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1、DRAFT FOR DEVELOPMENT DD CEN/TS 15407:2006 Solid recovered fuels Method for the determination of carbon (C), hydrogen (H) and nitrogen (N) content ICS 75.160.10 ? Licensed Copy: London South Bank University, London South Bank University, Sun Dec 24 04:44:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI
2、 DD CEN/TS 15407:2006 This Draft for Development was published under the authority of the Standards Policy and Strategy Committee on 30 November 2006 BSI 2006 ISBN 0 580 48566 8 National foreword This Draft for Development was published by BSI. It is the UK implementation of CEN/TS 15407:2006. This
3、publication is not to be regarded as a British Standard. It is being issued in the Draft for Development series of publications and is of a provisional nature. It should be applied on this provisional basis, so that information and experience of its practical application can be obtained. Comments ar
4、ising 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 not later than 3 years after its publication by the European organiz
5、ation so that a decision can be taken on its status. 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, the responsible BSI Committee will decide whether to su
6、pport the conversion into a European Standard, to extend the life of the Technical Specification or to withdraw it. Comments should be sent to the Secretary of the responsible BSI Technical Committee at British Standards House, 389 Chiswick High Road, London W4 4AL. The UK participation in its prepa
7、ration was entrusted to Technical Committee PTI/17, Solid biofuels. A list of organizations represented on PTI/17 can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. A
8、mendments issued since publication Amd. No. DateComments Licensed Copy: London South Bank University, London South Bank University, Sun Dec 24 04:44:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI TECHNICAL SPECIFICATION SPCIFICATION TECHNIQUE TECHNISCHE SPEZIFIKATION CEN/TS 15407 September 2006 ICS 7
9、5.160.10 English Version Solid recovered fuels - Method for the determination of carbon (C), hydrogen (H) and nitrogen (N) content Combustibles solides de rcupration - Mthode pour la dtermination de la teneur en carbone (C), en hydrogne (H) et en azote (N) Feste Sekundrbrennstoffe - Verfahren zur Be
10、stimmung des Gehaltes an Kohlenstoff (C), Wasserstoff (H) und Stickstoff (N) This Technical Specification (CEN/TS) was approved by CEN on 25 March 2006 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 r
11、equested to submit their comments, particularly on the question whether the CEN/TS can be converted into a European 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 f
12、orm. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS) until the final 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,
13、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 COMIT EUROPEN DE NORMALISATION EUROPISCH
14、ES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2006 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. CEN/TS 15407:2006: E Licensed Copy: London South Bank University, London South Bank University, Sun Dec 2
15、4 04:44:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 2 Contents Page Foreword3 Introduction.4 1 Scope 5 2 Normative references5 3 Terms and definitions .5 4 Safety remarks.5 5 Principle5 6 Reagents and calibration standards5 7 Apparatus .6 8 Procedure .6 9 Expression of results 7 10 Performance cha
16、racteristics 8 11 Test report8 Annex A (normative) Guidelines - Characteristics of the laboratory sample for chemical analysis of SRF .9 Bibliography11 CEN/TS 15407:2006 Licensed Copy: London South Bank University, London South Bank University, Sun Dec 24 04:44:14 GMT+00:00 2006, Uncontrolled Copy,
17、(c) BSI 3 Foreword This document (CEN/TS 15407:2006) has been prepared by Technical Committee CEN/TC 343 “Solid Recovered Fuels”, the secretariat of which is held by SFS. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to a
18、nnounce this CEN Technical Specification: Austria, Belgium, 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, Switzerla
19、nd and United Kingdom. CEN/TS 15407:2006 Licensed Copy: London South Bank University, London South Bank University, Sun Dec 24 04:44:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 4 Introduction The determination of carbon, hydrogen and nitrogen is usually performed using instrumental methods. The la
