les biostimulants des végétaux solides et/ou liquides.
Le présent document est également applicable aux mélanges de fertilisants dont la majeure partie est constituée de biostimulants des végétaux. Dans le cas contraire, la Spécification technique relative au constituant principal du mélange s’applique.
Les extraits conviennent pour une analyse selon la CEN/TS 17701-2 (ICP-AES) et la CEN/TS 17701-3 (analyse du Hg).
NOTE   Il est également possible d’utiliser la spectrométrie de masse avec plasma à couplage inductif (ICP-MS) pour la mesure, si l’utilisateur prouve que la méthode conduit aux mêmes résultats.

Rastlinski biostimulanti - Določevanje specifičnih elementov - 1. del: Razklop z zlatotopko za določevanje elementov

Ta dokument določa postopek za razklop različnih rastlinskih biostimulantov z zlatotopko, da se omogoči naknadno določanje arzena (As), kadmija (Cd), bakra (Cu), kroma (Cr), živega srebra (Hg), niklja (Ni), svinca (Pb) in cinka (Zn). Postopek je mogoče uporabiti tudi za določanje drugih elementov. Postopek se uporablja za vse trdne in/ali tekoče rastlinske biostimulante.
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.
Izvlečki so primerni za analizo v skladu s standardom CEN/TS 17701-2 (ICP-AES) in CEN/TS 17701-3 (analiza Hg).
OPOMBA:   Druga možnost je, da se za meritev uporabi masna spektrometrija z induktivno sklopljeno plazmo (ICP-MS), če uporabnik dokaže, da metoda daje enake rezultate.

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
01-februar-2023
Rastlinski biostimulanti - Določevanje specifičnih elementov - 1. del: Razklop z
zlatotopko za določevanje elementov
Plant biostimulants - Determination of specific elements - Part 1: Digestion by aqua regia
for subsequent determination of elements
Pflanzen-Biostimulanzien - Bestimmung spezifischer Elemente - Teil 1: Aufschluss durch
Königswasser zur anschließenden Bestimmung der Elemente
Biostimulants des végétaux - Dosage des éléments spécifiques - Partie 1 : Digestion à
l'eau régale pour le dosage ultérieur des éléments
Ta slovenski standard je istoveten z: CEN/TS 17701-1:2022
ICS:
65.080 Gnojila Fertilizers
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

CEN/TS 17701-1
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
March 2022
TECHNISCHE SPEZIFIKATION
ICS 65.080
English Version
Plant biostimulants - Determination of specific elements -
Part 1: Digestion by aqua regia for subsequent
determination of elements
Biostimulants des végétaux - Dosage des éléments Biostimulanzien für die pflanzliche Anwendung -
spécifiques - Partie 1 : Digestion à l'eau régale pour le Bestimmung spezifischer Elemente - Teil 1: Aufschluss
dosage ultérieur des éléments durch Königswasser zur anschließenden Bestimmung
der Elemente
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 17701-1:2022 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 Sampling and sample preparation . 5
6 Reagents . 6
7 Apparatus . 6
8 Procedure. 6
9 Test report . 7
Annex A (informative) Adjustment to different digestion procedures and measurement
apparatuses . 8
A.1 Adjustment of the procedure to different final volumes . 8
A.2 Calculation of the sample weight . 8
A.2.1 General . 8
A.2.2 Calculation of the weight of the sample (dry matter) . 9
A.2.3 Calculation of the weight of the sample for analysis . 9
A.2.4 Example . 9
Bibliography . 10

