1、November 2012 Translation by DIN-Sprachendienst.English price group 9No part of this translation 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).IC
2、S 13.030.01!$N“1922543www.din.deDDIN EN 15935Sludge, treated biowaste, soil and waste Determination of loss on ignition;English version EN 15935:2012,English translation of DIN EN 15935:2012-11Schlamm, behandelter Bioabfall, Boden und Abfall Bestimmung des Glhverlusts;Englische Fassung EN 15935:2012
3、,Englische bersetzung von DIN EN 15935:2012-11Boues, bio-dchets traits, sols et dchets Dtermination de la perte au feu;Version anglaise EN 15935:2012,Traduction anglaise de DIN EN 15935:2012-11www.beuth.deDocument comprises 15 pagesIn case of doubt, the German-language original shall be considered a
4、uthoritative.10.12 DIN EN 15935:2012-11 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 400 “Project Committee Horizontal standards in the fields of sludge, biowaste and soil” (Secretariat: DIN, Germany). The responsible German
5、 body involved in its preparation was the Normenausschuss Wasserwesen (Water Practice Standards Committee), Working Committee NA 119-01-02 Abfall- und BodenuntersuchungNA119-01-02-02 AA Chemische und physikalische Verfahren. , The DIN Standard corresponding to the International Standard referred to
6、in this document is as follows: ISO 5725-2 DIN ISO 5725-2 DIN EN 15935:2012-11 3 National Annex NA (informative) Bibliography DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a stan
7、dard measurement method DIN EN 15935:2012-11 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15935 August 2012 ICS 13.030.01 English Version Sludge, treated biowaste, soil and waste Determination of loss on ignition Boues, bio-dchets traits, sols et dchets Dte
8、rmination de la perte au feu Schlamm, behandelter Bioabfall, Boden und Abfall Bestimmung des Glhverlusts This European Standard was approved by CEN on 24 May 2012. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standa
9、rd the status of a national standard without any alteration. Up-to-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,
10、 French, German). A version in any other language made by translation 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, Bulg
11、aria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Tu
12、rkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN
13、 15935:2012: E EN 15935:2012 (E) 2 Contents PageForeword 3Introduction .41 Scope 52 Normative references 53 Terms and definitions .54 Principle 55 Interferences and sources of errors 56 Apparatus .67 Procedure .67.1 Samples with low content of volatiles .67.2 Samples containing volatile substances 7
14、8 Calculation and expression of results .79 Precision .810 Test report 8Annex A (informative) Repeatability and reproducibility data 9A.1 Materials used in the interlaboratory comparison study 9A.2 Interlaboratory comparison results 10Bibliography . 11DIN EN 15935:2012-11EN 15935:2012 (E) 3 Foreword
15、 This document (EN 15935:2012) has been prepared by Technical Committee CEN/TC 400 “Project Committee - Horizontal standards in the fields of sludge, biowaste and soil”, the secretariat of which is held by DIN. This European Standard shall be given the status of a national standard, either by public
16、ation of an identical text or by endorsement, at the latest by February 2013, and conflicting national standards shall be withdrawn at the latest by February 2013. 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
17、 shall not be held responsible for identifying any or all such patent rights. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association. The preparation of this document by CEN is based on a mandate by the European Commission (Man
18、date M/330), which assigned the development of standards on sampling and analytical methods for hygienic and biological parameters as well as inorganic and organic determinants, aiming to make these standards applicable to sludge, treated biowaste and soil as far as this is technically feasible. Acc
19、ording to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, German
20、y, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 15935:2012-11EN 15935:2012 (E) 4 Introduction This European Standard is applicable
21、and validated for several types of matrices as indicated in Table 1 (see also Annex A for the results of the validation). Table 1 Matrices for which this European Standard is applicable and validated Matrix Materials used for validation Sludge Municipal sludge Biowaste Compost, Fresh Compost Soil Sl
22、udge amended soil, Agricultural soil Waste Contaminated soil,Dredged sludge, Nickel sludge WARNING Persons using this European Standard should be familiar with usual laboratory practice. This European Standard does not purport to address all of the safety problems, if any, associated with its use. I
23、t is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. IMPORTANT It is absolutely essential that tests conducted according to this European Standard be carried out by suitably trained staff. Special m
24、easures shall be taken during the ignition process to prevent contamination of the laboratory atmosphere by flammable, explosive or toxic gases. DIN EN 15935:2012-11EN 15935:2012 (E) 5 1 Scope This European Standard specifies a method for the determination of the loss on ignition (LOI) of dry matter
25、 at 550 C. The dry matter is determined according to EN 15934. This method applies to the determination of loss on ignition of sludge, treated biowaste, soil and waste. The LOI of sediments can also be determined with this method. NOTE The loss on ignition is often used as an estimate for the conten
26、t of organic matter in the sample. Inorganic substances or decomposition products (e.g. H2O, CO2, SO2,O2) are released or absorbed and some inorganic substances are volatile under the reaction conditions. 2 Normative references The following documents, in whole or in part, are normatively referenced
27、 in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 15934, Sludge, treated biowaste, soil and waste Calculation of dry matter fr
28、action after determination of dry residue or water content 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 15934 and the following apply. 3.1 loss on ignition LOI mass fraction lost by burning up a dried sample to constant mass at a specified temperat
