prEN 16319

Inorganic fertilizers and liming materials - Determination of specific elements - Determination of cadmium, chromium, copper, lead, nickel and zinc by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution

This document specifies a method for the determination of the content of cadmium, chromium, copper, lead, nickel and zinc in fertilizers and liming materials using inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution. Limits of quantification are dependent on the sample matrix as well as on the instrument, but can roughly be expected to be 0,3 mg/kg for Cd and 1 mg/kg for Cr, Cu, Ni, Pb and Zn.
This document is applicable to the fertilizing products blends where a blend is a mix of at least two of the following components: fertilizers, liming materials, soil improvers, growing media, inhibitors, plant biostimulants and where the following category: inorganic fertilizers and liming materials is the highest % in the blend by mass or volume, or in the case of liquid form by dry mass. If inorganic fertilizers and liming materials is not the highest % in the blend, the European Standard for the highest % of the blend applies. In case a fertilizing product blend is composed of components in equal quantity, the user decides which standard to apply.
NOTE 1   The term fertilizer is used throughout this document and needs to be taken to include liming materials unless otherwise indicated.
NOTE 2   Dissolution by aqua regia is equivalent to digestion and extract and digest are equivalent terms in this sense for the purposes of this standard.

Anorganische Düngemittel und Kalkdünger - Bestimmung spezifischer Elemente - Bestimmung von Cadmium, Chrom, Kupfer, Blei, Nickel und Zink durch induktiv gekoppelte Plasma-Atomemissionsspektrometrie (ICP‑AES) nach Auflösung in Königswasser

Dieses Dokument legt ein Verfahren zur Bestimmung des Gehalts an Cadmium, Chrom, Kupfer, Blei, Nickel und Zink in Düngemitteln und Kalkdüngern mit Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP AES) nach Königswasseraufschluss fest. Die Bestimmungsgrenzen sind sowohl von der Probenmatrix als auch vom verwendeten Gerät abhängig, werden jedoch etwa bei 0,3 mg/kg für Cd und 1 mg/kg für Cr, Cu, Ni, Pb und Zn erwartet.
Dieses Dokument ist für Düngeproduktmischungen anwendbar, die sich aus mindestens zwei der Bestandteile Düngemittel, Kalkdünger, Bodenverbesserungsmittel, Kultursubstrate, Hemmstoffe und Pflanzen-Biostimulanzien zusammensetzen und bei denen die Kategorie „anorganische Düngemittel und Kalkdünger“ den größten prozentualen Anteil bezogen auf die Masse oder das Volumen, bzw. bei flüssiger Form bezogen auf die Trockenmasse, ausmacht. Bei Mischungen, bei denen anorganische Düngemittel und Kalkdünger nicht den größten prozentualen Anteil ausmachen, ist die Europäische Norm anwendbar, die für die Kategorie mit dem größten prozentualen Anteil gilt. Falls eine Düngeproduktmischung sich aus Bestandteilen gleicher Menge zusammensetzt, entscheidet der Anwender, welche Norm angewendet wird.
ANMERKUNG 1   Der Begriff Düngemittel ist durchgängig in diesem Dokument verwendet worden und schließt, wenn nicht anders angegeben, die Kalkdünger mit ein.
ANMERKUNG 2   Die Auflösung durch Königswasser entspricht dem Aufschluss und die Benennungen Extrakt und Aufschlussprodukt werden in diesem Sinne im Zusammenhang mit dieser Norm als äquivalent behandelt.

Engrais inorganiques et amendements minéraux basiques - Dosage des éléments spécifiques - Détermination du cadmium, du chrome, du cuivre, du plomb, du nickel et du zinc par spectrométrie d’émission atomique avec plasma induit par haute fréquence (ICP-AES) après digestion à l’eau régale

Le présent document spécifie une méthode permettant de déterminer la teneur en cadmium, chrome, cuivre, plomb, nickel et zinc dans les engrais et amendements minéraux basiques par spectrométrie d’émission atomique avec plasma induit par haute fréquence (ICP-AES) après digestion à l’eau régale. Les limites de quantification dépendent de la matrice de l’échantillon ainsi que de l’instrument, mais peuvent être attendues de l’ordre de 0,3 mg/kg pour Cd et 1 mg/kg pour Cr, Cu, Ni, Pb et Zn.
Le présent document est applicable aux mélanges de produits fertilisants constitués d’au moins deux des composants suivants : engrais, amendements minéraux basiques, amendements du sol, supports de culture, inhibiteurs, biostimulants des végétaux et dans lesquels la catégorie « engrais inorganiques et amendements minéraux basiques » 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 engrais inorganiques et amendements minéraux basiques 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 le mélange de produits fertilisants est constitué de composants en quantités égales, l’utilisateur décide quelle norme appliquer.
NOTE 1   Le terme engrais est utilisé dans le présent document et nécessite d’y inclure les amendements minéraux basiques sauf indication contraire.
NOTE 2   Le terme « digestion » fait référence à la digestion à l’eau régale, et les termes « extrait » et « digestat » sont équivalents au sens de la présente norme.

