Fertilizers and liming materials - Determination of cadmium, chromium, lead and nickel by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution

This European Standard specifies a method for the determination of the content of cadmium, chromium, nickel and lead in fertilizers with inductively coupled plasma atomic emission spectrometry (ICP-AES) after extraction with aqua regia. 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, Ni and Pb.
NOTE   Due to significant interference from Cu, Fe and Mn, no valid results can be reported using this method for fertilizer matrices containing high concentrations (>/= 10 %) of these micro-nutrients.

Düngemittel und Kalkdünger - Bestimmung von Cadmium, Chrom, Blei und Nickel mit Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-AES) nach Königswasseraufschluss

Diese Europäische Norm legt ein Verfahren zur Bestimmung des Gehalts an Cadmium, Chrom, Nickel und Blei in Düngemitteln 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, Ni und Pb erwartet.
ANMERKUNG   Aufgrund signifikanter Störungen durch Cu, Fe und Mn können bei Anwendung dieses Verfahrens für Düngemittelmatrizes mit hohen Konzentrationen (≥ 10 %) dieser Spurennährstoffe keine zuverlässigen Ergebnisse ausgewiesen werden.

Engrais et amendements minéraux basiques - Détermination du cadmium, chrome, plomb et nickel par spectrométrie d'émission atomique avec plasma induit par haute fréquence (ICP-AES) après digestion à l'eau régale

La présente norme européenne spécifie une méthode permettant de déterminer la teneur en cadmium, chrome, nickel et plomb dans les engrais par spectrométrie d’émission atomique avec plasma à couplage inductif (ICP-AES) après extraction 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, Ni et Pb.
NOTE Du fait d’une interférence significative du Cu, Fe et Mn, aucun résultat valide ne peut être donné en utilisant cette méthode pour les matrices engrais contenants des concentrations élevés (≥ 10%) en ces oligo-éléments.

Gnojila in sredstva za apnjenje - Določevanje kadmija, kroma, svinca in niklja z atomsko emisijsko spektrometrijo z induktivno sklopljeno plazmo (ICP/AES) po raztapljanju v zlatotopki (vključno z dopolnilom A1)

Ta evropski standard določa metodo za določevanje vsebnosti kadmija, kroma, niklja in svinca v gnojilih z atomsko emisijsko spektrometrijo z induktivno sklopljeno plazmo (ICP-AES) po ekstrakciji z zlatotopko. Meje kvantifikacije so odvisne od matrice vzorca in instrumenta, vendar za Cd običajno znašajo približno 0,3 mg/kg, za Cr, Ni in Pb pa 1 mg/kg.
OPOMBA: Zaradi znatne interference primesi Cu, Fe in Mn ni mogoče posredovati nobenih veljavnih rezultatov s to metodo za matrice gnojil, ki vsebujejo visoke koncentracije teh mikro hranil (>/= 10 %).

General Information

Status
Published
Publication Date
22-Dec-2015
Current Stage
9093 - Decision to confirm - Review Enquiry
Start Date
05-Jun-2025
Completion Date
23-Sep-2025

Relations

Effective Date
21-Oct-2015
Effective Date
21-Oct-2015
Effective Date
29-Jan-2025

Overview

EN 16319:2013+A1:2015 (CEN) specifies a validated laboratory method for determining cadmium (Cd), chromium (Cr), nickel (Ni) and lead (Pb) in fertilizers and liming materials. The method uses aqua regia dissolution (nitric + hydrochloric acid extraction) followed by measurement with inductively coupled plasma–atomic emission spectrometry (ICP‑AES). Typical limits of quantification are about 0.3 mg/kg for Cd and ~1 mg/kg for Cr, Ni and Pb, though actual LOQs depend on sample matrix and instrument performance.