29、ure 3.2 residue on ignition mass fraction remaining after burning up a dried sample to constant mass at a specified temperature 4 Principle A weighed test portion is burned up in a furnace to constant mass at (550 25) C. The difference in mass before and after the ignition process is used to calcula
30、te the loss on ignition. The determination is performed on a dried sample or directly on the undried sample including a drying step or by referring to the dry matter. 5 Interferences and sources of errors LOI is an empirical parameter, thus in principle there is no interference connected to the dete
31、rmination. However, for some purposes the determination of LOI is used for the assessment of the content of organic matter in the sample. It should be noted that elementary carbon in the sample will be included in the loss on ignition value. Furthermore, any volatilisation or chemical reactions of i
32、norganic compounds will also be included in the loss on ignition value. Chemically bound water could be released during heating, thereby contributing to the loss on ignition. DIN EN 15935:2012-11EN 15935:2012 (E) 6 Samples containing iron or other metals in low bonding state or in metallic state cou
33、ld be oxidised during heating, thereby contributing to the loss on ignition with a negative amount. Sulfides present in the sample could be oxidised to sulfate during heating, thereby contributing to the loss on ignition with a negative amount. Explosive ignition is likely to result in loss of resid
34、ue from the crucible, thereby contributing to the loss on ignition. Calcium hydroxide or calcium oxide present in large amounts (e.g. sludge conditioned with lime) may combine with sulfuric oxides liberated during ignition or with carbon dioxide formed during ignition resulting in too low a content
35、of the loss on ignition. Such reactions can be avoided using the stepwise heating procedure stated in 7.1 combined with a sufficient ventilation rate in the furnace and a height of the sample layer in the crucible not exceeding 5 mm. 6 Apparatus 6.1 Crucible, preferably flat bottom type and typicall
36、y 50 mm to 70 mm in diameter, suitable for ignition at 550 C, e.g. made of nickel, platinum, porcelain, or silica. 6.2 Muffle furnace, or equivalent equipment, capable of maintaining a temperature of (550 25) C. 6.3 Metal plate, or comparable plate, suitable for the initial cooling of crucibles. 6.4
37、 Desiccator, with an active drying agent, such as silica gel. 6.5 Precision balance, with an accuracy of at least 1 mg. 7 Procedure 7.1 Samples with low content of volatiles If the determination of dry matter fraction and the determination of loss on ignition are carried out in successive operations
38、 in the same crucible refer to EN 15934 for the initial crucible weighing. If the determinations are performed as separate operations, representative portions of the sample shall be used for the determination of loss on ignition and dry matter fraction according to EN 15934. Alternatively the sample
39、 material may be dried according to EN 15934 before the determination of the loss on ignition. Every necessary precaution shall be taken to avoid absorption of atmospheric humidity by the sample until weighed. Place a crucible (6.1) in the furnace (6.2) and heat to (550 25) C for at least 30 min. Tr
40、ansfer the crucible from the furnace after initial cooling on a metal plate (6.3) to a desiccator (6.4) and finish cooling to ambient temperature. Weigh the empty crucible using a precision balance (6.5) to the nearest 1 mg. Weigh into the crucible 0,5 g to 5 g of the test portion to the nearest 1 m
41、g, and place the crucible into the furnace. Raise the furnace temperature to (550 25) C and hold this temperature for at least 2 h. The sample layer in the crucible should not exceed a height of 5 mm. If the test portion has high organic matter content, losses may occur as a result of rapid ignition
42、 or deflagration of the sample. In this case heat the sample slowly until ignition. For certain wastes (e.g. paper wastes and demolition wood) a step-wise heating process can be used: the crucible is inserted in a cold furnace; the temperature is raised slowly to 250 C over a period of 50 min, allow
43、ing pyrolysis of the sample. Then the temperature is raised slowly to 550 C and the 550 C is kept for at least 2 h. If the sample contains higher amounts of moisture, insert the crucible in a cold furnace and raise the furnace temperature evenly to (550 25) C over a period of 1 h and hold this tempe
44、rature for at least 2 h. DIN EN 15935:2012-11EN 15935:2012 (E) 7 Place the hot crucible containing the residue on ignition on a metal plate (6.3) for a few minutes. While still warm, transfer the crucible to a desiccator (6.4) and leave to cool to ambient temperature. As soon as ambient temperature
45、is reached, weigh the crucible containing the ignition residue to the nearest 1 mg. If black carbon particles are still present (some organic substances burn slowly at 550 C), moisten the residue using a few drops of an ammonium nitrate solution. Insert the crucible into the furnace and slowly heat
46、to avoid losses by the steam development and continue heating the residue at (550 25) C. Ammonium nitrate solution is prepared by dissolving 10 g of reagent grade ammonium nitrate, NH4NO3, in 100 ml distilled water. 7.2 Samples containing volatile substances For samples containing significant amount
47、s of volatile substances the dry matter cannot be determined as dry residue. In this case the dry matter shall be calculated from the water content according to EN 15934 method B, and the loss on ignition is always performed directly on the undried sample. Place a crucible (6.1) in the furnace (6.2)
48、 and heat at (550 25) C for at least 30 min. Transfer the crucible from the furnace after initial cooling on a metal plate (6.3) to a desiccator (6.4) and finish cooling to ambient temperature. Weigh the empty crucible using a precision balance (6.5) to the nearest 1 mg. Weigh into the crucible 0,5 g to 5 g of the test portion to the nearest 1 mg. Larger masses may be taken if complete combustion can be assured. All necessary precautions should be taken to avoid l
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