1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 15936:2012Sludge, treated biowaste, soiland waste Determination oftotal organic carbon (TOC) bydry combustionBS EN 15936:2012 BRITISH STANDARDNational forewordThis British
2、Standard is the UK implementation of EN 15936:2012. 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
3、to include all the necessary 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 70595 3 ICS 13.030.01; 13.080.05 Compliance with a British Standard cannot confer immunity from lega
4、l obligations.This British 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 15936:2012EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15936 August 2012 ICS 13.030.0
5、1 English Version Sludge, treated biowaste, soil and waste - Determination of total organic carbon (TOC) by dry combustion Boues, bio-dchets traits, sols et dchets - Dtermination de la teneur en carbone organique total (COT) par combustion sche Schlamm, behandelter Bioabfall, Boden und Abfall - Best
6、immung des gesamten organischen Kohlenstoffs (TOC) mittels trockener Verbrennung 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 Standard the status of a natio
7、nal 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, French, German). A vers
8、ion 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, Bulgaria, Croatia, Cyprus, C
9、zech 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, Turkey and United Kingdom.
10、 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 15936:2012: EBS EN 1593
11、6:2012EN 15936:2012 (E) 2 Contents Page Foreword 3Introduction .41 Scope 52 Normative references 53 Terms and definitions .54 Principle 55 Interferences 66 Reagents .77 Apparatus .78 Sample pretreatment .89 Procedure - Method A (Indirect method) .810 Procedure Method B (direct method) . 1111 Precisi
12、on 1312 Test report . 13Annex A (informative) Repeatability and reproducibility data . 14Annex B (informative) Factors influencing dry combustion methods 17Annex C (informative) Determination of total organic carbon (TOC) in solid samples using the suspension method 20Bibliography . 24BS EN 15936:20
13、12EN 15936:2012 (E) 3 Foreword This document (EN 15936:2012) 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 natio
14、nal 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. Attention is drawn to the possibility that some of the elements of this document may be the subject of pat
15、ent 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 the European Free Trade Association. The preparation of this document by CEN is based on a mandate b
16、y 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 determinants, aiming to make these standards applicable to sludge, treated biowaste and soil as far as thi
17、s 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, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republi
18、c of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 15936:2012EN 15936:2012 (E) 4 Introduction This Europe
19、an 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 applicable and validated Matrix Materials used for validation Sludge Municipal sludge Biowaste Comp
20、ost, Fresh Compost Soil Sludge amended soil, Agricultural soil Waste Filter cake,Bottom ash, Electro-plating sludge, Dredged sludge, Rubble WARNING Persons using this European Standard should be familiar with usual laboratory practice. This European Standard does not purport to address all of the sa
21、fety 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 absolutely essential that tests conducted according to this European Standard be
22、 carried out by suitably trained staff. BS EN 15936:2012EN 15936:2012 (E) 5 1 Scope This European Standard specifies two methods for the determination of total organic carbon (TOC) in sludge, treated biowaste, soil, waste and sediment samples containing more than 1 g carbon per kg of dry matter (0,1
23、 %). For sludge, treated biowaste and soil only Method A is validated. 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 referen
24、ces, the latest edition of the referenced document (including any amendments) applies. EN 15002, Characterization of waste Preparation of test portions from the laboratory sample EN 15934, Sludge, treated biowaste, soil and waste Calculation of dry matter fraction after determination of dry residue
25、or water content EN 16179, Sludge, treated biowaste and soil Guidance for sample pretreatment 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 total carbon TC quantity of carbon present in the sample in the form of organic, inorganic and eleme
26、ntary carbon 3.2 total inorganic carbon TIC quantity of carbon that is liberated as carbon dioxide by acid treatment 3.3 total organic carbon TOC quantity of carbon that is converted into carbon dioxide by combustion and which is not liberated as carbon dioxide by acid treatment 4 Principle 4.1 Meth
27、od A (indirect procedure) In this procedure, the TOC is obtained by the difference between the results of the measurements of TC and TIC. The total carbon (TC) present in the sample is converted to carbon dioxide by combustion in an oxygen-containing gas flow free of carbon dioxide. To ensure comple
28、te combustion, catalysts and/or modifiers can be used. The released amount of carbon dioxide is measured by infrared spectrometry, thermal conductivity detection, flame ionisation detection after reduction to methane, or by gravimetry, coulometry, conductometry after absorption. BS EN 15936:2012EN 1
29、5936:2012 (E) 6 The TIC is determined separately from another sub-sample by means of acidification and purging of the released carbon dioxide. The carbon dioxide is measured by one of the techniques mentioned above. Alternatively, for soil the total organic carbon content may be calculated by determ
30、ining the total carbon content and subtracting the carbon present as carbonate, which can be determined according to ISO 10693 (volumetric method). 4.2 Method B (direct procedure) In this procedure, the carbonates present in the sample are previously removed by treating the sample with acid. The car