Anorganska gnojila in sredstva za apnjenje - Določanje specifičnih elementov - Določanje kadmija, kroma, bakra, svinca, niklja in cinka z atomsko emisijsko spektrometrijo z induktivno sklopljeno plazmo (ICP-AES) po raztapljanju v zlatotopki

General Information

• Status: Not Published
• Publication Date: 05-May-2027
• ICS: 65.080 - Fertilizers
• Technical Committee: CEN/TC 260 - Fertilizers and liming materials
• Drafting Committee: CEN/TC 260/WG 3 - Liming materials
• Current Stage: 4020 - Submission to enquiry - Enquiry
• Start Date: 25-Sep-2025
• Due Date: 18-Dec-2025
• Completion Date: 25-Sep-2025
• Directive: 2019/1009 - 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 and amending Regulations (EC) No 1069/2009 and (EC) No 1107/2009 and repealing Regulation (EC) No 2003/2003
• Mandate: M/564 - Fertilising products in support of Regulation (EU) 2019/1009
• Mandate: M/564 AMD 1 - amending Implementing Decision C(2020) 612 as regards certain harmonised standards and standardisation deliverables, deadlines for their adoption and the duration of the validity of the standardisation request
• Mandate: M/564 AMD 2 - Commission Implementing decision amending Implementing Decision C(2020)612 as regards harmonised standards, the deadlines for the adoption of those standards and the duration of the validity of the standardisation request to the European Committee for Standardisation as regards the EU fertilising products in support of Regulation (EU) 2019/1009 of the European Parliament and of the Council
• Ref Project: oSIST prEN 16319:2025 - Inorganic fertilizers and liming materials - Determination of specific elements - Determination of cadmium, chromium, copper, lead, nickel and zinc by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution

Relations

• Revises: EN 16319:2013+A1:2015 - Fertilizers and liming materials - Determination of cadmium, chromium, lead and nickel by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution
• Effective Date: 29-Jan-2025

Standards Content (Sample)

SLOVENSKI STANDARD
01-november-2025
Anorganska gnojila in sredstva za apnjenje - Določanje specifičnih elementov -
Določanje kadmija, kroma, bakra, svinca, niklja in cinka z atomsko emisijsko
spektrometrijo z induktivno sklopljeno plazmo (ICP-AES) po raztapljanju v
zlatotopki
Inorganic fertilizers and liming materials - Determination of specific elements -
Determination of cadmium, chromium, copper, lead, nickel and zinc by inductively
coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution
Anorganische Düngemittel und Kalkdünger - Bestimmung spezifischer Elemente -
Bestimmung von Cadmium, Chrom, Kupfer, Blei, Nickel und Zink durch induktiv
gekoppelte Plasma-Atomemissionsspektrometrie (ICP‑AES) nach Auflösung in
Königswasser
Engrais inorganiques et amendements minéraux basiques - Dosage des éléments
spécifiques - Détermination du cadmium, du chrome, du cuivre, du plomb, du nickel et
du zinc par spectrométrie d’émission atomique avec plasma induit par haute fréquence
(ICP-AES) après digestion à l’eau régale
Ta slovenski standard je istoveten z: prEN 16319
ICS:
65.080 Gnojila Fertilizers
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

DRAFT
EUROPEAN STANDARD
NORME EUROPÉENNE
EUROPÄISCHE NORM
September 2025
ICS 65.080 Will supersede EN 16319:2013+A1:2015
English Version
Inorganic fertilizers and liming materials - Determination
of specific elements - Determination of cadmium,
chromium, copper, lead, nickel and zinc by inductively
coupled plasma-atomic emission spectrometry (ICP-AES)
after aqua regia dissolution
Engrais inorganiques et amendements minéraux Anorganische Düngemittel und Kalkdünger -
basiques - Dosage des éléments spécifiques - Bestimmung spezifischer Elemente - Bestimmung von
Détermination du cadmium, du chrome, du cuivre, du Cadmium, Chrom, Kupfer, Blei, Nickel und Zink durch
plomb, du nickel et du zinc par spectrométrie induktiv gekoppelte Plasma-
d'émission atomique avec plasma induit par haute Atomemissionsspektrometrie (ICP-AES) nach
fréquence (ICP-AES) après digestion à l'eau régale Auflösung in Königswasser
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 260.
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
© 2025 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 16319:2025 E
worldwide for CEN national Members.