Key Topics and Requirements

  • Scope: Quantification of Cd, Cr, Ni, Pb after aqua regia extraction; intended for fertilizers and liming materials.
  • Analytical technique: ICP‑AES with axial or radial viewing; instrument operating conditions (gas flows, RF power, integration time) must be optimized per manufacturer guidance.
  • Extraction: Aqua regia digestion (mixed HNO3 and HCl) following the procedure in the standard to prepare a representative test solution.
  • Calibration & matrix correction:
    • Preferred routine approach: external calibration combined with a single spike recovery to correct for multiplicative matrix effects.
    • Alternatives: standard additions (multiple standards) or matrix‑matched calibration for strong matrix effects, and internal standardization if validated.
  • Limitations: Significant interference occurs from high Cu, Fe or Mn concentrations - no valid results if these micronutrients are present at ≥10% in the fertilizer matrix.
  • Quality control: Use certified stock solutions and regular renewal of standards; follow sampling and sample preparation per referenced norms.

Practical Applications

  • Routine compliance testing of fertilizers and liming materials for heavy metal content under European regulatory frameworks.
  • Quality control in fertilizer manufacturing to monitor Cd, Cr, Ni and Pb levels.
  • Environmental and agronomic laboratories assessing contamination risks or verifying product safety.
  • Regulatory bodies and inspection labs performing batch certification or market surveillance.

Who should use it: analytical chemists, QC managers in fertilizer industry, accredited testing laboratories, and regulatory laboratories requiring a harmonized European method.

Related Standards

  • EN 1482-2 - Sampling and sample preparation for fertilizers and liming materials
  • EN 12944-1 / EN 12944-2 (and EN 12944-3) - Vocabulary for fertilizers and liming materials
  • EN ISO 3696 - Water for analytical laboratory use

Keywords: EN 16319, ICP‑AES, aqua regia, fertilizers, liming materials, cadmium, chromium, lead, nickel, matrix effects, spike recovery, CEN.

Standard

EN 16319:2013+A1:2016

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Frequently Asked Questions

EN 16319:2013+A1:2015 is a standard published by the European Committee for Standardization (CEN). Its full title is "Fertilizers and liming materials - Determination of cadmium, chromium, lead and nickel by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution". This standard covers: This European Standard specifies a method for the determination of the content of cadmium, chromium, nickel and lead in fertilizers with inductively coupled plasma atomic emission spectrometry (ICP-AES) after extraction with aqua regia. 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, Ni and Pb. NOTE Due to significant interference from Cu, Fe and Mn, no valid results can be reported using this method for fertilizer matrices containing high concentrations (>/= 10 %) of these micro-nutrients.

This European Standard specifies a method for the determination of the content of cadmium, chromium, nickel and lead in fertilizers with inductively coupled plasma atomic emission spectrometry (ICP-AES) after extraction with aqua regia. 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, Ni and Pb. NOTE Due to significant interference from Cu, Fe and Mn, no valid results can be reported using this method for fertilizer matrices containing high concentrations (>/= 10 %) of these micro-nutrients.

EN 16319:2013+A1:2015 is classified under the following ICS (International Classification for Standards) categories: 65.080 - Fertilizers. The ICS classification helps identify the subject area and facilitates finding related standards.

EN 16319:2013+A1:2015 has the following relationships with other standards: It is inter standard links to EN 16319:2013, EN 16319:2013/FprA1:2015, prEN 16319. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.

EN 16319:2013+A1:2015 is associated with the following European legislation: Standardization Mandates: M/418. When a standard is cited in the Official Journal of the European Union, products manufactured in conformity with it benefit from a presumption of conformity with the essential requirements of the corresponding EU directive or regulation.

EN 16319:2013+A1:2015 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.

