1、BS EN 15170:2008ICS 13.030.20NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDCharacterization of sludges Determination of calorific valueIncorporating corrigendum September 2009This British Standard was published under the authority of the Standards Policy and S
2、trategy Committee on 30 June 2009. BSI 2009ISBN 978 0 580 69205 5Amendments/corrigenda issued since publicationDate CommentsBS EN 15170:2008National forewordThis British Standard is the UK implementation of EN 15170:2008.BSI, as a member of CEN, is obliged to publish EN 15170 as a British standard.
3、However, attention is drawn to the fact that during the development of this European Standard, the UK committee voted against its approval as a European Standard.Determination of calorific value has been standardized for many other materials, such as coal and oil. In the opinion of the UK committee,
4、 in this standard, it should only be necessary to refer to exceptional analytical problems that apply specifically to sludges.This standard sets out how the two types of calorimeter (static jacket and adiabatic) are assembled, operated and calibrated and the method for correcting for heat loss in on
5、e type. In the opinion of the UK committee this is not necessary because such theory and practice are contained in the operating instructions for the equipment, almost without exception.The UK committee believes that information on the different types of equipment that can be used, the standard for
6、calibration (but not the precise method of application as this is equipment dependent)and the potential for errors can be found in such British Standards as BS 1016-105:1992 and BS 7420:1991, as well as in guides produced by the oil companies. Without exception, the reference material for calibratio
7、n is benzoic acid, because it can be dried to a water content of 0.01%, is chemically stable and is not prone to bacterial attack. It has also been subject to assessment for at least 60 years. The UK participation in its preparation was entrusted to TechnicalCommittee EH/5, Sludge characterization.A
8、 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 cannot confer immunityfrom leg
9、al obligations.30 September 2009 Correction to national forewordBS EN 15170:2008EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15170November 2008ICS 13.030.40English VersionCharacterization of sludges - Determination of calorific valueCaractrisation des boues - Dtermination du pouvoircalorifiqueC
10、harakterisierung von Schlmmen - Bestimmung desBrenn- und HeizwertesThis European Standard was approved by CEN on 11 October 2008.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard
11、 without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other langu
12、age made by translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,F
13、rance, 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 STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR
14、NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2008 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15170:2008: EBS EN 15170:2008EN 15170:2008 (E) 2 Contents Page Foreword3 Introduction .4 1 Scope 5 2 Normative referen
15、ces 5 3 Terms and definitions .5 4 Principle6 5 Reagents.6 6 Apparatus .7 7 Procedure .9 8 Calibration 13 9 Gross calorific value .14 10 Calculation of net calorific value15 11 Precision.17 12 Test report 17 Annex A (informative) Example of a calorimeter18 Annex B (informative) Temperature evolution
16、 .19 Annex C (informative) Results of the interlaboratory comparison 20 Bibliography 21 BS EN 15170:2008EN 15170:2008 (E) 3 Foreword This document (EN 15170:2008) has been prepared by Technical Committee CEN/TC 308 “Characterization of sludges”, the secretariat of which is held by AFNOR. This Europe
17、an 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 2009, and conflicting national standards shall be withdrawn at the latest by May 2009. Attention is drawn to the possibility that some of the elements of t
18、his 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. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European St
19、andard: 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, Switzerland and the United Kingdo
20、m. BS EN 15170:2008EN 15170:2008 (E) 4 Introduction This method is a simple way to evaluate the amenability of sludge and sludge products to be treated by thermal processes. In this European Standard some thermo-chemical corrections are not considered. For detailed descriptions of analytical procedu
21、res and theoretical background see ISO 1928 or CEN/TS 14918. The result obtained is the gross calorific value of the sample at constant volume with both the water of the combustion products and the moisture of the sludge as liquid water. The net calorific value can be obtained by calculation from th
22、e gross calorific value. For this either the hydrogen content of the sludge or the amount of water found in the combustion test has to be determined. Sludges usually contain much water and (un-burnable) solids. Therefore their calorific value especially on the “as received” basis is quite low. For m
23、any purposes it may be sufficient to determine the gross calorific value only, and not the net calorific value for which additional determinations are necessary. The calculation of the net calorific value at constant volume is described here only, for calculation at constant pressure refer to either
24、 ISO 1928 or CEN/TS 14918. BS EN 15170:2008EN 15170:2008 (E) 5 1 Scope This European Standard specifies a method for the determination of the gross calorific value of sludge at constant volume and at the reference temperature 25 C in a bomb calorimeter calibrated by combustion of certified benzoic a
25、cid. The result obtained is the gross calorific value of the sample at constant volume with both the water of the combustion products and the moisture of the sludge as liquid water. In practice, sludges are burned at constant (atmospheric) pressure and the water is not condensed but is removed as va
26、pour with the flue gases. Under these conditions, the operative heat of combustion to be used is the net calorific value of the fuel at constant pressure. In this European Standard the net calorific value at constant volume is described as it requires less additional determinations. This method is a
27、pplicable to all kinds of sludges. 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)
28、applies. EN 12832:1999, Characterization of sludges Utilization and disposal of sludges Vocabulary EN 12880, Characterization of sludges Determination of dry residue and water content EN ISO 16720, Soil quality Pretreatment of samples by freeze-drying for subsequent analysis (ISO 16720:2005) ISO 651
