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1、DRAFT FOR DEVELOPMENT DD CEN/TS 15290:2006 Solid Biofuels Determination of major elements ICS 75.160.10 ? Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:43:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI DD CEN/TS 15290:2006 This Draft for Development was publ
2、ished under the authority of the Standards Policy and Strategy Committee on 28 April 2006 BSI 2006 ISBN 0 580 48224 3 National foreword This Draft for Development is the official English language version of CEN/TS 15290:2006. This publication is not to be regarded as a British Standard. It is being
3、issued in the Draft for Development series of publications and is of a provisional nature because the Technical Committee needs some time to collect the data in this relatively new area of technology. It should be applied on this provisional basis, so that information and experience of its practical
4、 application may be obtained. Comments arising from the use of this Draft for Development are requested so that UK experience can be reported to the European organization responsible for its conversion to a European standard. A review of this publication will be initiated 2 years after its publicati
5、on by the European organization so that a decision can be taken on its status at the end of its 3-year life. Notification of the start of the review period will be made in an announcement in the appropriate issue of Update Standards. According to the replies received by the end of the review period,
6、 the responsible BSI Committee will decide whether to support the conversion into a European Standard, to extend the life of the Technical Specification or to withdraw it. Comments should be sent in writing to the Secretary of BSI Technical Committee PTI/17, Solid biofuels, at British Standards Hous
7、e, 389 Chiswick High Road, London W4 4AL, giving the document reference and clause number and proposing, where possible, an appropriate revision of the text. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards whic
8、h implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publicat
9、ion does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Summary of pages This document comprises a front cover, an inside front cover, the CEN/TS title page, pages 2 to 12, an inside back cover and a back cover. The BSI copyright
10、 notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:43:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI TECHNICAL SPECIFICATION
11、SPCIFICATION TECHNIQUE TECHNISCHE SPEZIFIKATION CEN/TS 15290 March 2006 ICS 75.160.10 English Version Solid Biofuels - Determination of major elements Biocombustibles solides - Dtermination des lments mineurs Feste Biobrennstoffe - Bestimmung von Hauptelementen This Technical Specification (CEN/TS)
12、was approved by CEN on 22 November 2005 for provisional application. The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their comments, particularly on the question whether the CEN/TS can be converted into a Europ
13、ean Standard. CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS) until the fin
14、al decision about the possible conversion of the CEN/TS into an EN is reached. CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Nether
15、lands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2006 CENAll rights of exploitation
16、in any form and by any means reserved worldwide for CEN national Members. Ref. No. CEN/TS 15290:2006: E Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:43:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI CEN/TS 15290:2006 2 Contents Page Foreword3 Introduction .
17、4 1 Scope 5 2 Normative references 5 3 Terms and definitions .5 4 Symbols and abbreviations 5 5 Principle6 6 Reagents.6 7 Apparatus .7 8 Preparation of the test sample .7 9 Procedure .7 10 Calculations9 11 Precision of the method10 12 Test Report .10 Annex A (informative) List of conversion factors
18、11 Bibliograhpy 12 Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:43:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI CEN/TS 15290:2006 3 Foreword This Technical Specification (CEN/TS 15290:2006) has been prepared by Technical Committee CEN/TC 335 “Solid biofue
19、ls”, the secretariat of which is held by SIS. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to announce this CEN Technical Specification: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, German
20、y, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:43:43 GMT+00:
21、00 2006, Uncontrolled Copy, (c) BSI 4 Introduction The 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 may be helpful to predict the melting behaviour and slagging of the ashes. Moreover,
22、contamination of fuel with sand or soil is indicated by high values of several elements. In this Technical Specification, wet chemical methods are described. As an alternative, X-ray fluorescence (XRF) may be used when validated with suitable materials (biomass reference materials). CEN/TS 15290:200
23、6 Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:43:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 5 1 Scope This Technical Specification describes methods for the determination of major elements of solid biofuels respectively of their ashes, which are Al, Ca
24、, Fe, Mg, P, K, Si, Na, Ti. The determination of barium (Ba) and manganese (Mn) is also possible with the methods described in this Technical Specification. The Standard includes two parts: Part A describes the direct determination on the fuel, this method is also applicable for sulfur and minor ele
25、ments, part B gives a method of determination on a prepared 550C ash. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced d
26、ocument (including any amendments) applies. CEN/TS 14588:2003, Solid biofuels Terminology, definitions and descriptions CEN/TS 14775, Solid biofuels Methods for the determination of ash content CEN/TS 14780, Solid biofuels Methods for sample preparation prCEN/TS 15296, Solid biofuels Calculation of
27、analyses to different bases EN ISO 7980, Water quality Determination of calcium and magnesium Atomic absorption spectrometric method (ISO 7980:1986) EN ISO 11885, Water quality Determination of 33 elements by inductively coupled plasma atomic emission spectrometry (ISO 11885:1996) EN ISO 17294-2, Wa
28、ter quality Application of inductively coupled plasma mass spectrometry (ICP/MS) Part 2: Determination of 62 elements (ISO 17294-2:2003) ISO 9964-1, Water quality Determination of sodium and potassium Part 1: Determination of sodium by atomic absorption spectrometry ISO 9964-2, Water quality Determi
