EN 16317:2013

Fertilizers - Determination of trace elements - Determination of arsenic 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 arsenic in fertilizers 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 1,5 mg/kg for As.

Düngemittel - Bestimmung von Elementspuren - Bestimmung von Arsen mit Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-AES) nach Königswasseraufschluss

Diese Europäische Norm legt ein Verfahren zur Bestimmung von Arsen in Düngemitteln mittels Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-AES) nach Königswasseraufschluss fest. Die Bestimmungsgrenzen sind sowohl von der Probenmatrix als auch vom eingesetzten Gerät abhängig, werden jedoch für Arsen bei etwa 1,5 mg/kg erwartet.

Engrais - Dosage des éléments trace - Détermination de l'arsenic par spectrométrie d'émission atomique avec plasma induit par haute fréquence (ICP-AES) après digestion à l'eau régale

Cette norme européenne spécifie une méthode permettant de déterminer la teneur en arsenic dans les engrais par spectrométrie d’émission atomique avec plasma à couplage inductif (ICP-AES) après dissolution dans l’eau régale. Les limites de quantification dépendent de la matrice de l’échantillon ainsi que de l’instrument, mais devraient se situer autour de 1,5 mg/kg pour l’As.

Gnojila - Določevanje elementov v sledovih - Določevanje arzena z atomsko emisijsko spektrometrijo z induktivno sklopljeno plazmo (ICP-AES) po raztapljanju v zlatotopki

Ta evropski standard določa metodo za določevanje vsebnosti arzena v gnojilih z atomsko emisijsko spektrometrijo z induktivno sklopljeno plazmo (ICP-AES) po raztapljanju v zlatotopki. Meje kvantifikacije so odvisne od matrice vzorca in instrumenta, vendar so za As običajno približno 1,5 mg/kg.

General Information

• Status: Withdrawn
• Publication Date: 01-Oct-2013
• Withdrawal Date: 21-Feb-2017
• ICS: 65.080 - Fertilizers
• Technical Committee: CEN/TC 260 - Fertilizers and liming materials
• Drafting Committee: CEN/TC 260/WG 7 - Chemical analysis
• Current Stage: 9960 - Withdrawal effective - Withdrawal
• Completion Date: 22-Feb-2017
• Directive: 2003/2003 - Regulation (EC) N° 2003/2003 of the European Parlament and of the council of 13 October 2003 relating to fertilisers
• 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/418 - Standardization mandate M/335 assigned to CEN concerning the modernisation of the methods of analysis of fertilizers
• Ref Project: SIST EN 16317:2013 - Fertilizers - Determination of trace elements - Determination of arsenic by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution

Relations

• Replaces: CEN/TS 16317:2012 - Fertilizers - Determination of trace elements - Determination of arsenic by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution
• Effective Date: 09-Oct-2013
• Merged Into: EN 16317:2013+A1:2017 - Fertilizers and liming materials - Determination of arsenic by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution
• Effective Date: 18-Jan-2023
• Amended By: EN 16317:2013/FprA1:2016 - Fertilizers and liming materials - Determination of arsenic by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution
• Effective Date: 18-Sep-2013

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Düngemittel - Bestimmung von Elementspuren - Bestimmung von Arsen mit Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-AES) nach KönigswasseraufschlussEngrais - Dosage des éléments traces - Détermination de l'arsenic par spectrométrie d'émission atomique avec plasma induit par haute fréquence (ICP-AES) après digestion à
l'eau régaleFertilizers - Determination of trace elements - Determination of arsenic by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution65.080GnojilaFertilizersICS:Ta slovenski standard je istoveten z:EN 16317:2013SIST EN 16317:2013en,fr,de01-december-2013SIST EN 16317:2013SLOVENSKI
STANDARDSIST-TS CEN/TS 16317:20121DGRPHãþD

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16317
October 2013 ICS 65.080 Supersedes CEN/TS 16317:2012English Version
Fertilizers - Determination of trace elements - Determination of arsenic by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution
Engrais - Dosage des éléments traces - Détermination de l'arsenic par spectrométrie d'émission atomique avec plasma induit par haute fréquence (ICP-AES) après digestion à
l'eau régale
Düngemittel - Bestimmung von Elementspuren - Bestimmung von Arsen mit Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-AES) nach Königswasseraufschluss This European Standard was approved by CEN on 29 August 2013.
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. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member.
This European Standard exists 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2013 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16317:2013: ESIST EN 16317:2013

Results of the inter-laboratory test . 13 A.1 Inter-laboratory tests . 13 A.2 Statistical results for the determination of arsenic by ICP-AES . 13 Bibliography. 14
6.1 Water, according to EN ISO 3696, grade 2. 6.2 Hydrochloric acid, c(HCl) = 12 mol/l; 37 % volume fraction;
≈ 1,18 g/ml. 6.3 Nitric acid, c(HNO3) = 16 mol/l; not less than 65 % volume fraction, ρ ≈ 1,42 g/ml. SIST EN 16317:2013

= 1 000 mg/l in arsenic. Use suitable stock solutions. Single-element stock solutions with adequate specification stating the acid used and the preparation technique are commercially available. It is recommended to use a commercially available standard stock solution for arsenic. 6.6 Working standard solutions. Depending on the scope, different working standard solutions may be necessary. 6.6.1 Working standard solution I,
= 100 mg/l for arsenic.
Dilute 10,0 ml of the stock solution of arsenic (6.5) to 100,0 ml with the mixed acid solution (6.4) in the same 100 ml flask. 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 arsenic. Dilute 10,0 ml of the working standard solution I (6.6.1) to 100,0 ml with the mixed acid solution (6.4) in a 100 ml flask. 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. The settings of the working conditions (e.g. gas flows, RF or plasma power, sample uptake rate, integration time, number of replicates) shall be optimised according to the manufacturer’s instructions. Radial viewing of the plasma may be used if it can be shown that the limit of quantification for arsenic is below the required legal limit values. The use of axial orientation of the viewing optics requires good control of the matrix effects coming from "easily ionisable elements" (i.e. the influence of easily ionisable elements in varying concentrations on the signal intensities of the analytes). For alkali-elements, this can be achieved by adding caesium-chloride solution (CsCl). In general, matrix matching of calibration solutions or calibration by standard additions with several calibration standards will correct accurately for these matrix effects. Spike recovery of one known standard combined with external calibration can, if used properly, also correct sufficiently for matrix effects (see 8.1). Correction by internal standardisation is also a good option, but the accuracy of the measurements after internal standard correction should be validated properly prior to use on unknown fertilizer samples. 7.4 Dilutor. Instrument used for automated volumetric dilutions or other appropriate equipment (e.g. pipettes and volumetric glassware) to perform dilutions. The precision and accuracy of this type of equipment for volumetric dilutions shall be established, and controlled and documented regularly.
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