29、, Solid-stem calorimeter thermometers ISO 652, Enclosed-scale calorimeter thermometers ISO 1770, Solid-stem general purpose thermometers ISO 1771, Enclosed-scale general purpose thermometers ISO/TS 12902, Solid mineral fuels Determination of total carbon, hydrogen and nitrogen Instrumental methods 3
30、 Terms and definitions For the purposes of this document, the terms and definitions given in EN 12832:1999 and the following apply. 3.1 gross calorific value (at constant volume) absolute value of the specific energy of combustion, in Joules, for unit mass of a solid sludge burned in oxygen in a cal
31、orimetric bomb under the conditions specified. The products of combustion are assumed to consist of gaseous oxygen, nitrogen, carbon dioxide and sulfur dioxide, of liquid water (in equilibrium with its vapour) saturated with carbon dioxide under the conditions of the bomb reaction, and of solid ash,
32、 all at the reference temperature 3.2 net calorific value (at constant volume) absolute value of the specific energy of combustion, in Joules, for unit mass of a solid sludge burned in oxygen under conditions of constant volume and such that all the water of the reaction products remains as BS EN 15
33、170:2008EN 15170:2008 (E) 6 water vapour (in a hypothetical state at 0,1 MPa), the other products being as for the gross calorific value, all at the reference temperature 3.3 net calorific value (at constant pressure) absolute value of the specific energy of combustion, in Joules, for unit mass of a
34、 solid sludge burned in oxygen at constant pressure under such conditions that all the water of the reaction products remains as water vapour (in a hypothetical state at 0,1 MPa), the other products being as for the gross calorific value, all at the reference temperature 3.4 corrected temperature ri
35、se change in calorimeter temperature caused solely by the processes taking place within the combustion bomb. It is the total observed temperature rise corrected for heat exchange, stirring power etc. 4 Principle 4.1 Gross calorific value A weighed portion of the analysis sample of the solid sludge i
36、s burned in high-pressure oxygen in a bomb calorimeter under specified conditions. The effective heat capacity of the calorimeter is determined in calibration experiments by combustion of certified benzoic acid under similar conditions, accounted for in the certificate. The corrected temperature ris
37、e is established from observations of temperature before, during and after the combustion reaction takes place. The duration and frequency of the temperature observations depend on the type of calorimeter used. Water is added to the bomb initially to give a saturated vapour phase prior to combustion
38、, thereby allowing all the water formed, from the hydrogen and moisture in the sample, to be regarded as liquid water. The gross calorific value is calculated from the corrected temperature rise and the effective heat capacity of the calorimeter, with allowances made for contributions from ignition
39、energy, combustion of the fuse(s) and for thermal effects from side reactions such as the formation of nitric acid. Furthermore, a correction is applied to account for the difference in energy between the aqueous sulfuric acid formed in the bomb reaction and gaseous sulfur dioxide, i. e. the require
40、d reaction product of sulfur in the sludge. The corresponding energy effect between aqueous and gaseous hydrochloric acid can be neglected due to the usually low chlorine content of most sludges. 4.2 Net calorific value The net calorific value at constant volume of the sludge is obtained by calculat
41、ion from the gross calorific value at constant volume determined on the analysis sample. The calculation of the net calorific value at constant volume requires information about the moisture and hydrogen contents of the analysis sample. In principle, the calculation of the net calorific value at con
42、stant pressure also requires information about the oxygen and nitrogen contents of the sample. NOTE The main difference between the gross and net calorific values is related to the physical state of water in the reaction products. 5 Reagents 5.1 Oxygen, at a pressure high enough to fill the bomb to
43、3 MPa, pure with an assay of at least 99,5 % (V/V), and free from combustible matter. NOTE Oxygen made by the electrolytic process may contain up to 4 % (V/V) of hydrogen. BS EN 15170:2008EN 15170:2008 (E) 7 5.2 Fuse 5.2.1 Ignition wire, of nickel-chromium 0,16 mm to 0,20 mm in diameter, platinum 0,
44、05 mm to 0,10 mm in diameter, or another suitable conducting wire with well-characterized thermal behaviour during combustion. 5.2.2 Cotton fuse, of white cellulose cotton, or equivalent, if required. It is necessary to use a fuse with the same length and sections both in the calibration step and in
45、 the measurements. 5.3 Combustion aids of known gross calorific value, composition and purity, like benzoic acid, n-dodecane, paraffin oil, combustion bags or capsules may be used. 5.4 Benzoic acid, of calorimetric-standard quality, certified by (or with certification unambiguously traceable to) a r
46、ecognized standardizing authority. The benzoic acid is burned in the form of pellets. It is normally used without drying or any treatment other than pelletizing; consult the sample certificate. 6 Apparatus 6.1 General The calorimeter (see a typical example in Annex A), consists of the assembled comb
47、ustion bomb, the calorimeter can (with or without a lid), the calorimeter stirrer, water, temperature sensor, and leads with connectors inside the calorimeter can required for ignition of the sample or as part of temperature measurement or control circuits. During measurements the calorimeter is enc
48、losed in a thermostat. The manner in which the thermostat temperature is controlled defines the working principle of the instrument and hence the strategy for evaluation of the corrected temperature rise. In combustion calorimetric instruments with a high degree of automation, especially in the eval
49、uation of the results, the calorimeter is in a few cases not as well-defined as the traditional, classical-type calorimeter. Using such an automated calorimeter is, however, within the scope of this European Standard as long as the basic requirements are met with respect to calibration conditions, comparability between calibration and fuel experiments, ratio of sample mass to bomb volume, oxygen pressure, bomb liquid, reference temperature of the measurements and repeatability of the results. A print-out of some specified parameters from the individual measurem
