EN 15148-2009 en Solid biofuels - Determination of the content of volatile matter《固体燃料 挥发性物质含量的测定》.pdf

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1、BS EN 15148:2009ICS 75.160.10NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDSolid biofuels Determination of thecontent of volatilematterThis British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 31 March2010 BSI 2010IS

2、BN 978 0 580 66694 0Amendments/corrigenda issued since publicationDate CommentsBS EN 15148:2009National forewordThis British Standard is the UK implementation of EN 15148:2009. Itsupersedes DD CEN/TS 15148:2005 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalComm

3、ittee PTI/17, Solid biofuels.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance with a British Standard c

4、annot confer immunityfrom legal obligations.BS EN 15148:2009EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15148 November 2009 ICS 75.160.10 Supersedes CEN/TS 15148:2005English Version Solid biofuels - Determination of the content of volatile matter Biocombustibles solides - Mthode de dtermina

5、tion de la teneur en matires volatiles Feste Biobrennstoffe - Bestimmung des Gehaltes an flchtigen Substanzen This European Standard was approved by CEN on 3 October 2009. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this Europea

6、n 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 application to the CEN Management Centre or to any CEN member. This European Standard exists in three official versions (English,

7、 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 Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cy

8、prus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION

9、COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15148:2009: EBS EN 15148:2009EN 15148:2009 (E) 2 Contents Page

10、Foreword 3Introduction .41 Scope 52 Normative references 53 Terms and definitions .54 Principle 55 Apparatus .56 Temperature calibration . 107 Preparation of the test sample 108 Procedure 109 Calculation . 1010 Precision 1111 Test report . 11Bibliography . 12BS EN 15148:2009EN 15148:2009 (E) 3 Forew

11、ord This document (EN 15148:2009) has been prepared by 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 the latest by May

12、 2010, and conflicting national standards shall be withdrawn at the latest by May 2010. 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

13、. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. This document supersedes CEN/TS 15148:2005. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound

14、to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Swit

15、zerland and the United Kingdom. BS EN 15148:2009EN 15148:2009 (E) 4 Introduction The volatile matter content is determined as the loss in mass, less that due to moisture, when solid biofuel is heated out of contact with air under standardised conditions. The test is empirical and, in order to ensure

16、 reproducible results, it is essential that the rate of heating, the final temperature and the overall duration of the test are carefully controlled. It is also essential to exclude air from the solid biofuel during heating to prevent oxidation. The fit of the crucible lid is therefore critical. The

17、 moisture content of the general analysis sample is determined at the same time as the volatile matter so that the appropriate correction can be made. BS EN 15148:2009EN 15148:2009 (E) 5 1 Scope This European Standard aims to define the requirements and method used to determine the volatile matter c

18、ontent of solid biofuels. It is intended for persons and organisations that manufacture, plan, sell, erect or use machinery, equipment, tools and entire plants related to solid biofuels, and to all persons and organisations involved in producing, purchasing, selling and utilising solid biofuels. The

19、 volatile matter content is determined as the loss in mass, less that due to moisture, when solid biofuel is heated out of contact with air under standardized conditions. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated refer

20、ences, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. CEN/TS 14588:2003, Solid biofuels Terminology, definitions and descriptions CEN/TS 14780, Solid biofuels Methods for sample preparation EN 14774-3, Solid b

21、iofuels Determination of moisture content Oven dry method Part 3: Moisture in general analysis sample 3 Terms and definitions For the purposes of this document, the terms and definitions given in CEN/TS 14588:2003 shall apply. 4 Principle A test portion of the general analysis sample is heated out o

22、f contact with ambient air at (900 10) C for 7 min. The percentage of volatile matter is calculated from the loss in mass of the test portion after deducting the loss in mass due to moisture. Automatic equipment may be used when the method is validated with biomass reference samples of an adequate b

23、iomass type. This equipment shall fulfil all the requirements given in Clauses 5 to 8 regarding sample size, atmosphere, temperatures and weighing accuracy. 5 Apparatus 5.1 Furnace The furnace shall be heated by electricity, in which a zone of uniform temperature of (900 10) C can be maintained. It

24、may be of the stop-ended type or fitted at the back with a flue (see Figure 1, as example). NOTE It is important for furnaces with flues that the furnace door seals well. The flue should not reach far out of the oven and should be fitted with a butterfly valve to restrict airflow through the furnace

25、. Its heat capacity shall be such that, with an initial temperature of (900 10) C, the temperature is regained within 4 min after insertion of a cold stand and its crucibles. The temperature is measured with a thermocouple, as described in 5.2. BS EN 15148:2009EN 15148:2009 (E) 6 Normally the furnac

26、e will be designed specifically either for multiple determinations using a number of crucibles in one stand or for receiving one crucible and its stand. The crucible stand shall be placed in the middle of the furnace. The temperature of 900 C shall be attained as closely as possible with a specified

27、 tolerance of 10 C in order to compensate for inherent errors in the temperature measurement and lack of uniformity in the temperature distribution. 5.2 Thermocouples A sheathed thermocouple shall be permanently installed in the furnace (see Figure 1) with its thermojunction as close as possible to

28、the centre of the heating chamber. An unsheathed thermocouple long enough to reach the centre of the heating chamber. This thermocouple is used for calibration. 5.3 Crucible The crucible shall be cylindrical, with a well-fitting lid, both of fused silica. The crucible with lid shall have a mass betw

29、een 10 g and 14 g and dimensions approximating to those shown in Figure 2. The fit of the lid on the crucible is critical to the determination and a lid shall be selected to match the crucible so that the horizontal clearance between them is no greater than 0,5 mm. After selection, the crucible and

