EN 16319-2013 en Fertilizers - Determination of trace elements - Determination of cadmium chromium lead and nickel by inductively coupled plasma-atomic emission spectrometry (ICP-A.pdf

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1、BSI Standards PublicationBS EN 16319:2013+A1:2015Fertilizers and liming materials Determination of cadmium, chromium, lead and nickel by inductively coupled plasmaatomic emission spectrometry (ICPAES) after aqua regia dissolutionBS EN 16319:2013+A1:2015 BRITISH STANDARDNational forewordThis British

2、Standard is the UK implementation of EN 16319:2013+A1:2015. It supersedes BS EN 16319:2013 which is withdrawn.The start and finish of text introduced or altered by amendment is indicated in the text by tags. Tags indicating changes to CEN text carry the number of the CEN amendment. For example, text

3、 altered by CEN amendment A1 is indicated by .The UK participation in its preparation was entrusted to Technical Committee CII/37, Fertilisers and related chemicals.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to

4、include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2016. Published by BSI Standards Limited 2016ISBN 978 0 580 87901 2ICS 65.080Compliance with a British Standard cannot confer immunity from legal obligations.This

5、British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 October 2013.Amendments/corrigenda issued since publicationDate Text affected29 February 2016 Implementation of CEN amendment A1:2015: Title amendedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NOR

6、M EN 16319:2013+A1 December 2015 ICS 65.080 Supersedes EN 16319:2013English Version Fertilizers and liming materials - Determination of cadmium, chromium, lead and nickel by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution Engrais et amendements minraux

7、basiques - Dtermination du cadmium, chrome, plomb et nickel par spectromtrie dmission atomique avec plasma induit par haute frquence (ICP-AES) aprs digestion leau rgale This European Standard was approved by CEN on 15 September 2013 and includes Amendment 1 approved by CEN on 7 November 2015. CEN me

8、mbers 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 applica

9、tion 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 Manag

10、ement 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

11、, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix

12、17, B-1000 Brussels 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16319:2013+A1:2015 EEN 16319:2013+A1:2015 (E) 2 Contents Page European foreword . 3 1 Scope 4 2 Normative references 4 3 Terms and definitions . 4 4 Principle

13、 . 4 5 Sampling and sample preparation 4 6 Reagents . 4 7 Apparatus . 5 8 Procedure. 6 8.1 General 6 8.2 Preparation of the test solution . 7 8.2.1 General 7 8.2.2 Preparation . 7 8.3 Preparation of the test solution for the correction of matrix effects by spike recovery . 7 8.4 Preparation of the b

14、lank test solution 8 8.5 Preparation of the calibration solutions for the analysis of cadmium, chromium, nickel and lead . 8 8.6 Determination of cadmium, chromium, nickel and lead by ICP-AES 8 8.6.1 General 8 8.6.2 Determination by ICP-AES . 8 9 Calculation and expression of the results . 10 9.1 Ex

15、ternal calibration 10 9.2 Correction for spike recovery 10 9.3 Standard addition method 11 9.4 Calculation of the element content in the sample 11 10 Precision 12 10.1 Inter-laboratory tests . 12 10.2 Repeatability 12 10.3 Reproducibility . 12 11 Test report 13 Annex A (informative) Results of the i

16、nter-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 BS EN 163

17、19:2013+A1:2015EN 16319:2013+A1:2015 (E) 3 European foreword This document (EN 16319:2013+A1:2015) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard,

18、 either by publication of an identical text or by endorsement, at the latest by June 2016, and conflicting national standards shall be withdrawn at the latest by June 2016. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/o

19、r CENELEC shall not be held responsible for identifying any or all such patent rights. This document includes Amendment 1 approved by CEN on 2015-11-07. This document supersedes !EN 16319:2013“. The start and finish of text introduced or altered by amendment is indicated in the text by tags !“. !del

20、eted text“ 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

21、: 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,

22、 Sweden, Switzerland, Turkey and the United Kingdom. BS EN 16319:2013+A1:2015EN 16319:2013+A1:2015 (E) 4 1 Scope !This European Standard specifies a method for the determination of the content of cadmium, chromium, nickel and lead in fertilizers and liming materials using inductively coupled plasma-

23、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, Ni and Pb. !NOTE 1“ Due to significant interference from Cu, Fe and M

24、n, no valid results can be reported using this method for fertilizer matrices containing high concentrations ( 10 %) of these micro-nutrients. !NOTE 2 The term fertilizer is used throughout the body of this European Standard and needs to be taken to include liming materials unless otherwise indicate

25、d.“ 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any a

26、mendments) applies. EN 1482-2, Fertilizers and liming materials Sampling and sample preparation Part 2: Sample preparation EN 12944-1:1999, Fertilizers and liming materials and soil improvers Vocabulary Part 1: General terms EN 12944-2:1999, Fertilizers and liming materials and soil improvers Vocabu

27、lary Part 2: Terms relating to fertilizers !EN 12944-3:2001, Fertilizers and liming materials Vocabulary Part 3: Terms relating to liming materials“ EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696) 3 Terms and definitions !For the purposes of this document,

28、the terms and definitions given in EN 12944-1:1999, EN 12944-2:1999 and EN 12944-3:2001 apply.“ 4 Principle Cadmium, chromium, nickel and lead are extracted from the sample with aqua regia and conventional boiling. The concentrations in the extract are measured by inductively coupled plasmaatomic em

29、ission spectrometry (ICP-AES), with axial or radial viewing. 5 Sampling and sample preparation Sampling is not part of the method specified in this European Standard. A recommended sampling method is given in EN 1482-1. Sample preparation shall be carried out in accordance with EN 1482-2. 6 Reagents

30、 Use only reagents of recognized analytical grade. BS EN 16319:2013+A1:2015EN 16319:2013+A1:2015 (E) 5 Commercially available stock solutions shall be replaced according to the specifications from the supplier or after one year if prepared in the laboratory from available salts. Standard solutions s

31、hall be renewed monthly as a general rule. 6.1 Water, conforming to grade 2 according to EN ISO 3696. 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; 1,42 g/ml. 6.4 Mixed solution of 0,8 mol/l nitric

32、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-el

33、ement 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 so

34、lutions. 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

35、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 lea

36、d 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 wi

37、th 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 so

38、lution 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,

39、 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

40、 plasma-atomic emission spectrometer, with axial or radial viewing of the plasma and with suitable background correction. BS EN 16319:2013+A1:2015EN 16319:2013+A1:2015 (E) 6 The settings of the working conditions (e.g. gas flows, RF or plasma power, sample uptake rate, integration time and number of

41、 replicates) shall be optimized according to the manufacturers 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 opt

42、ics 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 gene

43、ral, 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

44、effects (see 8.1). 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. 7.4 Dilutor. Instrument used for automated volumetric dilutions or other a

45、ppropriate 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. 7.5 Ash-free filter paper, i.e. Whatman 589/21)or equivalent quality. 8 Pro

46、cedure 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 in

47、terferences) 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 ca

48、libration 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 inte

49、rnal 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 wi