1、September 2015 Translation by DIN-Sprachendienst.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).
2、ICS 75.160.10!%F0%“2351302www.din.deDDIN EN ISO 16968Solid biofuels Determination of minor elements (ISO 16968:2015);English version EN ISO 16968:2015,English translation of DIN EN ISO 16968:2015-09Biogene Festbrennstoffe Bestimmung von Spurenelementen (ISO 16968:2015);Englische Fassung EN ISO 16968
3、:2015,Englische bersetzung von DIN EN ISO 16968:2015-09Biocombustibles solides Dtermination des lments mineurs (ISO 16968:2015);Version anglaise EN ISO 16968:2015,Traduction anglaise de DIN EN ISO 16968:2015-09SupersedesDIN EN 15297:2011-04www.beuth.deDocument comprises 19 pagesIn case of doubt, the
4、 German-language original shall be considered authoritative.08.15 DIN EN ISO 16968:2015-09 2 A comma is used as the decimal marker. National foreword This document (EN ISO 16968:2015) has been prepared by Technical Committee ISO/TC 238 “Solid biofuels” in collaboration with Technical Committee CEN/T
5、C 335 “Solid biofuels” (Secretariat: SIS, Sweden). The responsible German body involved in its preparation was the DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-05-82 AA Biogene Festbrennstoffe. The DIN Standards corresponding to the Interna
6、tional Standards referred to in this document are as follows: ISO 5725-2 DIN ISO 5725-2 ISO 11885 DIN EN ISO 11885 ISO 16559 DIN EN ISO 16559 ISO 16993 DIN EN ISO 16993 ISO 17225-1 DIN EN ISO 17225-1 ISO 17294-2 DIN EN ISO 17294-2 ISO 18134-3 E DIN EN ISO 18134-3 ISO/TS 21748 see NOTE 2 NOTE ISO 181
7、34-3 is still in preparation and the final version has not yet been published. Please note that the title of the final version of this document might be different from that of the draft version. NOTE 2 There is no DIN Standard available which corresponds to ISO/TS 21748:2004, but TS 2010 has been in
8、corporated in ISO 21748, which has been adopted at national level as DIN ISO 21748. Amendments This standard differs from DIN EN 15297:2011-04 as follows: a) the content of DIN EN 15297:2011-04 has been largely adopted and partially revised to be in line with International Standards; b) the German t
9、ranslation of “solid biofuels” has been changed throughout the document from Feste Biobrennstoffe to Biogene Festbrennstoffe; c) the standard has been editorially revised. Previous editions DIN CEN/TS 15297: 2006-06 DIN EN 15297: 2011-04 DIN EN ISO 16968:2015-09 3 National Annex NA (informative) Bib
10、liography DIN EN ISO 11885, Water quality Determination of selected elements by inductively coupled plasma optical emission spectrometry (ICP-OES) DIN EN ISO 16559, Solid biofuels Terminology, definitions and description DIN EN ISO 16993, Solid biofuels Conversion of analytical results from one basi
11、s to another DIN EN ISO 17225-1, Solid biofuels Fuel specifications and classes Part 1: General requirements DIN EN ISO 17294-2, Water quality Application of inductively coupled plasma mass spectrometry (ICP-MS) Part 2: Determination of 62 elements E DIN EN ISO 18134-3, Solid biofuels Determination
12、of moisture content Oven dry method Part 3: Moisture in general analysis sample1)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 DIN ISO 21748, Guidan
13、ce for the use of repeatability, reproducibility and trueness estimates in measurement uncertainty estimation 1) The final version is due to be published in October 2015. DIN EN ISO 16968:2015-09 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 16968 May 20
14、15 ICS 75.160.10 Supersedes EN 15297:2011English Version Solid biofuels - Determination of minor elements(ISO 16968:2015) Biocombustibles solides - Dtermination des lments mineurs (ISO 16968:2015) Biogene Festbrennstoffe - Bestimmung von Spurenelementen (ISO 16968:2015) This European Standard was ap
15、proved by CEN on 14 February 2015. 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 nati
16、onal 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 langu
17、age 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,
18、 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 COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN
19、-CENELEC Management Centre: Avenue Marnix 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 ISO 16968:2015 EForeword 3Introduction 41 Scope . 52 Normative references 53 Terms and definitions . 54 Symbols and
20、abbreviated terms . 64.1 Symbols . 64.2 Abbreviated terms . 65 Principle 76 Reagents 77 Apparatus . 88 Preparation of the test sample . 89 Procedure. 89.1 Digestion. 89.2 Detection methods . 99.3 Calibration of the apparatus 99.4 Analysis of the digests 99.5 Blank test . 910 Calculations. 1011 Perfo
21、rmance characteristics . 1012 Test report 10Annex A (informative) Performance data 11Bibliography .15Contents PageDIN EN ISO 16968:2015-09 EN ISO 16968:2015 (E) 2 Foreword This document (EN ISO 16968:2015) has been prepared by Technical Committee ISO/TC 238 “Solid biofuels” in collaboration with Tec
22、hnical Committee CEN/TC 335 “Solid biofuels” the secretariat of which is held by SIS. 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 November 2015, and conflicting national standards shall be wit
23、hdrawn at the latest by November 2015. Attention is drawn 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 supersedes EN 15297:2011. This do
24、cument has been prepared under a mandate given to CENELEC 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, Bel
25、gium, 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, Switz
26、erland, Turkey and the United Kingdom. Endorsement notice The text of ISO 16968:2015 has been approved by CEN as EN ISO 16968:2015 without any modification. DIN EN ISO 16968:2015-09 EN ISO 16968:2015 (E) 3 IntroductionThe minor elements present in solid biofuels can, in some cases, be of environment
27、al concern, e.g. it has been shown that certain energy crops will concentrate cadmium and, in polluted areas, other toxic elements may be found at elevated concentrations in the biofuels. This can be a problem if, for example, the ash from the combustion is to be put back in the forest as a fertiliz
