Plant biostimulants - Determination of specific elements - Part 2: Determination of total content of Cd, Pb, Ni, As, Cr, Cu and Zn

This document specifies a method for the determination of arsenic (As), cadmium (Cd), copper (Cu), chromium (Cr), lead (Pb), nickel (Ni) and zinc (Zn) in plant biostimulant digests using inductively coupled plasma-atomic emission spectrometry (ICP-AES).
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.
This method is applicable to aqua regia digests prepared according to CEN/TS 17701-1. The method can be used for the determination of other elements, provided the user has verified the applicability.

Pflanzen-Biostimulanzien - Bestimmung spezifischer Elemente - Teil 2: Bestimmung des Gesamtgehaltes an Cd, Pb, Ni, As, Cr, Cu und Zn

Dieses Dokument legt ein Verfahren zur Bestimmung des Gehalts an Arsen (As), Cadmium (Cd), Kupfer (Cu), Chrom (Cr), Blei (Pb), Nickel (Ni) und Zink (Zn) in Pflanzen-Biostimulanzien mit Atomemissions¬spektrometrie mit induktiv gekoppeltem Plasma (ICP AES) nach Aufschluss fest.
Dieses Dokument ist auch für die Mischungen von Düngeprodukten anwendbar, in denen die Pflanzen-Biostimulanzien der Hauptbestandteil der Mischung sind. Andernfalls gilt die Technische Spezifikation für den Hauptbestandteil der Mischung.
Das Verfahren ist für Königswasseraufschlüsse anwendbar, die nach CEN/TS 17701 1 hergestellt wurden. Das Verfahren kann zur Bestimmung anderer Elemente angewendet werden, vorausgesetzt der Anwender hat die Anwendbarkeit überprüft.

Biostimulants des végétaux - Dosage des éléments spécifiques - Partie 2 : Détermination de la teneur totale en Cd, Pb, Ni, As, Cr, Cu et Zn

Le présent document spécifie une méthode pour le dosage de l’arsenic (As), du cadmium (Cd), du cuivre (Cu), du chrome (Cr), du plomb (Pb), du nickel (Ni) et du zinc (Zn) dans les digestats de biostimulants des végétaux par spectrométrie d’émission atomique par un plasma à couplage inductif (ICP-AES).
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.
Cette méthode est applicable aux digestats à l’eau régale préparés conformément à la CEN/TS 17701-1. La méthode peut également être utilisée pour le dosage d’autres éléments, à condition que l’utilisateur ait vérifié son applicabilité.

Rastlinski biostimulanti - Določevanje specifičnih elementov - 2. del: Določevanje celotnega Cd, Pb, Ni, As, Cr, Cu in Zn

General Information

Status
Published
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
23-Mar-2022
Completion Date
23-Mar-2022

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SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 17701-2:2021
01-november-2021
Rastlinski biostimulansi - Določevanje določenih elementov - 2. del: Določevanje
celotnega Cd, Pb, Ni, As, Cr, Cu in Zn

Plant biostimulants - Determination of specific elements - Part 2: Determination of total

content of Cd, Pb, Ni, As, Cr, Cu and Zn

Biostimulanzien für die pflanzliche Anwendung - Bestimmung spezifischer Elemente -

Teil 2: Bestimmung des Gesamtgehaltes an Cd, Pb, Ni, As, Cr, Cu und Zn
Biostimulants des plantes - Détermination des éléments spécifiques - Partie 2 :
Détermination du contenu total en Cd, Pb, Ni, As, Cr, Cu et Zn
Ta slovenski standard je istoveten z: FprCEN/TS 17701-2
ICS:
65.080 Gnojila Fertilizers
kSIST-TS FprCEN/TS 17701-2:2021 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 17701-2:2021
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kSIST-TS FprCEN/TS 17701-2:2021
FINAL DRAFT
TECHNICAL SPECIFICATION
FprCEN/TS 17701-2
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
September 2021
ICS 65.080
English Version
Plant biostimulants - Determination of specific elements -
Part 2: Determination of total content of Cd, Pb, Ni, As, Cr,
Cu and Zn

Biostimulants des plantes - Détermination des Biostimulanzien für die pflanzliche Anwendung -

éléments spécifiques - Partie 2 : Détermination du Bestimmung spezifischer Elemente - Teil 2:

contenu total en Cd, Pb, Ni, As, Cr, Cu et Zn Bestimmung des Gesamtgehaltes an Cd, Pb, Ni, As, Cr,

Cu und Zn

This 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 17701-2:2021 E

worldwide for CEN national Members.
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kSIST-TS FprCEN/TS 17701-2:2021
FprCEN/TS 17701-2:2021 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

Introduction .................................................................................................................................................................... 4

1 Scope .................................................................................................................................................................... 5

2 Normative references .................................................................................................................................... 5

3 Terms and definitions ................................................................................................................................... 5

4 Principle ............................................................................................................................................................. 6

5 Interferences .................................................................................................................................................... 6

5.1 General ................................................................................................................................................................ 6

5.2 Spectral interferences ................................................................................................................................... 6

5.3 Transport interferences ............................................................................................................................... 6

5.4 Excitation interferences ............................................................................................................................... 6

5.5 Chemical interferences ................................................................................................................................. 7

5.6 Memory interferences ................................................................................................................................... 7

6 Reagents ............................................................................................................................................................. 7