29、nation of sodium and potassium Part 2: Determination of potassium by atomic absorption spectrometry ISO 9964-3, Water quality Determination of sodium and potassium Part 3: Determination of sodium and potassium by flame emission spectrometry 3 Terms and definitions For the purposes of this Technical
30、Specification, the terms and definitions given in CEN/TS 14588:2003 apply. 4 Symbols and abbreviations 4.1 Symbols Al Aluminium CEN/TS 15290:2006 Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:43:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 6 Ca Calcium Fe
31、Iron Mg Magnesium P Phosphorus K Potassium Si Silicon Na Sodium Ti Titanium 4.2 Abbreviations ICP-OES Inductively Coupled Plasma Optical Emission Spectrometry ICP-MS Inductively Coupled Plasma Mass Spectrometry FAAS Flame Atomic Absorption Spectrometry FES Flame Emission Spectrometry 5 Principle The
32、 sample is digested in a closed vessel by the help of reagents, 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 may be done by Inductively Coupled Plasma Optical Emission Spectrometry (ICP/
33、OES), Inductively Coupled Plasma Mass Spectrometry (ICP/MS) or Flame Atomic Absorption Spectrometry (FAAS). 6 Reagents 6.1 General All reagents should be of analytical grade or better. If minor elements are also to be determined, the best qualities should be used. 6.2 Water Water containing negligib
34、le amounts of major elements, i.e. amounts that do not contribute significant to the determinations. Deionised water will normally fulfil this requirement. 6.3 Nitric acid (HNO3) 65 % (w/w), = 1.40 g/ml 6.4 Hydrogen peroxide (H2O2) CEN/TS 15290:2006 Licensed Copy: London South Bank University, Londo
35、n South Bank University, Tue Dec 12 05:43:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 7 30 % (w/w), = 1.11 g/ml 6.5 Hydrofluoric acid (HF) 40 % (w/w), = 1.13 g/ml CAUTION Hydrofluoric acid may lead to health hazards. 6.6 Boric acid (H3BO3) 4 % (w/w) 7 Apparatus 7.1 Heating oven or heating block su
36、itable for the decomposition system in use Resistance heated oven or heating block that can be used at a temperature of at least 220C with an accuracy of +/- 10C. 7.2 Microwave oven Intended for laboratory use and preferably equipped with temperature control. 7.3 Sample digestion vessels Intended fo
37、r the heating system used, normally made of a fluoro plastic. 7.4 Balance With a resolution of least 1 mg. 7.5 Plastic volumetric flasks 8 Preparation of the test sample The test sample is the general analysis test sample with a nominal top size of 1 mm or less, prepared in accordance with CEN/TS 14
38、780. The results are to be calculated on a dry basis. Therefore the moisture content of the test sample should be determined as described in CEN/TS 14774-3. 9 Procedure 9.1 Digestion NOTE Hydrofluoric acid may cause volatile compounds during the digestion. 9.1.1 Part A: Direct determination on the f
39、uel The decomposition shall be carried out in closed vessels. It can be done in a heating oven, a heating block or in a microwave oven. CEN/TS 15290:2006 Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:43:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 8 Mix 50
40、0 mg of ground and homogenised sample with 3,0 ml H2O2 (30 %), 8,0 ml HNO3 (65 %) and 1,0 ml HF (40 %) in a closed decomposition vessel. A reaction time of 5 min should be kept before closing the vessel. The heating of the vessel should not be to fast. Heat the sample according to the following heat
41、ing programmes for digestion: Resistance heating1) : Step 1: In 1 h heat to 220 C, rate 3,33 C /min Step 2: Hold for 1 h at 220 C Microwave heating2) : Step 1: In 15 min heat to 190 C, rate 11,3 in C /min Step 2: Hold for 20 min at 190 C After cooling to room temperature, HF is neutralised by adding
42、 10 ml H3BO3 (4 %). Reheat the sample according to the following heating programmes for neutralisation: Resistance heating1): Step 1: Heat as fast as possible up to 180 C Step 2: Hold for 15 min at 180 C Microwave heating2): Step 1: Heat as fast as possible to 150 C Step 2: Hold for 15 min at 150 C
43、After cooling, transfer the digest to a volumetric flask. Rinse the digestion vessel carefully and transfer the rinse solution to the volumetric flask. Add deionised water to the digest to an appropriate volume, depending on the detection method to be used. NOTE Some available digestion bomb systems
44、 use fluoropolymer vessels, which cannot withstand temperatures above 170 C. In such cases this lower temperature can be used, provided that the sample is hold longer at this temperature and that comparable results can be obtained, e.g. by the use of equivalent biomass reference materials. 9.1.2 Par
45、t B: determination on a prepared 550C ash Heat the sample according to the procedure described in CEN/TS 14775 to obtain ash. For the digestion of the ash similar working steps, as for the digestion of the fuel, are evident: Mix 50 mg of homogenised sample with 2,0 ml H2O2 (30 %), 3,0 ml HNO3 (65 %)
46、 and 0,75 ml HF (40 %) in a closed decomposition vessel. Digest the sample following one of the heating programmes described in section 9.1.1 for digestion. After cooling to room temperature, the HF is neutralized by adding 7,5 ml H3BO3 (4 %) and 20 ml deionised water. Reheat the sample according to
47、 the heating programmes for neutralisation described in section 9.1.1. 1) The stated temperature refers to heating device (e.g. oven). 2) The stated temperature refers to digest solution. CEN/TS 15290:2006 Licensed Copy: London South Bank University, London South Bank University, Tue Dec 12 05:43:43
48、 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 9 After cooling, transfer the digest to a volumetric flask. Rinse the digestion vessel carefully and transfer the rinse solution to the volumetric flask. Add deionised water to the digest to an appropriate volume, depending on the detection method to be us
49、ed. NOTE The digestion of the ash has to be carried out immediately after the preparation. Otherwise there is the risk of moisture absorption. 9.2 Detection methods For the detection of the concentrations of Al, Ca, Fe, Mg, P, K, Si, Na, Ti in the digests the following methods can be used: ICP/OES according to EN ISO 11885. ICP/MS according to EN ISO 17294-2. AAS according to EN ISO 7980, ISO 9964-1 and ISO 996