EN 16319:2013

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Düngemittel - Bestimmung von Elementspuren - Bestimmung von Cadmium, Chrom, Blei und Nickel mit Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-AES) nach KönigswasseraufschlussEngrais - Dosage des éléments traces - Détermination du cadmium, chromium, plomb et nickel 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 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 16319:2013SIST EN 16319:2013en,fr,de01-december-2013SIST EN 16319:2013SLOVENSKI
STANDARDSIST-TS CEN/TS 16319:20121DGRPHãþD

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16319
October 2013 ICS 65.080 Supersedes CEN/TS 16319:2012English Version
Fertilizers - Determination of trace elements - Determination of cadmium, chromium, lead and nickel by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution
Engrais - Dosage des éléments trace - 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
Düngemittel - Bestimmung von Elementspuren - Bestimmung von Cadmium, Chrom, Blei und Nickel mit Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-AES) nach Königswasseraufschluss This European Standard was approved by CEN on 15 September 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
CEN-CENELEC 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 16319:2013: ESIST EN 16319:2013

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 . 15 Bibliography . 17
 the document has been editorially revised. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: 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 the United Kingdom.
≈ 1,18 g/ml. 6.3 Nitric acid, c(HNO3) = 16 mol/l; not less than 65 % volume fraction;
≈ 1,42 g/ml. SIST EN 16319:2013

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. The settings of the working conditions (e.g. gas flows, RF or plasma power, sample uptake rate, integration time and number of replicates) shall be optimized according to the manufacturer’s instructions. Radial viewing of the plasma may be used if it can be shown that the limits of quantification for cadmium, chromium, nickel and lead are 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).
7.5 Ash-free filter paper, i.e. Whatman® 589/21) or equivalent quality. 8 Procedure 8.1 General Calibrations by standard additions with several standards or by matrix matching are very powerful calibration techniques and can be used to accurately correct for matrix effects from easy-ionisable elements (multiplicative matrix effects). Additive matrix effects (i.e. spectral interferences) are not corrected for with standard additions calibration. For matrix matching, additive matrix effects will be corrected for when the added matrix is the cause of the matrix effect. The main drawback of calibration by standard addition with several standards is the requirement for a calibration function for each sample type, which is a time consuming process. For matrix matching a profound knowledge of the sample matrix is needed, which is not always necessarily available. These two techniques may thus not be practical to use in routine fertilizer laboratories. Correction by internal standardization 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. It is therefore suggested that calibrations are to be performed by means of external calibration and correction of matrix effects by addition of one known spike of a standard solution (spike recovery). The method of external calibration and correction for spike recovery allows for the analysis of fertilizers with unknown matrix composition or with a matrix that cannot be synthetically imitated easily. This calibration technique may not be as precise as calibration by standard additions with several standards but the increased uncertainty is small compared to the total uncertainty of the method, if the total analyte concentration is in the linear working range after the spike and the added spike corresponds to at least a doubling of the analyte concentration. Many matrix errors can be compensated for by this procedure, if they are not additive (e.g. spectral interferences). Aliquots of the sample solution are analyzed by the means of external calibration and then one aliquot is spiked with known concentrations of the analytes without changing the matrix of the s
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