1、May 2009DEUTSCHE NORM English price group 13No part of this standard 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 13.030.20; 13.030.40!$Wk4“
2、1527217www.din.deDDIN EN 15170Characterization of sludges Determination of calorific valueEnglish version of DIN EN 15170:2009-05Charakterisierung von Schlmmen Bestimmung des Brenn- und HeizwertesEnglische Fassung DIN EN 15170:2009-05www.beuth.deDocument comprises 23 pagesDIN EN 15170:2009-05 2 Nati
3、onal foreword This standard has been prepared by Technical Committee CEN/TC 308 “Characterization of sludges” (Secretariat: AFNOR, France), Working Group WG 1 “Characterization methods”. The responsible German body involved in its preparation was the Normenausschuss Wasserwesen (Water Practice Stand
4、ards Committee), Technical Committee NA 119-01-02 AA Abfall- und Bodenuntersuchung. The national standards bodies listed in the foreword are bound to adopt this European Standard in its entirety and without any modifications. The only difference between the two types of calorific value referred to h
5、ere is the physical state of the water in the reaction products. In the English-language version of this standard, the two parameters “gross calorific value” and “net calorific value” are indicated by the indices “gr” and “net”, respectively. Because these values are sometimes translated into German
6、 as “oberer Heizwert” (with the index “o”) and “unterer Heizwert” (with the index “u”), respectively, these indices have been used in the German version of EN 15170 and not the English indices. In general practice, however, “gross calorific value” is called the Brennwert and the “net calorific value
7、” is called the Heizwert in German; these terms are therefore used in the German text of EN 15170. The calorific values can be given on the basis of various reference conditions referring to different water contents (and therefore can only represent operands). In the German version of EN 15170 the G
8、erman terms are used. Table NA.1 gives an overview of the English terms and the respective German terms, and their indices. The indices are listed in the order given in German standards on fuels. Table NA.1 Comparison of German and English indices German term German index English index English term
9、oberer (Heizwert) OR Brennwert o gr gross (calorific value) unterer (Heizwert) OR Heizwert u net net (calorific value) wasserfrei wf d dry analysenfeucht (also: lufttrocken) an ad as analysed (also: air-dried) roharoh ar as received aA fuel or sludge is referred to as being “roh” at the time of samp
10、ling. In the German version of EN 15170, the German indices are used in equations (6) to (11). The DIN Standard corresponding to the International Standard referred to in this document is as follows: ISO 5725-1 DIN ISO 5725-1 National Annex NA (informative) Bibliography DIN ISO 5725-1, Accuracy (tru
11、eness and precision) of measurement methods and results Part 1: General principles and definitions EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15170November 2008ICS 13.030.40English VersionCharacterization of sludges - Determination of calorific valueCaractrisation des boues - Dtermination du
12、pouvoircalorifiqueCharakterisierung 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
13、a national standard 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
14、 in any other language 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,
15、 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 Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEURO
16、PISCHES KOMITEE FR 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: EEN 15170:2008 (E) 2 Contents Page Foreword3 Introduction .4 1 Scope 5 2 Normative refe
17、rences 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 evolut
18、ion .19 Annex C (informative) Results of the interlaboratory comparison 20 Bibliography 21 DIN EN 15170:2009-05 EN 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. Thi
19、s 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 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 eleme
20、nts 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. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this Eur
21、opean Standard: 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 Unite
22、d Kingdom. DIN EN 15170:2009-05 EN 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 analy
23、tical procedures 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 calcul
24、ation from the 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 qui
25、te low. For many 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 re
26、fer to either ISO 1928 or CEN/TS 14918. DIN EN 15170:2009-05 EN 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 c
27、ertified benzoic acid. 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 bu
28、t is removed as vapour 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
29、. This method is applicable 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 (includin
30、g any amendments) 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 1
31、6720:2005) ISO 651, 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 Inst
32、rumental methods 3 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
33、in oxygen in a calorimetric 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,
34、 and of solid ash, 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 r
35、emains as DIN EN 15170:2009-05 EN 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 Jou
36、les, for unit mass of a 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 c
37、orrected temperature rise 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 sampl
38、e of the solid sludge is 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 co
39、rrected temperature rise 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 ph
40、ase prior to combustion, 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 contr
41、ibutions from ignition 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 dio
42、xide, i. e. the required 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
43、is obtained by calculation 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
44、 calorific value at constant 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 enou
45、gh to fill the bomb to 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. DIN EN 15170:2009-05 EN 15170:2008 (E) 7 5.2 Fuse 5.2.1 Ignition wire, of nickel-chromium 0,16 mm to 0,20
46、 mm in diameter, platinum 0,05 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
47、 the calibration step and in 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 una
48、mbiguously traceable to) a recognized 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), co
49、nsists of the assembled combustion 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 enclosed 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
