1、BSI Standards PublicationBS EN ISO 16967:2015Solid biofuels Determinationof major elements Al, Ca,Fe, Mg, P, K, Si, Na and Ti (ISO16967:2015)BS EN ISO 16967:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO16967:2015. It supersedes BS EN 15290:2011 which
2、is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PTI/17, Solid biofuels.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Use
3、rs are responsible for its correctapplication. The British Standards Institution 2015. Published by BSI StandardsLimited 2015ISBN 978 0 580 81464 8ICS 75.160.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of t
4、heStandards Policy and Strategy Committee on 31 May 2015.Amendments issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 16967 April 2015 ICS 75.160.10 Supersedes EN 15290:2011English Version Solid biofuels - Determination of major elements - Al, Ca, Fe,
5、 Mg, P, K, Si, Na and Ti (ISO 16967:2015) Biocombustibles solides - Dtermination des lments majeurs - Al, Ca, Fe, Mg, P, K, Si, Na et Ti (ISO 16967:2015) Biogene Festbrennstoffe - Bestimmung von Hauptelementen - Al, Ca, Fe, Mg, P, K, Si, Na und Ti (ISO 16967:2015) This European Standard was approved
6、 by CEN on 28 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 national s
7、tandards 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 an
8、d 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, Hunga
9、ry, 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-CENEL
10、EC 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 16967:2015 EBS EN ISO 16967:2015EN ISO 16967:2015 (E) 3 Foreword This document (EN ISO 16967:2015) has been prepared b
11、y Technical Committee ISO/TC 238 “Solid biofuels“ in collaboration with Technical 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 t
12、he latest by October 2015, and conflicting national standards shall be withdrawn at the latest by October 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 o
13、r all such patent rights. This document supersedes EN 15290:2011. 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, Es
14、tonia, 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. Endorsement notice Th
15、e text of ISO 16967:2015 has been approved by CEN as EN ISO 16967:2015 without any modification. BS EN ISO 16967:2015ISO 16967:2015(E) ISO 2015 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope . 12 Normative references 13 Terms and definitions . 14 Symbols and abbreviated terms .
16、 24.1 Symbols . 24.2 Abbreviated terms . 25 Principle 36 Reagents 37 Apparatus . 38 Preparation of the test sample . 49 Procedure. 49.1 Digestion. 49.2 Detection methods . 69.3 Calibration of the apparatus 69.4 Analysis of digests 69.5 Blank test . 610 Calculations 711 Performance characteristics 71
17、2 Test report . 7Annex A (informative) List of conversion factors 9Annex B (informative) Performance data 10Bibliography .13BS EN ISO 16967:2015ISO 16967:2015(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies)
18、. The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non
19、-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are describ
20、ed in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives). Attention is drawn to
21、the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the IS
22、O list of patent declarations received (see www.iso.org/patents). Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as
23、 well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 238, Solid biofuels.iv ISO 2015 All rights reservedBS EN ISO 16967:2015ISO 16967:2
24、015(E)IntroductionThe elements described as major elements of solid biofuels are in fact major elements of the fuel ashes more than of the fuels. The determination of these elements can be used to assess ash behaviour in a thermal conversion process or to assess utilization of ashes. Moreover, fuel
25、contamination or process additives are indicated by high values of certain elements. Contamination of fuel with sand or soil is indicated by high values of several elements.In this International Standard, wet chemical methods are described. ISO 2015 All rights reserved vBS EN ISO 16967:2015BS EN ISO
26、 16967:2015Solid biofuels Determination of major elements Al, Ca, Fe, Mg, P, K, Si, Na and Ti1 ScopeThis International Standard describes methods for the determination of major elements of solid biofuels respectively of their ashes, which are Al, Ca, Fe, Mg, P, K, Si, Na, Ti. The determination of ot
27、her elements such as barium (Ba) and manganese (Mn) is also possible with the methods described in this International Standard.This International Standard includes two parts: Part A describes the direct determination on the fuel, this method is also applicable for sulfur and minor elements, Part B g
28、ives a method of determination on a prepared 550 C ash.2 Normative referencesThe 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 e
29、dition of the referenced document (including any amendments) applies.ISO 7980, Water quality Determination of calcium and magnesium Atomic absorption spectrometric methodISO 9964-1, Water quality Determination of sodium and potassium Part 1: Determination of sodium by atomic absorption spectrometryI
30、SO 9964-2, Water quality Determination of sodium and potassium Part 2: Determination of potassium by atomic absorption spectrometryISO 9964-3, Water quality Determination of sodium and potassium Part 3: Determination of sodium and potassium by flame emission spectrometryISO 11885, Water quality Dete