Contents Page
European foreword . 3
1 Scope . 4
2 Normative references . 4
3 Terms and definitions . 4
4 Principle . 5
5 Sampling and sample preparation . 5
6 Reagents . 6
7 Apparatus . 7
8 Procedure . 7
8.1 Preparation of the test solution – sample digestion . 7
8.2 Preparation of the test solution for the correction of matrix effects by spike recovery . 8
8.3 Preparation of the blank test solution . 8
8.4 Preparation of the calibration solutions for the analysis of cadmium, chromium,
copper, lead, nickel and zinc . 8
8.5 Determination of cadmium, chromium, copper, lead, nickel and zinc by ICP-AES . 8
8.5.1 Instrument conditions . 8
8.5.2 Measurement . 9
8.5.3 Interferences . 9
9 Calculation and expression of the results . 10
9.1 General. 10
9.2 Correction for spike recovery . 11
9.3 Calculation of the element content in the sample . 11
10 Precision . 12
10.1 Inter-laboratory study . 12
10.2 Repeatability . 12
10.3 Reproducibility . 12
11 Test report . 14
Annex A (informative) Adjustment of the procedure to different final volumes . 15
Annex B (informative) Results of the inter-laboratory study . 16
B.1 Inter-laboratory study . 16
B.2 Statistical results for the determination of cadmium, chromium, copper, lead, nickel
and zinc by inductively coupled plasma-atomic emission spectrometry (ICP-AES)
after aqua regia dissolution . 16
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 . 23
Bibliography . 25
European foreword
This document (prEN 16319:2025) has been prepared by Technical Committee CEN/TC 260 “Fertilizers
and liming materials”, the secretariat of which is held by DIN.
This document is currently submitted to the CEN Enquiry.
This document will supersede EN 16319:2013+A1:2015.
In comparison with EN 16319:2013+A1:2015, the following technical modifications have been made:
— determination of Cu and Zn included in Clause 1 (Scope), Clause 6 (Reagents) and Clause 8
(Procedure) of the text;
— extraction procedure adapted (8.1) for technical progress (graphite blocks and smaller volumes of
acids included);
— normative references and bibliography updated;
— terms and definitions updated;
— Clause 10 (Precision) updated;
— Annex B updated (results of inter-laboratory study added);
— Annex ZA added.
This document has been prepared under a standardization request addressed to CEN by the European
Commission. The Standing Committee of the EFTA States subsequently approves these requests for its
Member States.
For the relationship with EU Legislation, see informative Annex ZA, which is an integral part of this
document.
1 Scope
This document specifies a method for the determination of the content of cadmium, chromium, copper,
lead, nickel and zinc in fertilizers and liming materials using inductively coupled plasma-atomic emission
spectrometry (ICP-AES) after aqua regia dissolution. Limits of quantification are dependent on the
sample matrix as well as on the instrument, but can roughly be expected to be 0,3 mg/kg for Cd and
1 mg/kg for Cr, Cu, Ni, Pb and Zn.
This document is applicable to the fertilizing products blends where a blend is a mix of at least two of the
following components: fertilizers, liming materials, soil improvers, growing media, inhibitors, plant
biostimulants and where the following category: inorganic fertilizers and liming materials is the
highest % in the blend by mass or volume, or in the case of liquid form by dry mass. If inorganic fertilizers
and liming materials is not the highest % in the blend, the European Standard for the highest % of the
blend applies. In case a fertilizing product blend is composed of components in equal quantity, the user
decides which standard to apply.
NOTE 1 The term fertilizer is used throughout this document and needs to be taken to include liming materials
unless otherwise indicated.
NOTE 2 Dissolution by aqua regia is equivalent to digestion and extract and digest are equivalent terms in this
sense for the purposes of this standard.
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.
EN 1482-2:2024, Fertilizers, liming materials and inhibitors — Sampling and sample preparation —
Part 2: General sample preparation provisions
EN 12944-1:1999, Fertilizers and liming materials — Vocabulary — Part 1: General terms
EN 12944-2:1999, Fertilizers and liming materials — Vocabulary — Part 2: Terms relating to fertilizers
EN 12944-3:2019, Fertilizers and liming materials — Vocabulary — Part 3: Terms relating to liming
materials
EN 14787:2005, Fertilizers and liming materials — Determination of water content — Guidelines and
recommendations
3 Terms and definitions
For the purposes of this document, the terms and definitions given in EN 12944-1:1999,
EN 12944-2:1999 and EN 12944-3:2019, and the following apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https://www.iso.org/obp/
— IEC Electropedia: available at https://www.electropedia.org/

As impacted by EN 12944-1:1999/AC:2000.
As impacted by EN 12944-2:1999/AC:2000.
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
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
3.6
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
3.7
stock solution
solution with accurately known analyte
...