1、BS EN 15169:2007ICS 13.030.40NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDCharacterization ofwaste Determinationof loss on ignitionin waste, sludge andsedimentsThis British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee
2、on 30 June2009. BSI 2009ISBN 978 0 580 55086 7Amendments/corrigenda issued since publicationDate CommentsBS EN 15169:2007National forewordThis British Standard is the UK implementation of EN 15169:2007.The UK participation in its preparation was entrusted to TechnicalCommittee B/508/3, Characterizat
3、ion of waste.A 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 imm
4、unityfrom legal obligations.BS EN 15169:2007EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15169February 2007ICS 13.030.40English VersionCharacterization of waste - Determination of loss on ignition inwaste, sludge and sedimentsCaractrisation des dchets - Dtermination de la perte aufeu des dchets
5、, des boues et des sdimentsCharakterisierung von Abfall - Bestimmung desGlhverlustes in Abfall, Schlamm und SedimentenThis European Standard was approved by CEN on 13 January 2007.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
6、 EuropeanStandard the status of 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 (Eng
7、lish, French, German). A version 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,
8、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 Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCO
9、MIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2007 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15169:2007: EBS EN 15169:2007EN 15169:2007 (E) 2 Contents Page Fore
10、word3 1 Scope 4 2 Normative references 4 3 Terms and definitions .4 4 Principle5 5 Interference 5 6 Hazards .5 7 Sample preservation and preparation .5 8 Apparatus .6 9 Procedure .6 10 Expression of results 8 11 Performance characteristics 9 12 Test report 9 Annex A (informative) Summary of general
11、requirements and recommendations .10 Annex B (informative) Additional validation data 11 B.1 General11 B.2 Type of samples and sample preparation.11 B.3 Homogeneity and stability 11 B.4 Validation data for sludge from EN 12879.12 Bibliography 13 BS EN 15169:2007EN 15169:2007 (E) 3 Foreword This docu
12、ment (EN 15169:2007) has been prepared by Technical Committee CEN/TC 292 “Characterization of waste”, the secretariat of which is held by NEN. 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 Augus
13、t 2007, and conflicting national standards shall be withdrawn at the latest by August 2007. The method described in this standard has been derived from EN 12879 which was prepared by CEN/TC 308. Anyone dealing with waste and sludge analysis should be aware of the risks of that kind of material, irre
14、spective of the parameters to be determined. Waste and sludge samples may contain hazardous (e. g. toxic, reactive, flammable, infectious) substances, which can be prone to biological and/or chemical reaction. Consequently these samples should be handled with special care. Gases which may be produce
15、d by microbiological or chemical activity are potentially flammable and will pressurise sealed bottles. Bursting bottles are likely to result in hazardous shrapnel, dust and/or aerosol. National regulations should be followed with respect to all hazards associated with this method. According to the
16、CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania
17、, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. BS EN 15169:2007EN 15169:2007 (E) 4 1 Scope This European Standard specifies a method for the determination of the loss on ignition. This procedure is applicable to
18、 all kinds of waste, sludge and sediments. The loss on ignition is often used as an estimate for the content of non-volatile organic matter in waste, sludge and sediments. It should be noted that any content of elementary carbon and volatilisation of organic materials or chemical reactions by inorga
19、nic compounds, is included in the loss on ignition. 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
20、 any amendments) applies. EN 14346, Characterisation of waste Calculation of dry matter by determination of dry residue or water content 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 loss on ignition change in mass as a result of heating a
21、sample under specified conditions. The loss on ignition is expressed in weight percent of the dry matter 3.2 residue on ignition mass remaining after heating a sample under specified conditions. The residue on ignition is expressed in weight percent of the dry matter 3.3 dry residue wdrremaining mas
22、s fraction of a sample after a drying process at 105 C, as specified in EN 14346 3.4 water content wwmass fraction of water in a sample determined by Karl-Fischer titration, as specified in EN 14346 3.5 dry matter wdmmass fraction of a sample excluding water expressed as a percentage by mass, calcul
23、ated by determination of dry residue or water content according to EN 14346 3.6 constant mass constant mass is obtained when the change in mass during a further period of heating of 1 h is within 0,5 % (m/m) or 2 mg, whatever is greater BS EN 15169:2007EN 15169:2007 (E) 5 4 Principle A test portion
24、is heated in a furnace up to (550 25) C. The difference in mass before and after the heating process is used to calculate the loss on ignition. The determination is performed on a beforehand dried sample following EN 14346 or directly on the undried sample including a drying step or by referring to
25、the dry matter. 5 Interference In principle there are no interferences connected to the determination, as the loss on ignition is an empirical parameter. However, for many purposes the determination is used for assessing the content of organic matter in waste, sludge or sediment samples. It should b
26、e noted that any elementary carbon in the sample will be included in the loss on ignition value. Furthermore, any volatilisation or chemical reactions of inorganic compounds will also be included in the loss of ignition value. NOTE 1 Chemically bound water or volatile metals (e. g. in hydroxides fro
27、m flue gas cleaning processes) could be released during heating, contributing to the loss on ignition with a positive amount. NOTE 2 Iron or other metals present in the sample in the metallic state could be oxidised during heating, contributing to the loss on ignition with a negative amount. NOTE 3
28、Sulphides present in the sample could be oxidised to sulphate during heating, contributing to the loss on ignition with a negative amount. 6 Hazards It is advised not to store samples in the open laboratory. If samples are to be stored, this has to be done in a well ventilated place. 7 Sample preser
