1、May 2011 Translation by DIN-Sprachendienst.English price group 10No 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).ICS 75
2、.160.10!$p_j“1776071www.din.deDDIN EN 15407Solid recovered fuels Methods for the determination of carbon (C), hydrogen (H) andnitrogen (N) contentEnglish translation of DIN EN 15407:2011-05Feste Sekundrbrennstoffe Verfahren zur Bestimmung des Gehaltes an Kohlenstoff (C), Wasserstoff (H) undStickstof
3、f (N)Englische bersetzung von DIN EN 15407:2011-05Combustibles solides de rcupration Mthodes pour la dtermination de la teneur en carbone (C), en hydrogne (H) et enazote (N)Traduction anglaise de DIN EN 15407:2011-05SupersedesDIN CEN/TS 15407:2006-12www.beuth.deDocument comprises pagesIn case of dou
4、bt, the German-language original shall be considered authoritative.1604.11 DIN EN 15407:2011-05 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 343 “Solid recovered fuels” (Secretariat: SFS, Finland). The responsible German body
5、involved in its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee), Working Committee NA 062-05-83 AA Sekundrbrennstoffe. The DIN Standard corresponding to the International Standard referred to in this document is as follows: ISO 5725-5 DIN ISO 5725-5 Amendme
6、nts This standard differs from DIN CEN/TS 15407:2006-12 as follows: a) the prestandard status has been changed to that of a full standard; b) Annex B “Data on performance characteristics” and Annex C “Major results of ruggedness testing” (both informative) have been included; c) the Bibliography has
7、 been updated; d) the standard has been editorially revised. Previous editions DIN CEN/TS 15407: 2006-12 National Annex NA (informative) Bibliography DIN ISO 5725-5, Accuracy (trueness and precision) of measurement methods and results Part 5: Alternative methods for the determination of the precisio
8、n of a standard measurement method 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15407 March 2011 ICS 75.160.10 Supersedes CEN/TS 15407:2006English Version Solid recovered fuels Methods for the determination of carbon (C), hydrogen (H) and nitrogen (N) content Combustibles solides de rcupra
9、tion Mthodes pour la dtermination de la teneur en carbone (C), en hydrogne (H) et en azote (N) Feste Sekundrbrennstoffe Verfahren zur Bestimmung des Gehaltes an Kohlenstoff (C), Wasserstoff (H) und Stickstoff (N) This European Standard was approved by CEN on 22 January 2011. CEN members are bound to
10、 comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard 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-CEN
11、ELEC 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 and notified to the CEN-CENELEC Management Centre has th
12、e same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland
13、,Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by any
14、means reserved worldwide for CEN national Members. Ref. No. EN 15407:2011: EEN 15407:2011 (E) 2 Contents Page Foreword 3Introduction .41 Scope 42 Normative references 43 Terms and definitions .44 Safety remarks .45 Principle 56 Reagents and calibration standards 57 Apparatus .58 Procedure .69 Expres
15、sion of results 710 Performance characteristics 711 Test report 7Annex A (normative) Guidelines - Characteristics of the laboratory sample for chemical analysis of SRF .9Annex B (informative) Data on performance characteristics 11Annex C (informative) Major results of ruggedness testing 13Bibliograp
16、hy . 14DIN EN 15407:2011-05 EN 15407:2011 (E) 3 Foreword This document (EN 15407:2011) has been prepared by Technical Committee CEN/TC 343 “Solid recovered fuels”, the secretariat of which is held by SFS. This European Standard shall be given the status of a national standard, either by publication
17、of an identical text or by endorsement, at the latest by September 2011, and conflicting national standards shall be withdrawn at the latest by September 2011. This document supersedes CEN/TS 15407:2006. Attention is drawn to the possibility that some of the elements of this document may be the subj
18、ect of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. This document differs from CEN/TS 15407:2006 only edi
19、torially. 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, Estonia, Finland, France, Germany, Greece, Hungary, Icelan
20、d, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. DIN EN 15407:2011-05 EN 15407:2011 (E) 4 Introduction The determination of carbon, hydrogen and nitrogen is usually performed us
21、ing instrumental methods. The latter 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 o
22、rder to obtain the required precision. 1 Scope This European Standard specifies a method for the determination of total carbon, hydrogen and nitrogen contents in solid recovered fuels by instrumental techniques. This method is applicable for concentrations on dry matter basis of C over 0,1 %, N over
23、 0,01 % and H over 0,1 %. 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 document (including any amendments) applies.
