1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 15105:2011Solid biofuels Determinationof the water soluble chloride,sodium and potassium contentCopyright European Committee for Standardization Provided by IHS under licen
2、se with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 15105:2011 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN 15105:2011. Itsupersedes DD CEN/TS 15105:2005 which is withdrawn.The UK participation in its preparatio
3、n was entrusted to TechnicalCommittee PTI/17, Solid biofuels.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI
4、2011ISBN 978 0 580 71233 3ICS 75.160.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 28 February 2011.Amendments issued since publicationDate Text affectedCopyri
5、ght European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 15105:2011EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15105 February 2011 ICS 75.160.10 Supersedes CEN/TS 15105:2005Engli
6、sh Version Solid biofuels - Determination of the water soluble chloride, sodium and potassium content Biocombustibles solides - Mthodes de dtermination de la teneur en chlorure, sodium et potassium solubles dans leau Feste Biobrennstoffe - Bestimmung des wasserlslichen Gehaltes an Chlorid, Natrium u
7、nd Kalium This European Standard was approved by CEN on 25 December 2010. 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-date lists and bibliogr
8、aphical 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 translation under the responsibi
9、lity 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, France, Germany, Greece,
10、 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 KOMITEE FR NORMUNG Management
11、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 15105:2011: ECopyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or net
12、working permitted without license from IHS-,-,-BS EN 15105:2011EN 15105:2011 (E) 2 Contents Page Foreword 3Introduction .41 Scope 52 Normative references 53 Terms and definitions .54 Principle 55 Reagents .66 Apparatus .67 Preparation of the test sample .68 Procedure .68.1 Extraction .68.2 Detection
13、 methods.78.2.1 General 78.2.2 Methods for the determination of chloride concentration.78.2.3 Methods for the determination of sodium and potassium concentration .78.3 Blank test 79 Calculation 810 Performance characteristics 811 Test report 8Annex A (informative) Performance data 9Bibliography . 11
14、Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 15105:2011EN 15105:2011 (E) 3 Foreword This document (EN 15105:2011) has been prepared by Technical Committee CEN/TC 335 “So
15、lid 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 August 2011, and conflicting national standards shall be withdrawn at the latest by August 2
16、011. This document supersedes CEN/TS 15105:2005. In the pre-normative project BIONORM I Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 15105:2011EN 15105:2011 (E) 6 NOTE B
17、e aware that when potentiometric titration with silver nitrate is used, any contents of water soluble bromide and iodide will be included in the determination. sodium and potassium: Flame Emission Spectroscopy (FES) or Flame Atomic Absorption Spectroscopy (FAAS) or Inductively Coupled Plasma Optical
18、 Emission Spectroscopy (ICP-OES). 5 Reagents Water, containing negligible amounts of chloride, sodium and potassium i.e. amounts that do not contribute significant to the determinations. Deionised water will normally fulfil this requirement. 6 Apparatus 6.1 Heating oven or autoclave, capable of bein
19、g maintained at a temperature of (120 5) C. 6.2 Vessel, made of fluoropolymer with a volume of about 100 ml and provided with a tight screw cap. The vessel and the cap shall be capable of withstanding at least 125 C at 232 kPa. If only the water soluble content of chloride is to be determined, an eq
20、uivalent Pyrex glass vessel can be used. 6.3 Balance, with a resolution of at least 1 mg. 6.4 General laboratory equipment as volumetric flasks and measuring cylinders. If sodium and potassium are to be determined, the use of glass equipments shall be avoided. 6.5 Membrane filtering apparatus, with
21、membrane filters of mean pore size 0,45 m. 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 FprEN 14780. If the results are to be calculated other than on an “as determined” basis, the moisture conten
22、t of the test sample shall be determined concurrently by the method described in EN 14774-3, using another portion of the test sample. 8 Procedure 8.1 Extraction a) Weigh, in an empty clean vessel (see 6.2), 1,0 g of the analysis sample to the nearest 1 mg. b) Add 50,0 ml water, swirl the content an
23、d close the vessel tight. c) Leave the closed vessel in a heating oven or an autoclave at 120 C for 60 min. d) Take the closed vessel out of the oven or the autoclave and let it cool to room temperature. WARNING Do not attempt to open the vessel before it is cool. e) Transfer the content of the vess
24、el to a 100 ml volumetric flask. Wash the inside of the vessel with small portions of water; add the washings to the volumetric flask and fill it to the 100 ml volume with water. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or n
25、etworking permitted without license from IHS-,-,-BS EN 15105:2011EN 15105:2011 (E) 7 f) Filter a portion of the solution (see e) through a membrane filter of pore size 0,45 m, discarding the first portion of the filtrate. Alternatively the filtering can be carried out using a syringe equipped with a
26、 0,45 m pore size filter tip. NOTE If only the water soluble content of chloride is to be determined, filtering may be omitted or a coarse folded filter paper may be used instead of the membrane filter. 8.2 Detection methods 8.2.1 General Complete the determination by measuring the concentration of
27、the elements in the prepared solution; for chloride by using one of the methods stated in 8.2.2 and for sodium and potassium by using one of the methods stated in 8.2.3. 8.2.2 Methods for the determination of chloride concentration For the determination of the chloride concentration one of the follo