30、the lid shall be ground together to give smooth surfaces and then be given a common distinguishing mark. 5.4 Crucible stand The crucible stand on which the crucible is placed in the furnace, shall be such that the appropriate rate of heating can be achieved. For example, it may consist of the follow

31、ing: a) for single determinations, a ring of heat-resistant steel wire as shown in Figure 3 a) with ceramic discs, 25 mm diameter and 2 mm thick, resting on the inner projection of its legs; or b) for multiple determinations, a tray of heat-resistant steel wire as shown in Figure 3 b), of appropriat

32、e size, with ceramic plates 2 mm thick supporting the crucibles. 5.5 Balance The balance shall be capable of reading to the nearest 0,1 mg. BS EN 15148:2009EN 15148:2009 (E) 7 Key 1 Flue 2 Valve 3 Thermocouple 4 Heating system 5 Zone of uniform temperature 6 Check thermocouple 7 Chamber (width 200 m

33、m) Figure 1 Example of suitable furnace BS EN 15148:2009EN 15148:2009 (E) 8 Dimensions in millimetres Figure 2 Silica crucible and lid BS EN 15148:2009EN 15148:2009 (E) 9 Key 1 Three legs spaced 120 apart 2 Ring 3 Handle 4 Ceramic plates Figure 3 Examples of crucible stands BS EN 15148:2009EN 15148:

34、2009 (E) 10 6 Temperature calibration The furnace temperature readings shall be checked at regular time intervals with an unsheathed calibrated thermocouple. The unsheathed thermocouple (see Clause 5) shall be positioned as close as possible to the area of the permanently installed thermocouple. NOT

35、E The temperature/electromotive force relationship of a thermojunction maintained at elevated temperatures gradually changes with time. 7 Preparation of the test sample The test sample is the general analysis sample with a nominal top size of 1 mm or less, prepared in accordance with CEN/TS 14780. T

36、he general analysis sample shall be well mixed and in moisture equilibrium with the laboratory atmosphere, or oven-dry (dried by the same procedure as described in EN 14774-3). A test portion of the general analysis sample shall be separated for the determination of moisture content at the same time

37、 to the determination of volatile matter. The moisture content shall be determined according to EN 14774-3. 8 Procedure Fill either a stand with one empty crucible and lid (Figure 3a) or a stand with the requisite number of empty crucibles and lids (Figure 3b) and insert in the oven. Maintain at (90

38、0 10) C for 7 min. Remove the crucible(s) from the furnace and allow to cool to room temperature on a plate of thermo-resistant material and store in desiccator. Weigh cool empty crucible(s) and lid(s) and weigh (1 0,1) g test portion of the general analysis sample into the crucible(s) to the neares

39、t 0,1 mg. Replace the lid(s) and tap the crucible(s) on a clean hard surface until the test portion forms a layer of even thickness on the bottom of the crucible Place the charged crucible(s) in a cold stand, transfer to the furnace, close the door and leave for 7 min 5 s. Place the crucible(s) on a

40、 thermo-resistant plate and allow to cool to 30 C to 50 C above room temperature and finally to room temperature in a dessicator. When cool, weigh the crucible(s) to the nearest 0,1 mg. NOTE 1 The same treatment of the crucible before and after the determination minimizes the effect of any film of w

41、ater adsorbed on its surface, while the rapid cooling reduces absorption of moisture by the solid biofuel residue. NOTE 2 If multiple determinations are being made, any vacant places in the stand should be filled with empty crucibles. NOTE 3 For some types of solid biofuels it may be necessary to ca

42、rry out the determination on dry sample in order to avoid loss of material due to violent reactions during the heating process. In this case, the charged crucibles are dried at 105 C and cooled, according to EN 14774-3, before the transfer in the furnace. 9 Calculation The volatile matter Vdin the s

43、ample, expressed as a percentage by mass on the dry basis, is given by the equation:BS EN 15148:2009EN 15148:2009 (E) 11 )100100()(1001232adadMMmmmmVd= (1) where m1 is the mass, in g, of the empty crucible and lid; m2 is the mass, in g, of the crucible and lid and test portion before heating; m3 is

44、the mass, in g, of the crucible and lid and contents after heating; Mad is the moisture, as a percentage by mass, in the general analysis sample as analysed, determined according to EN 14774-3. Report the result, as the mean of duplicate determinations, rounded to the nearest 0,1 % (m/m). The result

45、s of the determination described in this European Standard are reported on the dry basis. 10 Precision 10.1 Repeatability The results of the duplicate determinations (performed within a short period of time, but not simultaneously) in the same laboratory, by the same operator, using the same apparat

46、us on two representative test portions taken from the same general analysis sample, shall not differ by more than the value given in Table 1. See 2 in the bibliography. 10.2 Reproducibility The means of the results of duplicate determinations, performed in each of two different laboratories on repre

47、sentative test portions taken from the same general analysis sample shall not differ by more than the values given in Table 1. Table 1 Volatile matter Maximum acceptable differences between results obtained (calculated to dry basis) Repeatability limit Reproducibility critical difference Solid biofu

48、el 2,0 % of the mean result 4,0 % of the mean result 11 Test report The test report shall include the following information: a) identification of the laboratory and the testing date; b) identification of the product or sample tested; c) reference to this European Standard; d) any deviations from thi

49、s European Standard; e) test results of the determination on dry basis; f) conditions and observations, i.e. unusual features, during the test procedure, which may affect the results. The test results shall be expressed with relevant symbols. BS EN 15148:2009EN 15148:2009 (E) 12 Bibliography 1 ISO 562, Hard coal and coke Determination of volatile matter 2 OFI VT 2007 (interlaboratory comparison tests, round robins), Final Report , Vienna, December 2007 3 ASTM D6374