24、EN 15357:2011, Solid recovered fuels Terminology, definitions and descriptions EN 154131), Solid recovered fuels Methods for the preparation of the test sample from the laboratory sample EN 15414-3, Solid recovered fuels Determination of moisture content using the oven dry method Part 3: Moisture in
25、 general analysis sample 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 15357:2011 apply. 4 Safety remarks The safety in handling of potentially hazardous materials is dealt with relevant national and European regulations, which every laboratory shou
26、ld refer to. In addition the following information is given: only experienced personnel, following the safety instructions of the manufacturer, shall use instruments for carbon, hydrogen and nitrogen determination. 1)To be published. DIN EN 15407:2011-05 EN 15407:2011 (E) 5 5 Principle The method is
27、 based on the complete oxidation of the sample (“flash combustion“ instruments can also be used) which converts all organic substances into combustion products. The resulting combustion gases pass through a reduction furnace and are swept into the chromatographic column by the carrier gas (helium) w
28、here they are separated and detected quantitatively by appropriate instrumental gas analysis procedures (for example by a thermal conductivity detector (TCD). The samples are held in a suitable container (tin or other crucible) and then dropped inside the quartz tube furnace at about 1 000 C in an o
29、xygen 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 nitrogen. 6 Reagents and calibration standards All reagents shall be at least of analytical grade and suitable for their specific p
30、urposes. 6.1 Carrier gas: Helium, 99,99 % or other gases as specified by the instrument manufacturer. 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 standar
31、ds Examples are given in Table 1. Table 1 Calibration standards Name Formula C% H % N % Acetanilide C8H9NO 71,1 6,7 10,4 Atropine C17H23NO370,6 8,0 4,8 Benzoic acid C7H6O268,8 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 C9H1
32、1NO265,4 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,
33、hydrogen 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; DIN EN 15407:2011-05 EN 15407:2011 (E) 6 c) nitrogen shall be reduced t
34、o the elemental form before the detection; 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 tes
35、t portion shall be prepared from the laboratory sample according to EN 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 EN 15413. For some types of instruments it is ne
36、cessary to carry out the determination of hydrogen on dried analysis samples. For some other types of instruments it is necessary to carry out the determination of carbon on analysis samples that are not completely dried. Working with samples that has been dried at 105 C and then equilibrated with t
37、he moisture in the air on the lab where the CHN analysis are handled, is a good compromise for the C and H moisture artefact, but then extra moisture determinations on the air-dry sample will have to be done. The nominal top size of the test sample shall be 1 mm or less. For some instruments it may
38、be necessary to prepare a test sample with a lower nominal top size than 1 mm, e.g. 0,25 mm, in order to keep the desired precision. For “new products” an adequate particle size shall be determined by validation experiments. Whereas the determination is carried out on dry basis, the moisture content
39、 shall be determined according to EN 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 portion shall be weig
40、hed 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 analyzer. Select 3 to
41、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 different amounts of the s
42、ame substance may 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 from the standard value by
43、 no more than the repeatability limit for the test method. Otherwise repeat the calibration procedure. DIN EN 15407:2011-05 EN 15407:2011 (E) 7 8.5 Analysis of samples Weight the test portion and transfer it into the instrumental apparatus. Start the cycle following then operating instruction for th
44、e specific instruments. 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 follo
45、wing equations shall be used: for the carbon content: adaddMCC=100100(1) for the nitrogen content: adaddMNN=100100(2) for the hydrogen content: adadaddMMHH=100100937,8(3) where dis dry basis; adis as determined; Madis the moisture content of the general analysis sample when analysed. 10 Performance
46、characteristics Data on performance characteristics of the present method are given in Annex B which presents the results of the QUOVADIS validation project (Quality Management, Organisation, Validation of standards, Developments and Inquiries for SRF) 9. 11 Test report The test report shall contain
47、 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; DIN EN 15407:2011-05 EN 15407:2011 (E) 8 c) date of receipt of laboratory sample and date(s) of performance of test; d) a referen
48、ce to this European Standard, i.e. EN 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 European Standard or which are optional, and any other factors which may have affected the results; 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
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