31、bon dioxide released by the following combustion step is measured by one of the techniques mentioned in 4.1 and indicates the TOC directly. 4.3 Applicability of Methods A or B Methods A and B have the same applicability for the determination of TOC and/or the determination of the TIC to TOC ratio. I
32、n samples with relatively high inorganic carbon contents method B should be applied. Method B may lead to incorrect results in the following cases: the sample contains volatile substances that evaporate during the acidification (e.g. volatile hydrocarbons from sludge of oil separators); side reactio
33、ns between the sample and the acid take place (e.g. decarboxylation, volatile reaction products). NOTE The quality of results of Method B is dependent on experience and practice, especially regarding the steps before the determination of TOC. Use of automatic dispensing units regarding removal of ca
34、rbonates prior to determination of TOC may improve the performance of Method B. 5 Interferences Volatile organic substances may be lost during sample preparation. If necessary, the carbon content resulting from volatile organic substances shall be determined separately. Depending on the laboratory e
35、xperience with samples containing high amounts of carbonate the procedures may lead to unreliable TOC results if the TIC to TOC ratio is very high (e.g. 10). Depending on the detection method used, different interferences may occur, for instance: the presence of cyanide may interfere with the coulom
36、etric detection of TIC by modifying the pH value (dissolution of HCN); high content of halogenated compounds may lead to an overestimation of TOC when coulometric detection is used; in some cases the classical silver or copper trap can be insufficient to absorb all halides. When present, elementary
37、carbon, carbides, cyanides, cyanates, isocyanates, isothiocyanates and thiocyanates are determined as organic carbon using the methods described in this European Standard. An interpretation of the measured value may therefore be problematic in cases where the sample contains relevant levels of the a
38、bove-mentioned components. If needed, these components shall be determined separately by means of a suitable validated method and be recorded in the test report. Elementary carbon, determined separately, may be subtracted if required for the sample. If this is done this shall be reported by the labo
39、ratory. BS EN 15936:2012EN 15936:2012 (E) 7 6 Reagents Use only reagents of recognized analytical grade, unless otherwise specified. Hygroscopic substances shall be stored in a desiccator. 6.1 Calcium carbonate, CaCO3. 6.2 Sodium carbonate, Na2CO3, anhydrous. 6.3 Tetrasodium ethylenediamine tetraace
40、tate-tetra-hydrate, Na4-EDTA 4 H2O (C10H12N2O8Na4 4 H2O), heated at 80 C for 2 h. Other forms of Na4-EDTA hydrates may be used if the water content is exactly known. In these cases, the composition of the control mixtures has to be recalculated accordingly (see also 6.10 and 6.11). 6.4 Potassium hyd
41、rogen phthalate, C8H5O4K. 6.5 Acetanilide, C8H9NO. 6.6 Atropine, C17H23NO3. 6.7 Spectrographic graphite powder, C. 6.8 Sodium salicylate, C7H5O3Na. 6.9 Aluminium oxide, Al2O3, neutral, granular size 200 m, annealed at 600 C. 6.10 Control mixture A prepared from sodium carbonate (6.2), Na4-EDTA 4 H2O
42、 (6.3) and aluminium oxide (6.9) in a mass ratio of 2,34:1,00:1,97. The mixture shall be homogenized. It should contain 50,00 g/kg TIC and 50,00 g/kg TOC (e.g. 44,13 g of sodium carbonate, 18,83 g Na4-EDTA 4 H2O, 37,04 g of aluminium oxide). 6.11 Control mixture B prepared from sodium salicylate (6.
43、8), calcium carbonate (6.1), Na4-EDTA 4 H2O (6.3) and aluminium oxide (6.9) in a mass ratio of 1,00:4,36:1,97:8,40. The mixture shall be homogenized. It should contain 33,3 g/kg TIC and 66,6 g/kg TOC (e.g. 6,36 g of sodium salicylate, 27,78 g of calcium carbonate, 12,50 g of Na4-EDTA 4 H2O, 53,36 g
44、of aluminium oxide). 6.12 Non-oxidizing mineral acid used for carbon dioxide expulsion, e.g. phosphoric acid H3PO4(w = 85 %). NOTE Due to possible corrosion by hydrochloric acid, phosphoric acid is preferred. 6.13 Carrier gas, e.g. synthetic air, nitrogen, oxygen or argon, free of carbon dioxide and
45、 organic impurities in accordance with the manufacturers instructions. 7 Apparatus 7.1 Precision balance, accurate to at least 0,5 % of test portion weight. 7.2 Equipment for determination of carbon in solids, with accessories. BS EN 15936:2012EN 15936:2012 (E) 8 7.3 Purging unit for TIC determinati
46、on, for Method A only. 7.4 Crucibles or boats, made of e.g. ceramics, silica glass, silver or platinum. NOTE Tin and nickel crucibles are not acid-resistant. Tin crucibles are suitable only for Method A. 8 Sample pretreatment Pretreat the sample according to EN 16179 or EN 15002, if not otherwise sp
47、ecified. For soil, dried samples shall be used. Moist or paste-like samples may be mixed with aluminium oxide (6.9) until granular material is obtained and then be comminuted. In this case, the ratio of aluminium oxide to sample shall be considered in the calculation of TOC (according to 9.4 or 10.4
48、). If samples contain depending on the accuracy of the method negligible amounts of volatile compounds except water, the samples may be dried. 9 Procedure - Method A (Indirect method) 9.1 Determination 9.1.1 General The mass of the test portion should be as large as possible and shall be chosen so t
49、hat the liberated quantity of carbon dioxide lies within the working range of the equipment/calibration. 9.1.2 Determination of the TC The sample prepared according to Clause 8 is weighed into a suitable vessel (7.4). To minimize carbon blank values the vessel may be pre-treated by heating (in a muffle furnace or the TC apparatus itself). The sample is burned or decomposed in a flow of carrier gas containing oxygen (6.13). The combustion temperature shall be high enough to convert all carbon complet
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