European foreword
This document (CEN/TS 17701-1:2022) 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.
The CEN/TS 17701 series, Plant biostimulants - Determination of specific elements, consists of the
following parts:
— Part 1: Digestion by aqua regia for subsequent determination of elements;
— Part 2: Determination of total content of Cd, Pb, Ni, As, Cr, Cu and Zn;
— Part 3: Determination of mercury.
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 the European Parliament and of the Council of 5 June 2019 laying down
rules on the making available on the market of EU fertilising 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”. Working Group 4 “Other safety parameters” was
created to develop a work program as part of this standardization request. 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.
Aqua regia is applied to digest different matrices for the subsequent determination of many elements.
For example, a multi-matrix standard for aqua regia extraction of soils, sludges and biowaste was
prepared by CEN/TC 444. A similar procedure was applied for determination of aqua regia extractable
contents of arsenic, mercury, cadmium, chromium, nickel and lead in fertilizers and liming materials
(standard prepared by CEN/TC 260). CEN/TC 260 also prepared a standard for extraction of a total
micronutrients content in fertilizers using aqua regia. CEN/TC 223 published a standard for a similar
procedure for soil improvers and growing media. Wide use of the aqua regia digestion, availability of the
instruments and the possibility to merge the standards for different matrices in future, were the main
reasons for also applying this method of digestion for plant biostimulants. A simple pre-concentration
procedure is a part of this document to also cover the digestion of liquid samples with low dry matter
content in the case that the measurement method is not sufficiently sensitive. An Annex A describes in
detail the calculation of the initial sample weight to be taken for the pre-concentration step to achieve
concentrations of the individual elements above the limit of quantification (LOQ).
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 the method for the digestion of different plant biostimulants with aqua regia to
enable a subsequent determination of arsenic (As), cadmium (Cd), copper (Cu), chromium (Cr), mercury
(Hg), nickel (Ni), lead (Pb) and zinc (Zn). The method can be also applied for determination of other
elements. The method is applicable for all solid and/or liquid plant biostimulants.
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.
The extracts are suitable for analysis using CEN/TS 17701-2 (ICP-AES) and CEN/TS 17701-3
(Hg analysis).
NOTE Alternatively, inductively coupled plasma mass spectrometry (ICP-MS) can be used for the measurement
if the user proves that the method gives the same results.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
digestion
mineralization of the organic matter of a sample and dissolution of its mineral part, more or less
completely, when reacting with a reagent mixture
3.2
blank test solution
solution prepared in the same way as the test sample solution but omitting the test portion
4 Principle
The samples are digested by boiling in aqua regia for two hours under reflux conditions.
5 Sampling and sample preparation
Sampling and sample preparation are not part of this document. A recommended sampling and a sample
preparation method is given in:
CEN/TS 17702-1, Plant biostimulants - Sampling and sample preparation - Part 1: Sampling;
CEN/TS 17702-2, Plant biostimulants - Sampling and sample preparation - Part 2: Sample preparation.
6 Reagents
6.1 Water with a specific conductivity not higher than 0,2 mS/m at 25 °C, free from the
elements to be determined.
6.2 Hydrochloric acid 37 %, c(HCl) ≈ 12 mol/l, ρ ≈ 1,18 g/ml.
6.3 Nitric acid 65 %, c(HNO3) ≈ 14,3 mol/l, ρ ≈ 1,4 g/ml.
6.4 Antifoaming agent, e.g. n-dodecane (C H ) or octanol (C H O) are suitable.
12 26 8 18
7 Apparatus
7.1 Common laboratory glassware. All glassware and plastic ware shall be adequately
cleaned and stored to avoid any contamination.
7.2 Apparatus for thermal heating digestion, temperature controlled with reaction vessel
and reflux condenser. The capacity of the reaction vessel should be at least 5 times of the
volume of the aqua regia used.
7.3 Filter paper, ash free and of recognized and tested quality.
7.4 Analytical balance capable of weighing to an accuracy of 1 mg or better.
8 Procedure
CAUTION – Suitable precautions shall be taken to avoid any contact of laboratory staff with acid fumes.
The digestion procedure shall be carried out in a well-ventilated fume cupboard.
8.1 Sample digestion
This procedure can be used for all samples of plant biostimulants if a sufficiently sensitive method for
determination is used. For some liquid samples with a low dry matter content, a pre-concentration step
(8.2) can be necessar
...

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