28、wing methods shall be used: Ion-chromatographic determination according to the principles of EN ISO 10304-1; Potentiometric titration with silver nitrate according to Std. Meth. 4500-Cl-D 7 or equivalent national standards e.g. 3, 4 or 6. Other methods may be used, provided that it can be proved tha
29、t the obtained results are comparable to results obtained by determinations using one of the above stated methods, within the performance characteristics of these methods. 8.2.3 Methods for the determination of sodium and potassium concentration For the determination of the concentration of sodium a
30、nd potassium one of the following methods shall be used: ICP-OES according to the principles of EN ISO 11885; FAAS according to the principles of ISO 9964-1 and ISO 9964-2; FES according to the principles of ISO 9964-3. For the instrumental technique used, an initial control for eventual interferenc
31、es shall be performed using a standard addition method and/or a dilution method. Other methods may be used, provided that it can be proved that the obtained results are comparable to results obtained by determinations using one of the above stated methods, within the performance characteristics of t
32、hese methods. 8.3 Blank test Carry out a blank test, using the same procedure and methods as described in 8.1 and 8.2 but omitting the test portion. This assesses both the contents of the elements in the reagents and any contamination from equipments and in the laboratory atmosphere. This shall not
33、be quantitatively significant. The measured blank value has to be subtracted from the sample value. NOTE At high element level the blank should be less than 10 % of the sample content. For low element level (a content below 500 mg/kg in the sample), it is adequate that the contents of the elements i
34、n the blank solution are 30 % or less of the contents of the elements in the sample solution. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 15105:2011EN 15105:2011 (E) 8
35、9 Calculation The water soluble content of the element in the sample as analysed, wX, expressed in mg/kg is given by the equation: mVccwX=)(0where c is the concentration of the element (chloride, sodium or potassium), in mg/l, in the extract solution (see 8.1 e); c0is the concentration of the elemen
36、t (chloride, sodium or potassium), in mg/l, in the extract solution of the blank experiment (see 8.3); V is the volume, in ml, of the extract solution; m is the mass, in g, of the test portion used. Report the results as the mean of duplicate determinations. The results shall be calculated to a dry
37、basis or to an as received basis according to EN 15296. 10 Performance characteristics The achievable performance of the method is given in Annex A showing the results obtained by a European intercomparison study carried out for a sample of wood chips and a sample of an exhausted olive residue. Thes
38、e two samples represent the extremity of the method. The wood chip sample represents samples with low contents of water soluble chloride, sodium and potassium and the olive residue samples with high amounts of water soluble chloride and potassium. 11 Test report The test report shall include at leas
39、t the following information: a) Identification of the laboratory performing the test and the date of the test; b) Identification of product (or sample) tested; c) Reference to this European Standard (EN 15105); d) Method for the determination e) The results of the test including the basis in which t
40、hey are expressed, as indicated in Clause 9; f) Any unusual features noted during the determination; g) Any operation not included in this European Standard, or regarded as optional. Copyright European Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction
41、or networking permitted without license from IHS-,-,-BS EN 15105:2011EN 15105:2011 (E) 9 Annex A (informative) Performance data The round robin was carried out by laboratories in Austria, Belgium, Denmark, Finland, Germany, Ireland, Italy, the Netherlands, Spain, Sweden and the United Kingdom. The v
42、ariety of instruments and other analytical conditions were used in accordance with the quality parameters specified in the method. The tests were carried out using two samples, wood chips and exhausted olive residues produced in the EU-project BioNorm in 2008 in accordance with CEN/TS 14780. The sam
43、ple “wood chips” was made of German coniferous wood chips; the chips were dried and milled to 1 mm by means of cutting mill. The sample “exhausted olive residues” was obtained from olive oil industry in Spain from a typical outdoor storage facility. In the original sample stones and other natural im
44、purities were present. These impurities and stones were removed manually and the sample was prepared from the residues in two steps using a coarse cutting mill equipped with a 10 mm sieve and a laboratory cutting mill equipped with WC cutting tools and a 1 mm sieve. All data is reported on dry basis
45、. The performance data according to ISO 5725-2 1 are presented in Tables A.1, A.2 and A.3. NOTE 1 See Table A.1 for definition of the symbols used in Tables A.1 to A.3. NOTE 2 A guideline can be found in EN 15296 on how to use these validation parameters. Table A.1 Performance data for water soluble
46、 chloride Sample n l 0 x sRCVRsrCVr% mg/kg mg/kg % mg/kg % wood chips 7 35 15 26 13 45 5 19 exhausted olive residues 7 35 0 2 100 150 7,4 49 2,4 Definition symbols n is the number of laboratories after outlier elimination l is the number of outlier free individual analytical values o is the percenta
47、ge of outlying values from replicate determination x is the overall mean sRis the reproducibility standard deviation CVRis the coefficient of the variation of the reproducibility sris the repeatability standard deviation CVris the coefficient of the variation of the repeatability Copyright European
48、Committee for Standardization Provided by IHS under license with CENNot for ResaleNo reproduction or networking permitted without license from IHS-,-,-BS EN 15105:2011EN 15105:2011 (E) 10 Table A.2 Performance data for water soluble sodium Sample n l 0 x sRCVRsrCVr% mg/kg mg/kg % mg/kg % wood chips There is not enough data available exhausted olive residues 8 40 0 99 16 16 8 8,4 Table A.3 Performance data for water soluble potassium Sample n l 0 x sRCVRsrCVr% mg/kg mg/kg % mg/kg % wood chips 6 29 4,4