31、rmination of selected elements by inductively coupled plasma optical emission spectrometry (ICP-OES)EN 147801), Solid Biofuels Sample preparationISO 16559, Solid biofuels Terminology, definitions and descriptionsISO 16993, Solid biofuels Conversion of analytical results from one basis to anotherISO
32、17294-2, Water quality Application of inductively coupled plasma mass spectrometry (ICP-MS) Part 2: Determination of 62 elementsISO 181222), Solid biofuels Determination of ash contentISO 18134-32), Solid biofuels Determination of moisture content Oven dry method Part 3: Moisture in general analysis
33、 sample3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 16559 and the following apply.1) To be replaced by ISO 14780.2) To be published.INTERNATIONAL STANDARD ISO 16967:2015(E) ISO 2015 All rights reserved 1BS EN ISO 16967:2015ISO 16967:2015(E)3.1refer
34、ence materialRMmaterial or substance one or more of whose property values are sufficiently homogeneous and well established to be used for the calibration of an apparatus, the assessment of a measurement method, or for assigning values to materials3.2certified reference materialCRMreference material
35、, accompanied by a certificate, one or more of whose property values are certified by a procedure which 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 level of
36、 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 use(s)
37、of the material4 Symbols and abbreviated terms4.1 SymbolsAl AluminiumCa CalciumFe IronMg MagnesiumP PhosphorusK PotassiumSi SiliconNa SodiumTi Titanium4.2 Abbreviated termsCRM Certified Reference MaterialICP-OES Inductively Coupled Plasma Optical Emission SpectrometryICP-MS Inductively Coupled Plasm
38、a Mass SpectrometryFAAS Flame Atomic Absorption SpectrometryFES Flame Emission SpectrometrySRM Standard Reference Material2 ISO 2015 All rights reservedBS EN ISO 16967:2015ISO 16967:2015(E)NBS National Bureau of StandardsNIST The National Institute of Standards and Technology (NIST), known between 1
39、901 and 1988 as the National Bureau of Standards (NBS), is a measurement standards laboratory, also known as a National Metrological Institute (NMI), which is a non-regulatory agency of the United States Department of Commerce.5 PrincipleThe sample is digested in a closed vessel by the help of reage
40、nts, temperature, and pressure. The digestion is either carried out directly on the fuel (part A) or on a 550 C prepared ash (part B).The detection of the elements can be done by ICP-OES, ICP-MS, FAAS, or FES.6 ReagentsAll reagents should be of analytical grade or better. If minor elements are also
41、to be determined, the best qualities should be used.6.1 Water, containing negligible amounts of major elements, i.e. amounts that do not contribute significantly to the determinations. Deionised water will normally fulfil this requirement.6.2 Nitric acid (HNO3), 65 % (w/w), = 1,41 g/ml.6.3 Hydrogen
42、peroxide (H2O2), 30 % (w/w), = 1,11 g/ml.6.4 Hydrofluoric acid (HF), 40 % (w/w), = 1,13 g/ml.CAUTION Hydrofluoric acid might lead to health hazards.6.5 Boric acid (H3BO3), 4 % (w/w).6.6 Use of certified reference materials (CRM or SRM).Use certified reference materials, issued by an internationally
43、recognized authority, to check if the accuracy of the calibration meets the required performance characteristics. Examples of certified reference materials are: NBS 1570 spinach leaves, NBS1571 orchard leaves, NBS 1573 tomato leaves, and NBS 1575 pine needles.When, due to matrix effects or concentra
44、tion range limitations, no good recoveries for the certified reference materials can be obtained, calibration with at least two CRM or SRM materials can 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
45、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, institute quality control, determine performance characteristics, or measure a property at the state-of-the-art limit; and (3
46、) to ensure the long-term adequacy and integrity of measurement quality assurance programs.7 Apparatus7.1 Heating oven or heating block suitable for the decomposition system in use, resistance heated oven or heating block that can be used at a temperature of at least 220 C with an accuracy of 10 C.7
47、.2 Microwave oven, intended for laboratory use and equipped with temperature control. ISO 2015 All rights reserved 3BS EN ISO 16967:2015ISO 16967:2015(E)7.3 Sample digestion vessels, intended for the heating system used, normally made of a fluoro plastic.7.4 Balance.7.4.1 Part A, balance with a reso
48、lution of at least 1 mg.7.4.2 Part B, balance with a resolution of at least 0,1 mg.7.5 Plastic volumetric flasks.8 Preparation of the test sampleThe test sample is the general analysis test sample with a nominal top size of 1 mm or less, prepared in accordance with EN 147803).The moisture content of
49、 the test sample shall be determined as described in ISO 18134-3.9 Procedure9.1 Digestion9.1.1 Part A: Direct determination on the fuelThe decomposition shall be carried out in closed vessels. It can be done in a heating oven, a heating block or in a microwave oven. Mix 500 mg of ground and homogenized sample, weighed to the nearest 1 mg, with 3,0 ml H2O2(30 %), 8,0 ml HNO3(65 %), and 1,0 ml HF (40 %) in a closed digestion vessel. A reaction time of minimum 5 min shall be kept before closing the v
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