1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 15407:2011Solid recovered fuels Methods for the determinationof carbon (C), hydrogen (H) andnitrogen (N) contentBS EN 15407:2011 BRITISH STANDARDNational forewordThis Briti
2、sh Standard is the UK implementation of EN 15407:2011. Itsupersedes DD CEN/TS 15407:2006 which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee PTI/17, Solid biofuels.A list of organizations represented on this committee can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 secret
3、ary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2011ISBN 978 0 580 67708 3ICS 75.160.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published
4、 under the authority of theStandards Policy and Strategy Committee on 31 March 2011.Amendments issued since publicationDate Text affectedBS EN 15407:2011EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15407 March 2011 ICS 75.160.10 Supersedes CEN/TS 15407:2006English Version Solid recovered fue
5、ls - Methods for the determination of carbon (C), hydrogen (H) and nitrogen (N) content Combustibles solides de rcupration - 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),
6、Wasserstoff (H) und Stickstoff (N) This European Standard was approved by CEN on 22 January 2011. 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
7、-date lists and bibliographical references concerning such national standards 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 translat
8、ion under the responsibility of a CEN member into its own language and 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,
9、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 EUROPISCHES KOMITE
10、E FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15407:2011: EBS EN 15407:2011EN 15407:2011 (E) 2 Contents Page Foreword 3Introduction .41 Scope 42 Normative ref
11、erences 43 Terms and definitions .44 Safety remarks .45 Principle 56 Reagents and calibration standards 57 Apparatus .58 Procedure .69 Expression of results 710 Performance characteristics 711 Test report 7Annex A (normative) Guidelines - Characteristics of the laboratory sample for chemical analysi
12、s of SRF .9Annex B (informative) Data on performance characteristics 11Annex C (informative) Major results of ruggedness testing 13Bibliography . 14BS EN 15407:2011EN 15407:2011 (E) 3 Foreword This document (EN 15407:2011) has been prepared by Technical Committee CEN/TC 343 “Solid recovered fuels”,
13、the secretariat of which is held by SFS. 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 September 2011, and conflicting national standards shall be withdrawn at the latest by September 2011. This
14、 document supersedes CEN/TS 15407:2006. 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. This document has been prepared under a mandat
15、e given to CEN by the European Commission and the European Free Trade Association. This document differs from CEN/TS 15407:2006 only editorially. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European St
16、andard: Austria, Belgium, Bulgaria, Croatia, 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, Switzerland and United K
17、ingdom. BS EN 15407:2011EN 15407:2011 (E) 4 Introduction The determination of carbon, hydrogen and nitrogen is usually performed using 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; macr
18、o 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 precision. 1 Scope This European Standard specifies a method for the determination of total carbon, hydrogen and nitrogen contents in solid r
19、ecovered 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 document. For dated references, only th
20、e edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. 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
21、laboratory sample EN 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 document, the terms and definitions given in EN 15357:2011 apply. 4 Safety remarks The safety i
22、n handling of potentially hazardous materials is dealt with relevant national and European regulations, which every laboratory should refer to. In addition the following information is given: only experienced personnel, following the safety instructions of the manufacturer, shall use instruments for
23、 carbon, hydrogen and nitrogen determination. 1)To be published. BS EN 15407:2011EN 15407:2011 (E) 5 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 resulting
24、 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 are
25、 held in a suitable container (tin or other crucible) and then dropped inside the quartz tube furnace at about 1 000 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
26、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. 6.2 Oxygen, free of combustion material, purity 99,95 %, or as specified
27、 by the instrument manufacturer. 6.3 Additional reagents: as specified by the instrument manufacturer. 6.4 Calibration standards 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
28、,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 C9H11NO265,4 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
29、 available. The general requirements for a suitable apparatus are: a) the combustion conditions shall be such that all carbon, 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 pos
30、sible interference during the subsequent determination; BS EN 15407:2011EN 15407:2011 (E) 6 c) nitrogen shall be reduced to 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-t
31、reatment 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 laboratory sample according to EN 15413. The amount of test portion depends on the particular instrument used. The particle size of the test
32、sample should be related to the amount of sample to be used, according to EN 15413. For some types of instruments it is necessary 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 anal
33、ysis samples that are not completely dried. Working with samples that has been dried at 105 C and then equilibrated with the 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-dr
34、y 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 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
35、shall be determined by validation experiments. Whereas the determination is carried out on dry basis, the moisture content 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 approp
36、riate for the type of instrument and the expected content of carbon, hydrogen and nitrogen. The test 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 C
37、alibration Set up the instrument following the manufacturer instructions. Stabilize the furnace and 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 manu
38、facturer instructions. Use the same procedure as for sample analysis (see below). Alternatively different amounts of the same 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
39、than that used for the calibration. The calibration is acceptable if the measured value differs from the standard value by no more than the repeatability limit for the test method. Otherwise repeat the calibration procedure. BS EN 15407:2011EN 15407:2011 (E) 7 8.5 Analysis of samples Weight the test
40、 portion and transfer it into the instrumental apparatus. Start the cycle following then operating instruction for the 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 a
41、s a percentage by mass on the dry basis. Most commercially available instruments give the results directly. The following 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 dr
42、y basis; adis as determined; Madis the moisture content of the general analysis sample when analysed. 10 Performance 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, Organ
43、isation, Validation of standards, Developments and Inquiries for SRF) 9. 11 Test report The test report shall 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; BS EN 15407:
44、2011EN 15407:2011 (E) 8 c) date of receipt of laboratory sample and date(s) of performance of test; d) a reference 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 d
45、etails 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 a trace of any analytical s
46、teps and intermediate results (chromatograms, raw data and calculation details) that should be kept available in case of specific requirements (e.g. accreditation). BS EN 15407:2011EN 15407:2011 (E) 9 Annex A (normative) Guidelines - Characteristics of the laboratory sample for chemical analysis of
47、SRF The following requirements apply when preparing the laboratory sample for the chemical characterisation of SRF samples according to this European Standard. NOTE Equivalent requirements apply in all chemical test method specifications for SRF, i.e. this European Standard, EN 15408, EN 15410, EN 1
48、5411, CEN/TS 15412 and EN 15413. A maximum amount of laboratory sample of 10 kg and maximum particle size of 1 cm is established on the basis of number and type of parameters to be determined, sample representativeness and practical reasons for handling samples. In the Table A.1 the requirements are
49、 summarised both for single or grouped chemical parameters. Table A.1 Requirements for the laboratory sample for the analysis of SRF Parameter (single or group) Minimum laboratory sample amount (g) aShort term storage conditions before delivery to the lab Long term storage condition before delivery to the lab Container material C, H, N 100 In the same condition of SRF production refrigeration 4 C plastic bottle or bag Cl, S, Br, F 100 In the same condition of SRF production refrigeration 4 C
