1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 15935:2012Sludge, treated biowaste, soiland waste Determination ofloss on ignitionBS EN 15935:2012 BRITISH STANDARDNational forewordThis British Standard is the UK implemen
2、tation of EN 15935:2012. The UK participation in its preparation was entrusted to TechnicalCommittee H/-/4, Environmental testing programmes.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessar
3、y provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2012. Published by BSI Standards Limited 2012ISBN 978 0 580 70594 6 ICS 13.030.01; 13.080.05 Compliance with a British Standard cannot confer immunity from legal obligations.This British
4、Standard was published under the authority of the Standards Policy and Strategy Committee on 30 September 2012.Amendments issued since publicationDate T e x t a f f e c t e dBS EN 15935:2012EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15935 August 2012 ICS 13.030.01 English Version Sludge, t
5、reated biowaste, soil and waste - Determination of loss on ignition Boues, bio-dchets traits, sols et dchets - Dtermination 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 boun
6、d 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 bibliographical references concerning such national standards may be obtained on application to the CE
7、N-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 responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre h
8、as 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, L
9、uxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2012
10、CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15935:2012: EBS EN 15935:2012EN 15935:2012 (E) 2 Contents Page Foreword 3Introduction .41 Scope 52 Normative references 53 Terms and definitions .54 Principle 55 Interferences and sou
11、rces of errors 56 Apparatus .67 Procedure .67.1 Samples with low content of volatiles .67.2 Samples containing volatile substances 78 Calculation and expression of results .79 Precision .810 Test report 8Annex A (informative) Repeatability and reproducibility data 9A.1 Materials used in the interlab
12、oratory comparison study 9A.2 Interlaboratory comparison results 10Bibliography . 11BS EN 15935:2012EN 15935:2012 (E) 3 Foreword 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”, th
13、e secretariat of which is held by DIN. 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 February 2013, and conflicting national standards shall be withdrawn at the latest by February 2013. Attentio
14、n is drawn to the possibility that some of the elements 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. This document has been prepared under a mandate given to CEN by the European Commission and th
15、e European Free Trade Association. The preparation of this document by CEN is based on a mandate by the European Commission (Mandate M/330), which assigned the development of standards on sampling and analytical methods for hygienic and biological parameters as well as inorganic and organic determin
16、ants, aiming to make these standards applicable to sludge, treated biowaste and soil as far as this is technically feasible. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belg
17、ium, Bulgaria, 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, Switze
18、rland, Turkey and the United Kingdom. BS EN 15935:2012EN 15935:2012 (E) 4 Introduction This European Standard is applicable 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 a
19、pplicable and validated Matrix Materials used for validation Sludge Municipal sludge Biowaste Compost, Fresh Compost Soil Sludge amended soil, Agricultural soil Waste Contaminated soil,Dredged sludge, Nickel sludge WARNING Persons using this European Standard should be familiar with usual laboratory
20、 practice. This European Standard does not purport to address all of the safety problems, if any, associated with its use. It 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 absol
21、utely essential that tests conducted according to this European Standard be carried out by suitably trained staff. Special measures shall be taken during the ignition process to prevent contamination of the laboratory atmosphere by flammable, explosive or toxic gases. BS EN 15935:2012EN 15935:2012 (
22、E) 5 1 Scope This European Standard specifies a method for the determination of the loss on ignition (LOI) of dry matter 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
23、sediments can also be determined with this method. NOTE The loss on ignition is often used as an estimate for the content 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
24、the reaction conditions. 2 Normative references The following documents, in whole or in part, are normatively referenced 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 docu
25、ment (including any amendments) applies. EN 15934, Sludge, treated biowaste, soil and waste Calculation of dry matter fraction 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
26、apply. 3.1 loss on ignition LOI mass fraction lost by burning up a dried sample to constant mass at a specified temperature 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
27、 furnace to constant mass at (550 25) C. The difference in mass before and after the ignition process is used to calculate 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 Interferenc
28、es and sources of errors LOI is an empirical parameter, thus in principle there is no interference connected to the determination. 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
29、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 on ignition value. Chemically bound water could be released during heating, thereby contributing to the loss on ignition. BS EN
30、 15935:2012EN 15935:2012 (E) 6 Samples containing iron or other metals in low bonding state or in metallic state could 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
31、contributing to the loss on ignition with a negative amount. Explosive ignition is likely to result in loss of residue 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 sul
32、furic oxides liberated during ignition or with carbon dioxide formed during ignition resulting in too low a content 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
33、 sample layer in the crucible not exceeding 5 mm. 6 Apparatus 6.1 Crucible, preferably flat bottom type and typically 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
34、 temperature of (550 25) C. 6.3 Metal plate, or comparable plate, suitable for the initial cooling of crucibles. 6.4 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 det
35、ermination of dry matter fraction and the determination of loss on ignition are carried out in successive operations 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 us
36、ed for the determination of loss on ignition and dry matter fraction according to EN 15934. Alternatively the sample 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
37、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. 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 prec
38、ision 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, 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
39、 height of 5 mm. If the test portion has high organic matter content, losses may occur as a result of rapid ignition 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:
40、the crucible is inserted in a cold furnace; the temperature is raised slowly to 250 C over a period of 50 min, allowing 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 crucib
41、le in a cold furnace and raise the furnace temperature evenly to (550 25) C over a period of 1 h and hold this temperature for at least 2 h. BS EN 15935:2012EN 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, trans
42、fer the crucible to a desiccator (6.4) and leave to cool to ambient temperature. As soon as ambient temperature 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
43、residue using a few drops of an ammonium nitrate solution. Insert the crucible into the furnace and slowly heat 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,
44、 in 100 ml distilled water. 7.2 Samples containing volatile substances For samples containing significant amounts 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
45、loss on ignition is always performed directly on the undried sample. Place a crucible (6.1) in the furnace (6.2) 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 tempera
46、ture. 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 loss of volatiles fro
47、m the samples until it has been weighed. To avoid splashing caused by escaping vapours or sudden fire, most of the volatile components should be removed from the sample at ambient temperature in a fume hood prior to ignition. Samples containing highly flammable components e.g. solvents or waste oil
48、should be ignited and allowed to burn in a fume hood before being inserted into the furnace. When ready place the crucible into the cold furnace. Raise the furnace temperature to (550 25) C and hold this temperature for at least 1 h. Place the hot crucible containing the residue on ignition on a met
49、al 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 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 to avoid losses by the steam developm
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