29、vation and preparation 7.1 Preservation When not analysed immediately samples should be stored in tight containers. For biologically inactive samples special preservation may not be necessary. Biologically active samples may need to have the lids loosened to prevent build-up of gas pressure. If samp
30、les are known to be biologically active they should be made inactive e. g. by freezing or air drying. BS EN 15169:2007EN 15169:2007 (E) 6 7.2 Preparation The samples supplied for analysis should be as homogeneous as possible. Depending on the nature and appearance of the sample, different procedures
31、 can be used according EN 15002, e. g. a) Solid samples may be directly comminuted (avoiding heat) and reduced to a granular powder, preferably a particle size less than 200 m. If no volatiles are present samples may be air-dried prior to comminuting. The drying temperature shall not exceed 40 C. b)
32、 Moist or pasty-like samples may be mixed with aluminium oxide until a granular material is obtained and then comminuted, preferably a particle size less than 200 m. In this case the ratio of aluminium oxide to sample shall be considered in the calculation of the loss on ignition. c) Liquid samples
33、shall be homogenized immediately prior to weighing. Foreign bodies or non comminutable material (e. g. metallic parts such as nuts, bolts, scrap) should be separated from the sample and the weight and nature of the material be recorded. 8 Apparatus 8.1 Flat bottom crucible, typically 50 mm to 70 mm
34、in diameter, suitable for heating to 550 C e. g. made of porcelain, silica, nickel or platinum. 8.2 Muffle furnace or equivalent equipment, capable of maintaining a temperature of (550 25) C. 8.3 Desiccator, containing a desiccant. 8.4 Analytical balance with an accuracy of 1 mg or better. 8.5 Metal
35、 plate. 9 Procedure 9.1 Samples not containing volatiles The determination of loss on ignition and the determination of dry matter are performed as separate operations on different portions of the same sample. For some materials, however, it is convenient to carry out the determination of both dry r
36、esidue and loss on ignition in successive operations in the same crucible. Procedure for dry residue see EN 14346. In all cases necessary precautions should be taken to avoid absorption of atmospheric humidity by the sample until it is weighed. Prepare a crucible (8.1) by placing it in the furnace (
37、8.2) and heat at (550 25) C for at least 20 min. Transfer the crucible from the furnace (8.2) after initial cooling on a metal plate (8.5) to a desiccator (8.3) and finish cooling to ambient temperature. Weigh the empty crucible to constant mass to the nearest 1 mg (m(a) on an analytical balance (8.
38、4). Transfer 0,5 g to 5 g of the sample to the crucible and weigh to the nearest 1 mg (m(b). Larger masses may be taken if appropriate. NOTE 1 Masses larger than 5 g should not be used, unless it has been proven that a complete combustion of the actual sample material can be obtained at a higher loa
39、ding. BS EN 15169:2007EN 15169:2007 (E) 7 If the determination of loss on ignition and determination of dry matter are performed in successive operations, weigh the crucible with the dried sample to the nearest 1 mg (m(d). Insert the crucible into the furnace (8.2) and heat at (550 25) C for at leas
40、t 1 h. NOTE 2 If the dry matter is of high organic content, losses may occur as a result of rapid ignition or deflagration of the sample. In this case heat the sample slowly. Remove the hot crucible from the furnace (8.2) and allow cooling on a clean metal plate (8.5) for a few min. While still warm
41、, transfer the crucible to a desiccator (8.3) and finish cooling to ambient temperature. Weigh the crucible containing the ignition residue to the nearest 1 mg (m(c) as soon as ambient temperature is reached. Ignition can be regarded as complete when a constant mass is obtained. If even after a thir
42、d heating at (550 25) C constant mass is not obtained, record the value determined as the last measurement. This shall be recorded along with the result. NOTE 3 If black carbon particles are still present (some organic substances burn slowly at 550 C), wet the residue using a few drops of ammonium n
43、itrate solution. After repeated drying insert the crucible into the furnace and slowly heat to avoid losses by deflagration and continue heating the residue to (550 25) C. Ammonium nitrate solution is prepared by dissolving 10 g of reagent grade ammonium nitrate, NH4NO3, in 100 ml of demineralised w
44、ater. 9.2 Samples containing volatiles For samples containing significant amounts of volatile components dry matter can not be determined as dry residue. In this case the dry matter is calculated from the water content. For procedure see EN 14346. In this case the loss on ignition is always performe
45、d directly on the undried sample. Prepare a crucible (8.1) by placing it in the furnace (8.2) and heat to (550 25) C for at least 20 min. Transfer the crucible from the furnace (8.2) after initial cooling on a metal plate (8.5) to a desiccator (8.3) and finish cooling to ambient temperature. Weigh t
46、he empty crucible to constant mass to the nearest 1 mg (m(a) on an analytical balance (8.4). Transfer 0,5 g to 5 g of the sample to the crucible and weigh to the nearest 1 mg (m(b). Larger masses may be taken if appropriate. All necessary precautions should be taken to avoid loss of volatiles from t
47、he sample until it is weighed. NOTE 1 Masses larger than 5 g should not be used unless it has been proven that a complete combustion of the actual sample material can be obtained at a higher loading. NOTE 2 To avoid splashing from escaping vapours or sudden fire it is recommended to carefully remove
48、 most of the volatile components from the sample into a drying oven or at ambient temperature into a fume hood prior to ignition. NOTE 3 Samples of highly flammable waste e. g. solvents or waste oil should be ignited in the crucible and allowed to burn in a fume hood before being inserted into the f
49、urnace. When ready the crucible is inserted into a cold furnace (8.2) and heated to temperature for 1 h. Remove the hot crucible from the furnace (8.2) and allow it to cool on a clean metal plate (8.5) for a few minutes. While still warm, transfer the crucible to a desiccator (8.3) and finish cooling to ambient temperature. Weigh the crucible containing the ignition residue to the nearest 1 mg (m(c) as soon as ambient temperature is reached. Ignition is complete when constant mass is obtained. In cases when even after a third heating at (55