7 Apparatus ........................................................................................................................................................... 8

7.1 Common laboratory glassware. ................................................................................................................. 8

7.2 Inductively coupled plasma atomic emission spectrometer. .......................................................... 8

8 Procedure........................................................................................................................................................... 8

8.1 Preparation of test and blank solution ................................................................................................... 8

8.2 Preparation of the calibration solutions ................................................................................................ 8

8.3 Measurement .................................................................................................................................................... 9

8.3.1 Instrument conditions ................................................................................................................................... 9

8.3.2 Optimization of the instrument conditions ........................................................................................... 9

8.3.3 Interferences .................................................................................................................................................... 9

8.3.4 Measurement .................................................................................................................................................... 9

8.3.5 Matrix effects .................................................................................................................................................... 9

8.3.6 Spiking.............................................................................................................................................................. 10

9 Calculation and expression of the results ........................................................................................... 11

10 Test report ...................................................................................................................................................... 12

Bibliography ................................................................................................................................................................. 13

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kSIST-TS FprCEN/TS 17701-2:2021
FprCEN/TS 17701-2:2021 (E)
European foreword

This document (FprCEN/TS 17701-2:2021) has been prepared by the 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.

The CEN/TS 17701 series, Plant biostimulants - Determination of specific elements, consists of the

following parts:

— CEN/TS 17701-1, Plant biostimulants - Determination of specific elements - Part 1: Digestion by aqua

regia for subsequent determination of elements;

— CEN/TS 17701-2, Plant biostimulants - Determination of specific elements - Part 2: Determination of

total content of Cd, Pb, Ni, As, Cr, Cu and Zn;

— CEN/TS 17701-3, Plant biostimulants - Determination of specific elements - Part 3: Determination of

mercury.
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kSIST-TS FprCEN/TS 17701-2:2021
FprCEN/TS 17701-2:2021 (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 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 is part of a modular approach and concerns the analytical measurement step. “Modular”

means that a test standard concerns a specific step in assessing a property and not the whole chain of

measurements. Inductively coupled plasma atomic emission spectrometry (ICP-AES) is nowadays widely

used and a well-established method in many laboratories.

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.
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kSIST-TS FprCEN/TS 17701-2:2021
FprCEN/TS 17701-2:2021 (E)
1 Scope

This document specifies a method for the determination of arsenic (As), cadmium (Cd), copper (Cu),

chromium (Cr), lead (Pb), nickel (Ni) and zinc (Zn) in plant biostimulant digests using inductively coupled

plasma-atomic emission spectrometry (ICP-AES).

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.

This method is applicable to aqua regia digests prepared according to CEN/TS 17701-1. The method can

be used for the determination of other elements, provided the user has verified the applicability.

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 17701-1, Plant biostimulants - Determination of specific elements - Part 1: Digestion by aqua regia

for subsequent determination of elements
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
digest

solution received after mineralization of the organic matter of a sample and dissolution of its mineral

part, more or less completely, when reacting with a reagent mixture
3.6
stock solution

solution with accurately known analyte concentration(s), prepared from pure chemicals (6.5)

3.7
test sample solution

solution prepared after extraction or digestion of the test sample according to appropriate specifications

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kSIST-TS FprCEN/TS 17701-2:2021
FprCEN/TS 17701-2:2021 (E)
4 Principle

The method is based on the inductively coupled plasma atomic emission spectrometry (ICP-AES)

measurement of the concentration of arsenic, cadmium, copper, chromium, lead, nickel and zinc in plant

biostimulant aqua regia digests. The elements are determined after an appropriate dilution of the digest,

if necessary. The solution is dispersed by a suitable nebulizer of the ICP-AES instrument and the resulting

aerosol is transported into the plasma torch. Element specific emission spectra are produced by a

radiofrequency inductively coupled argon plasma where atoms or ions are excited at high temperature.

The emission spectra are dispersed by a spectrometer, and the intensities of the emission lines are

monitored by photosensitive devices. Multi-element determinations using sequential or simultaneous

optical systems and axial, radial or dual viewing of the plasma may be used.
5 Interferences
5.1 General

Interferences and matrix effects shall be recognized and appropriate measures to minimize them shall be

made. There are several types of interferences – see 5.2 – 5.6.
5.2 Spectral interferences

Spectral interferences are due to incomplete isolation of the radiation emitted by the analyte from other

detected radiation sources. Spectral interferences are caused by the background emission from

continuous or recombination phenomena, by stray light which causes background increase or overlap of

a spectral line from another element, or by the unresolved overlap of molecular band spectra. Background

emission and stray light can usually be compensated for by subtracting the background emission

measured adjacent to the analyte wavelength peak. To correct a sloping background shift background

correction points on each side of the peak are used. The increase of background is more intensive with

axial-view instruments. Background correction is not required in cases of line broadening where a

background correction measurement would actually degrade the analytical result. A spectral line overlap

usually leads to the choice of an alternative line. If this is not possible, mathematical correction

procedures (e.g. inter-element correction technique or multi-component spectral fitting) can be used to

compensate for the interference. These correction procedures are usually a part of the instrument

software.
5.3 Transport interferences

Transport interferences are caused by differences in the properties between the sample solutions and

the calibration solutions (viscosity, surface tension, density, dissolved solid content, type and

concentration of acids). As a consequence, the supply of solutio
...

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