20、tter can be divided in two groups depending on the amount of test portion used. Micro instrumental methods require few mg of sample; macro methods use grams of sample. If micro methods are used for SRF analysis, a very homogeneous test sample needs to be prepared in order to obtain the required prec
21、ision. CEN/TS 15407:2006 Licensed Copy: London South Bank University, London South Bank University, Sun Dec 24 04:44:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 5 1 Scope This Technical Specification describes a method for the determination of total carbon, hydrogen and nitrogen contents in solid
22、recovered fuels by instrumental techniques. This method is applicable for concentrations on dry matter basis of C over 0,1 %, N over 0,01 % and H over 0,1 %. 2 Normative references The following referenced documents are indispensable for the application of this Technical Specification. For dated ref
23、erences, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. CEN/TS 15357:2006, Solid recovered fuels Terminology, definitions and descriptions CEN/TS 15413, Solid recovered fuels Methods for the preparation of the
24、 test sample from the laboratory sample prCEN/TS 15414-3, Solid recovered fuels Determination of moisture content using the oven dry method Part 3: Moisture in general analysis sample 3 Terms and definitions For the purposes of this Technical Specification, the terms and definitions given in CEN/TS
25、15357:2006 apply. 4 Safety remarks The safety in handling of potentially hazardous materials is dealt with in relevant national and European regulations, which every laboratory should refer to. In addition the following information is given: instruments for carbon, hydrogen and nitrogen determinatio
26、n shall be used only by experienced personnel, following the safety instructions of the manufacturer. 5 Principle The method is based on the complete oxidation of the sample (“flash combustion“ instruments can also be used) which converts all organic substances into combustion products. The resultin
27、g combustion gases pass through a reduction furnace and are swept into the chromatographic column by the carrier gas (helium) where they are separated and detected quantitatively by appropriate instrumental gas analysis procedures (for example by a thermal conductivity detector (TCD). The samples ar
28、e held in a suitable container (tin or other crucible) and then dropped inside the quartz tube furnace at about 1000 C in an oxygen stream for complete oxidation in the presence of a catalyst layer. Excess oxygen is removed by contact with copper, while nitrogen oxides are reduced to elemental nitro
29、gen. 6 Reagents and calibration standards All reagents shall be at least of analytical grade and suitable for their specific purposes. 6.1 Carrier gas: Helium, 99,99 % or other gases as specified by the instrument manufacturer. CEN/TS 15407:2006 Licensed Copy: London South Bank University, London So
30、uth Bank University, Sun Dec 24 04:44:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 6 6.2 Oxygen, free of combustion material, purity 99,95 %, or as specified by the instrument manufacturer. 6.3 Additional reagents: as specified by the instrument manufacturer. 6.4 Calibration standards Examples are
31、given in the following table. Table 1 Calibration standards Name Formula % C % H % N Acetanilide C8H9NO 71,1 6,7 10,4 Atropin C17H23NO3 70,6 8,0 4,8 Benzoic acid C7H6O2 68,8 5,0 0,0 Cystine C6H12N2O4S2 30,0 5,0 11,7 Diphenylamine C12H11N 85,2 6,5 8,3 EDTA C10H16N2O8 41,1 5,5 9,6 Phenylalanine C9H11N
32、O2 65,4 6,7 8,5 Sulfanil amide C6H8N2O2S 41,8 4,7 16,3 Sulfanilic acid C6H7NO3S 41,6 4,1 8,1 TRIS C4H11NO3 39,7 9,1 11,6 7 Apparatus Various instrumental configurations are available. The general requirements for a suitable apparatus are: a) the combustion conditions shall be such that all carbon, h
33、ydrogen and nitrogen are converted to carbon dioxide, water vapour and nitrogen oxide or elemental nitrogen; b) a separation step is included to reduce or eliminate any possible interference during the subsequent determination; c) nitrogen shall be reduced to the elemental form before the detection;
34、 d) analytical balance, resolution of at least 1 part per thousand of the weighted amount. 8 Procedure 8.1 Sample conservation and pre-treatment The laboratory samples shall be stored according to guidelines defined in Annex A. 8.2 Sample preparation The test portion shall be prepared from the labor
35、atory sample according to CEN/TS 15413. The amount of test portion depends on the particular instrument used. The particle size of the test sample should be related to the amount of sample to be used, according to CEN/TS 15413. For some types of instruments it is necessary to carry out the determina