Standards Content (Sample)


2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Düngemittel und Kalkdünger - Bestimmung von Cadmium, Chrom, Blei und Nickel mit Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-AES) nach KönigswasseraufschlussEngrais et amendements minéraux basiques - Détermination du cadmium, chrome, plomb et nickel par spectrométrie d'émission atomique avec plasma induit par haute fréquence (ICP-AES) après digestion à l'eau régaleFertilizers and liming materials - Determination of cadmium, chromium, lead and nickel by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 16319:2013+A1:2015SIST EN 16319:2013+A1:2016en,fr,de01-marec-2016SIST EN 16319:2013+A1:2016SLOVENSKI
STANDARDSIST EN 16319:20131DGRPHãþD

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16319:2013+A1
December
t r s w ICS
x wä r z r Supersedes EN
s x u s {ã t r s uEnglish Version
Fertilizers and liming materials æ Determination of cadmiumá chromiumá lead and nickel by inductively after aqua regia dissolution Engrais et amendements minéraux basiques æ Détermination du cadmiumá chromeá plomb et nickel par spectrométrie d 5émission atomique avec plasma l 5eau régale
This European Standard was approved by CEN on
s w September
t r s u and includes Amendment
s approved by CEN on
y November
t r s wä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey andUnited Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
t r s w CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s x u s {ã t r s u ªA sã t r s w ESIST EN 16319:2013+A1:2016

Results of the inter-laboratory test . 15 A.1 Inter-laboratory tests . 15 A.2 Statistical results for the determination of cadmium, chromium, lead and nickel !for fertilizers" . 15 A.3 Statistical results for the determination of cadmium, chromium, lead and nickel for liming materials . 17 Bibliography . 20
1,18 g/ml. 6.3 Nitric acid, c(HNO3) = 16 mol/l; not less than 65 % volume fraction;
1,42 g/ml. 6.4 Mixed solution of 0,8 mol/l nitric acid and 1,8 mol/l hydrochloric acid. Mix 150 ml of hydrochloric acid (6.2) and 50 ml nitric acid (6.3) to 1,0 l of water (6.1). 6.5 Standard stock solutions, cadmium, chromium, nickel and lead standard stock solutions, e.g.
= 1 000 mg/l for each element. Use suitable stock solutions. Both single-element stock solutions and multi-element stock solutions with adequate specification stating the acid used and the preparation technique are commercially available. It is recommended to use commercially available standard stock solutions for cadmium, chromium, nickel and lead. 6.6 Working standard solutions. Depending on the scope, different working standard solutions may be necessary. In general, when combining elements in working standard solutions, their chemical compatibility shall be regarded. Spectral interferences from other elements present in working standard solutions also need to be considered. Various combinations of elements at different concentrations may be used, provided that the standard stock solutions (6.5) are diluted with the same acid and in equal concentration as the acid in the test solution. NOTE In equal concentrations (in mg/l), cadmium, chromium, nickel and lead are compatible in a multi-element standard solution for the determination by ICP-AES for this application. 6.6.1 Working standard solution I,
= 100 mg/l for cadmium, chromium, nickel and lead. Dilute 10,0 ml of each standard stock solution of cadmium, chromium, nickel and lead (6.5) to 100,0 ml with the mixed acid solution (6.4) in the same 100 ml flask. If non-equal concentrations of cadmium, chromium, nickel and lead are needed, dilute the required volumes into 100,0 ml. This solution is used to prepare spiked test solutions and standard and calibration solutions. 6.6.2 Working standard solution II,
= 10 mg/l for cadmium, chromium, nickel and lead. Dilute 10,0 ml of the working standard solution I of cadmium, chromium, nickel and lead (6.6.1) to 100,0 ml with the mixed acid solution (6.4) in a 100 ml flask. If non-equal concentrations of cadmium, chromium, nickel and lead are needed, dilute the require volume from the standard stock solutions (6.5) into 100,0 ml. This solution is used to prepare spiked test solutions and calibration solutions. 7 Apparatus 7.1 Common laboratory glassware. 7.2 Analytical balance, capable of weighing to an accuracy of 1 mg. 7.3 Inductively coupled plasma-atomic emission spectrometer, with axial or radial viewing of the plasma and with suitable background correction. SIST EN 16319:2013+A1:2016

1) Whatman® 589/2 is an example of a suitable product available commercially. This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of this product. Equivalent products can be used if they can be shown to lead to the same results. SIST EN 16319:2013+A1:2016
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