28、er. Trace elements in biofuels are often present at very low concentrations requiring great care to avoid contamination in the sample preparation and decomposition steps. The typical concentrations of minor elements in solid biofuels can be found in ISO 17225-1. In this International Standard, wet c
29、hemical methods are described. Alternative methods such as X-ray fluorescence (XRF) or direct mercury analysers may be used when validated with suitable materials (biomass reference materials).DIN EN ISO 16968:2015-09 EN ISO 16968:2015 (E) 4 1 ScopeThis International Standard is intended for the det
30、ermination of the minor elements Arsenic, Cadmium, Cobalt, Chromium, Copper, Mercury, Manganese, Molybdenum, Nickel, Lead, Antimony, Vanadium, and Zinc in all solid biofuels. Further, it describes methods for sample decomposition and suggests suitable instrumental methods for the determination of th
31、e elements of interest in the digests. The determination of other elements such as Selenium, Tin, and Thallium is also possible with the method described in this International Standard.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and
32、 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.ISO 11885, Water quality Determination of selected elements by inductively coupled plasma optical emi
33、ssion spectrometry (ICP-OES)ISO 16559, Solid biofuels Terminology, definitions and descriptionsISO 16993, Solid biofuels Conversion of analytical results from one basis to anotherISO 17294-2, Water quality Application of inductively coupled plasma mass spectrometry (ICP-MS) Part 2: Determination of
34、62 elementsISO 17378-2:2014, Water quality Determination of arsenic and antimony Part 2: Method using hydride generation atomic absorption spectrometry (HG-AAS)ISO 18134-31), Solid biofuels Determination of moisture content Oven dry method Part 3: Moisture in general analysis simpleEN 14780, Solid B
35、iofuels Sample preparationEN 12338, Water quality Determination of mercury Enrichment methods by amalgamation3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 16559 and the following apply.3.1reference materialRMone or more material or substance of whic
36、h property values are sufficiently homogeneous and well established to be used for the calibration of an apparatus, assessment of a measurement method, or assignment of values to materials1) To be published.DIN EN ISO 16968:2015-09 EN ISO 16968:2015 (E) 5 3.2certified reference materialCRMreference
37、material, accompanied by a certificate, one or more of which property values are certified by a procedure that establishes traceability to an accurate realisation of the unit in which the property values are expressed, and for which each certified value is accompanied by an uncertainty at a stated l
38、evel of confidence3.3NIST standard reference materialSRMCRM issued by NIST that also meets additional NIST-specific certification criteria and is issued with a certificate or certificate of analysis that reports the results of its characterisations and provides information regarding the appropriate
39、use(s) of the material4 Symbols and abbreviated terms4.1 SymbolsAs ArsenicCd CadmiumCo CobaltCr ChromiumCu CopperHg MercuryMn ManganeseMo MolybdenumNi NickelPb LeadSb AntimonyV VanadiumZn Zinc4.2 Abbreviated termsCV-AAS Cold vapour atomic absorption spectrometryGF-AAS Graphite furnace atomic absorpt
40、ion spectrometryHG-AAS Hydride generation atomic absorption spectrometryICP-OES Inductively coupled plasma optical emission spectrometryDIN EN ISO 16968:2015-09 EN ISO 16968:2015 (E) 6 ICP-MS Inductively coupled plasma mass spectrometryNBS National Bureau of StandardsNIST National Institute of Stand
41、ards and TechnologyaaKnown between 1901 and 1988 as the National Bureau of Standards (NBS), is a measurement standards laboratory, also known as National Metrological Institute (NMI), which is a non-regulatory agency of the United States Department of Commerce.5 PrincipleThe analysis sample is diges
42、ted in a closed vessel made from a fluoropolymer using nitric acid, hydrogen peroxide, and hydrofluoric acid in a microwave oven or a resistance oven or heating block. The digest is then diluted and the elements are determined with suitable instruments.6 ReagentsAll reagents shall be of analytical g
43、rade or better. If the blank level is unacceptably high, i.e. more than 30 % of the determined value, the use of ultra-pure reagents should be investigated.6.1 Water, containing negligible amount of the minor elements, i.e. amount that do not contribute significantly to the determinations. NOTE 1 De
44、ionised water or doubly distilled water normally fulfils this requirement.NOTE 2 The water used for analytical trace metal work is normally produced using a system for production of ultra-pure water for laboratory use conductivity = 0,056 S/cm.6.2 Hydrofluoric acid (HF), 40 % (w/w), = 1,13 g/ml.CAUT
45、ION Hydrofluoric acid may lead to health hazards.6.3 Hydrogen peroxide (H2O2), 30 % (w/w), = 1,11 g/ml.6.4 Nitric acid (HNO3), 65 % (w/w), = 1,41 g/ml.6.5 Boric acid (H3BO3), 4 % (w/w).6.6 Certified Reference Materials (CRM or SRM), issued by an internationally recognized authority, to check if the
46、accuracy of the calibration meets the required performance characteristics.EXAMPLE NBS 1570 spinach leaves, NBS1571 orchard leaves, NBS 1573 tomato leaves, and NBS 1575 pine needles.When no good recoveries for the certified reference materials can be obtained, due to matrix effects or concentration
47、range limitations, calibration with at least two CRM or SRM materials may solve these problems. In that case, CRM or SRM materials other than used for the calibration shall be used for verification purposes.NOTE A CRM or SRM is prepared and used for three main purposes: (1) to help develop accurate methods of analysis; (2) to calibrate measurement systems used to facilitate exchange of goods,
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