36、tion of hydrogen on dried analysis samples. Before carrying out direct analyses of moist analysis samples, it therefore should be controlled that identical results can be achieved compared with analyses carried out on dried samples. For a determination on dry sample, the analysis sample shall be dri
37、ed at 105 C as described in prCEN/TS 15414-3 immediately before the determination. CEN/TS 15407:2006 Licensed Copy: London South Bank University, London South Bank University, Sun Dec 24 04:44:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 7 Whereas the determination is carried out on dry basis, the
38、moisture content shall be determined according to prCEN/TS 15414-3. 8.3 Preparation of the test portion Weigh the appropriate amount of material as recommended by the instrument manufacturer as appropriate for the type of instrument and the expected content of carbon, hydrogen and nitrogen. The test
39、 portion shall be weighed directly into the sample capsule in the case of a micro- or semi-micro analyser. Otherwise it may be weighed directly or transferred from a suitable weighing container. 8.4 Calibration Set up the instrument following the manufacturer instructions. Stabilize the furnace and
40、analyzer. Select 3 to 5 reference materials with increasing concentration of nitrogen, hydrogen and carbon. Calibrate the instruments for nitrogen, hydrogen and carbon determination following the manufacturer instructions. Use the same procedure as for sample analysis (see below). Alternatively, dif
41、ferent amounts of the same substance can be used to prepare the calibration. Verify the calibration by analysing as a test sample a portion of a suitable standard, preferably with a different material than that used for the calibration. The calibration is acceptable if the measured value differs fro
42、m the standard value by no more than the repeatability limit for the test method. Otherwise repeat the calibration procedure. 8.5 Analysis of samples Weight the test portion and transfer it into the instrumental apparatus. Start the cycle following then operating instruction for the specific instrum
43、ents. At least 3 replicates are necessary. 9 Expression of results The total carbon, hydrogen and nitrogen contents of the solid recovered fuels shall be expressed as a percentage by mass on the dry basis. Most commercially available instruments give the results directly. The following equations sha
44、ll be used: for the carbon content: ad add M CC = 100 100 for the nitrogen content: ad add M NN = 100 100 for the hydrogen content: CEN/TS 15407:2006 Licensed Copy: London South Bank University, London South Bank University, Sun Dec 24 04:44:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 8 ad ad add
45、M M HH = 100 100 937, 8 where d is dry basis; ad is as determined; Mad is the moisture content of the general analysis sample when analysed. 10 Performance characteristics Data about performances of the methods will be available after validation in QUOVADIS project. 11 Test report The test report sh
46、all contain at least the following information: a) name, address and location of any laboratory involved in the analysis; b) description and identification of the laboratory sample; c) date of receipt of laboratory sample and date(s) of performance of test; d) a reference to this Technical Specifica
47、tion, i.e. CEN/TS 15407; e) reference to the analytical standard used for the determination for each element; f) the analytical results, referring to Clause 9; g) any details not specified in this Technical Specification or which are optional, and any other factors which may have affected the result
48、s; h) unique identification of report (such as serial number) and of each page and total number of pages of the report. The laboratory should keep a trace of any analytical steps and intermediate results (chromatograms, raw data and calculation details) that should be kept available in case of speci
49、fic requirements (e.g. accreditation). CEN/TS 15407:2006 Licensed Copy: London South Bank University, London South Bank University, Sun Dec 24 04:44:14 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 9 Annex A (normative) Guidelines - Characteristics of the laboratory sample for chemical analysis of SRF The following requirements apply when preparing the laboratory sample for the chemical characterisation of SRF samples according to this Technical Specification. NOTE Equivalent requiremen
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