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 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 % in the blend by mass or volume, or in the case of liquid form by dry mass. If Plant Biostimulants is not the highest % in the blend, the European Standard for the highest % 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.
The digests are suitable for analysis using EN 17701-2:2024 (ICP-AES) and EN 17701-3:2024 (Hg analysis).
NOTE   Alternatively, inductively coupled plasma mass spectrometry (ICP-MS) can be used for the determination of the elements in the aqua regia digests 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 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.
Die Aufschlüsse sind für die Analyse nach EN 17701-2:2024 (ICP AES) und EN 17701-3:2024 (Quecksilber-Analyse) geeignet.
ANMERKUNG   Alternativ kann die Massenspektrometrie mit induktiv gekoppeltem Plasma (ICP MS) für die Bestimmung der Elemente in den Königswasseraufschlüssen 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. La méthode est applicable à tous les biostimulants des végétaux solides et/ou liquides.
Le présent document est 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.
Les digestats conviennent pour une analyse selon l’EN 17701-2:2024 (ICP-AES) et l’EN 17701-3:2024 (analyse du Hg).
NOTE   Il est également possible d’utiliser la spectrométrie de masse avec plasma à couplage inductif (ICP-MS) pour le dosage des éléments dans les digestats à l’eau régale, si l’utilisateur prouve que la méthode conduit aux mêmes résultats.

Rastlinski biostimulanti - Določanje specifičnih elementov - 1. del: Razklop z zlatotopko za določanje elementov

General Information

Status
Published
Publication Date
26-Nov-2024
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
27-Nov-2024
Due Date
09-Apr-2024
Completion Date
27-Nov-2024

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SLOVENSKI STANDARD
oSIST prEN 17701-1:2023
01-maj-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 - Détermination des éléments spécifiques - Partie 1 :
Digestion par eau régale pour la détermination subséquente des éléments
Ta slovenski standard je istoveten z: prEN 17701-1
ICS:
65.080 Gnojila Fertilizers
oSIST prEN 17701-1:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

oSIST prEN 17701-1:2023
oSIST prEN 17701-1:2023
DRAFT
EUROPEAN STANDARD
prEN 17701-1
NORME EUROPÉENNE
EUROPÄISCHE NORM
March 2023
ICS 65.080 Will supersede CEN/TS 17701-1:2022
English Version
Plant biostimulants - Determination of specific elements -
Part 1: Digestion by aqua regia for subsequent
determination of elements
Biostimulants des végétaux - Détermination des Pflanzen-Biostimulanzien - Bestimmung spezifischer
éléments spécifiques - Partie 1 : Digestion par eau Elemente - Teil 1: Aufschluss durch Königswasser zur
régale pour la détermination subséquente des anschließenden Bestimmung der Elemente
éléments
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 17701-1:2023 E
worldwide for CEN national Members.

oSIST prEN 17701-1:2023
prEN 17701-1:2023 (E)
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 5
5 Sampling and sample preparation . 5
6 Reagents . 5
7 Apparatus . 6
8 Procedure . 6
8.1 Sample digestion . 6
8.2 Sample pre-concentration . 7
8.3 Blank . 7
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
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 . 10
Bibliography . 11
oSIST prEN 17701-1:2023
prEN 17701-1:2023 (E)
European foreword
This document (prEN 17701-1:2023) 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 17701-1:2022.
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.
EN 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.
oSIST prEN 17701-1:2023
prEN 17701-1:2023 (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 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 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 standardization
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 and M/564/Amd1) 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 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. 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.
oSIST prEN 17701-1:2023
prEN 17701-1:2023 (E)
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 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).
1 2
The extracts are suitable for analysis using EN 17701-2:— (ICP-AES) and EN 17701-3:— (Hg analysis).
NOTE Alternatively, inductively coupled plasma mass spectrometry (ICP-MS) can be used for the
determination of the elements in the aqua regia digests 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 method and
3 4
sample preparation method are given in EN 17702-1:— and EN 17702-2:— .
6 Reagents
6.1 The concentration of the analyte or interfering substances in the reagents and the water should be
negligible compared to the lowest concentration to be determined. 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.

Under preparation
Under preparation
Under preparation
Under preparation
oSIST prEN 17701-1:2023
prEN 17701-1:2023 (E)
6.3 Nitric acid 65 %, c(HNO ) ≈ 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 staf
...

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