DIN EN 16317-2017 Fertilizers and liming materials - Determination of arsenic by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution Germ.pdf

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1、May 2017 English price group 11No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 65.080!%e)p“2660677www.din.deDIN EN

2、16317Fertilizers and liming materials Determination of arsenic by inductively coupled plasmaatomic emission spectrometry (ICPAES) after aqua regia dissolution;English version EN 16317:2013+A1:2017,English translation of DIN EN 16317:2017-05Dngemittel und Kalkdnger Bestimmung von Arsen mit Atomemissi

3、onsspektrometrie mit induktiv gekoppeltem Plasma (ICPAES) nach Knigswasseraufschluss;Englische Fassung EN 16317:2013+A1:2017,Englische bersetzung von DIN EN 16317:2017-05Engrais et amendements minraux basiques Dtermination de larsenic par spectromtrie dmission atomique avec plasma induit par haute f

4、rquence (ICPAES) aprs digestion leau rgale;Version anglaise EN 16317:2013+A1:2017,Traduction anglaise de DIN EN 16317:2017-05SupersedesDIN EN 16317:201312www.beuth.deDocument comprises 17 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered autho

5、ritative.05.17DIN EN 16317:2017-05 2 A comma is used as the decimal marker. National foreword This document (EN 16317:2013+A1:2017) has been prepared by Technical Committee CEN/TC 260 “Fertilizers and liming materials” (Secretariat: DIN, Germany). The responsible German body involved in its preparat

6、ion was DIN-Normenausschuss Lebensmittel und landwirtschaftliche Produkte (DIN Standards Committee Food and Agricultural Products), Working Committee NA 057-03-02 AA “Fertilizers”. The DIN Standard corresponding to the International Standard referred to in this document is as follows: ISO 5725-1 DIN

7、 ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 Amendments This standard differs from DIN EN 16317:2013-12 as follows: a) the title and scope have been extended to include liming materials; b) Clause 10 “Precision” has been extended to include liming materials; c) statistics of the interlaboratory test for li

8、ming materials have been included in Annex A; d) the standard has been revised and brought in line with the current rules of presentation. Previous editions DIN CEN/TS 16317 (DIN SPEC 10787): 2012-06 DIN EN 16317: 2013-12 National Annex NA (informative) Bibliography DIN ISO 5725-1, Accuracy (truenes

9、s and precision) of measurement methods and results Part 1: General principles and definitions DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method EUROPEA

10、N STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16317:2013+A1 February 2017 ICS 65.080 English Version Fertilizers and liming materials - Determination of arsenic by inductively coupled plasma-atomic emission spectrometry (ICP-AES) after aqua regia dissolution Engrais et amendements minraux basiques -

11、 Dtermination de larsenic par spectromtrie dmission atomique avec plasma induit par haute frquence (ICP-AES) aprs digestion leau rgale Dngemittel und Kalkdnger - Bestimmung von Arsen mit Atomemissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-AES) nach Knigswasseraufschluss This European Sta

12、ndard was approved by CEN on 29 August 2013 and includes Amendment 1 approved by CEN on 11 December 2016. 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 alteratio

13、n. 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

14、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, F

15、inland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR ST

16、ANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2017 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16317:2013+A1:2017 E2 Contents Page E

17、uropean foreword . 3 1 Scope 4 2 Normative references 4 3 Terms and definitions . 4 4 Principle . 4 5 Sampling and sample preparation 4 6 Reagents . 5 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 te

18、st solution for the correction of matrix effects by spike recovery . 7 8.4 Preparation of the blank test solution 8 8.5 Preparation of the calibration solutions for the analysis of arsenic 8 8.6 Determination of arsenic by ICP-AES . 8 8.6.1 General 8 8.6.2 Determination by ICP-AES . 8 9 Calculation

19、and expression of the results 9 9.1 External calibration . 9 9.2 Correction for spike recovery 10 9.3 Standard addition method 10 9.4 Calculation of the element content in the sample 11 10 Precision 11 10.1 Inter laboratory tests 11 10.2 Repeatability 11 10.3 Reproducibility . 11 11 Test report 12 A

20、nnex A (informative) 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 . 15 EN 16317:2013+A1:2017 (E)DIN EN 16317:2017-05 3 European foreword This document (EN 16317:2013+A1:2017) has been pre

21、pared 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, either by publication of an identical text or by endorsement, at the latest by August 2017, and conflicting na

22、tional standards shall be withdrawn at the latest by August 2017. This document includes Amendment 1 approved by CEN on 11 December 2016. This document supersedes !EN 16317:2013“. The start and finish of text introduced or altered by amendment is indicated in the text by tags ! “. Attention is drawn

23、 to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document has been prepared under a mandate given to CEN by the European Commission and the European

24、 Free Trade Association. According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic

25、of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. EN 16317:2013+A1:2017 (E)DIN EN 16317:2017-05 4 1 Scop

26、e !This European Standard specifies a method for the determination of the content of arsenic 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

27、as on the instrument, but can roughly be expected to be 1,5 mg/kg for As. !NOTE The term fertilizer is used throughout the body of this European Standard and includes liming materials unless otherwise indicated.“ 2 Normative references The following documents, in whole or in part, are normatively re

28、ferenced 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 amendments) applies. EN 1482-2, Fertilizers and liming materials - Sampling and sample prepa

29、ration - 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 - Vocabulary - Part 2: Terms relating to fertilizers !EN 12944-3:2001, Fertilizers and li

30、ming materials and soil improvers 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, the terms and definitions given in EN 12944-1:1999, EN 1294

31、4-2:1999 !and EN 12944-3:2001“apply. 4 Principle Arsenic is extracted from the sample with aqua regia and conventional boiling. The concentration in the extract is measured by inductively coupled plasmaatomic emission spectrometry (ICP-AES) with axial or radial viewing. 5 Sampling and sample prepara

32、tion Sampling is not part of the methods 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. EN 16317:2013+A1:2017 (E)DIN EN 16317:2017-05 5 6 Reagents Use only reagents of recognized analytic

33、al grade. 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 shall be renewed monthly as a general rule. 6.1 Water, according to EN ISO 3696, grade 2. 6.2

34、Hydrochloric acid, c(HCl) = 12 mol/l; 37 % volume fraction; approximately 1,18 g/ml. 6.3 Nitric acid, c(HNO3) = 16 mol/l; not less than 65 % volume fraction, approximately 1,42 g/ml. 6.4 Mixed acid solution of 0,8 mol/l nitric acid and 1,8 mol/l hydrochloric acid. Mix 150 ml of hydrochloric acid (6.

35、2) and 50 ml nitric acid (6.3) to 1,0 l of water (6.1). 6.5 Standard stock solution arsenic standard stock solution, e.g. = 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 commerci

36、ally 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

37、 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 solutio

38、n 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 pla

39、sma-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 optimized according to the manufactur

40、ers 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”

41、(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 EN 16317:2013+A

42、1:2017 (E)DIN EN 16317:2017-05 6 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 interna

43、l 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 appropriate equipment (e.g. pipettes and

44、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 Procedure 8.1 General Calibrations by stan

45、dard 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

46、 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

47、, 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 op

48、tion, 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

49、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 easily imitated synthetically. 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 th