DIN EN 15936-2012 Sludge treated biowaste soil and waste - Determination of total organic carbon (TOC) by dry combustion German version EN 15936 2012《污泥 处理后生物废料 土壤和废弃物 干式燃烧法测定总有机碳(.pdf

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1、November 2012 Translation by DIN-Sprachendienst.English price group 13No 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).I

2、CS 13.030.01!$M“1922542www.din.deDDIN EN 15936Sludge, treated biowaste, soil and waste Determination of total organic carbon (TOC) by dry combustion;English version EN 15936:2012,English translation of DIN EN 15936:2012-11Schlamm, behandelter Bioabfall, Boden und Abfall Bestimmung des gesamten organ

3、ischen Kohlenstoffs (TOC) mittels trockenerVerbrennung;Englische Fassung EN 15936:2012,Englische bersetzung von DIN EN 15936:2012-11Boues, bio-dchets traits, sols et dchets Dtermination de la teneur en carbone organique total (COT) par combustion sche;Version anglaise EN 15936:2012,Traduction anglai

4、se de DIN EN 15936:2012-11www.beuth.deIn case of doubt, the German-language original shall be considered authoritative.Document comprises 28 pages10.12 DIN EN 15936:2012-11 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 400 “P

5、roject Committee Horizontal standards in the fields of sludge, biowaste and soil” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Wasserwesen (WaterPractice Standards Committee), Working Committee NA 119-01-02 Abfall- und Bodenuntersuchung

6、119-01-02-02 AA Chemische und physikalische Verfahren. NA The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 5725-2 DIN ISO 5725-2 ISO 8466-1 DIN 38402-51 ISO 10693 DIN ISO 10693 ,DIN EN 15936:2012-11 3 National Annex NA (informative) Bibl

7、iography DIN 38402-51, German standard methods for the examination of water, waste water and sludge General information (group A) Calibration of analytical methods, evaluation of analytical results and linear calibration functions used to determine the performance characteristics of analytical metho

8、ds (A 51) 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 standard measurement method DIN ISO 10693, Soil quality Determination of carbonate content Volumetric method DIN EN 1593

9、6:2012-11 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15936 August 2012 ICS 13.030.01 English Version Sludge, treated biowaste, soil and waste Determination of total organic carbon (TOC) by dry combustion Boues, bio-dchets traits, sols et dchets Dterminati

10、on de la teneur en carbone organique total (COT) par combustion sche Schlamm, behandelter Bioabfall, Boden und Abfall Bestimmung 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 t

11、he 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 CEN-CENELEC Manageme

12、nt 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 has the same status

13、 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, Luxembourg, Malta,

14、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 CEN All rights of

15、exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15936:2012: E EN 15936:2012 (E) 2 Contents PageForeword 3Introduction .41 Scope 52 Normative references 53 Terms and definitions .54 Principle 55 Interferences 66 Reagents .77 Apparatus .78 Sample pret

16、reatment .89 Procedure - Method A (Indirect method) .810 Procedure Method B (direct method) . 1111 Precision 1312 Test report . 13Annex A (informative) Repeatability and reproducibility data . 14Annex B (informative) Factors influencing dry combustion methods 17Annex C (informative) Determination of

17、 total organic carbon (TOC) in solid samples using the suspension method 20Bibliography . 24DIN EN 15936:2012-11EN 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 a

18、nd soil”, the 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 20

19、13. 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 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 Commi

20、ssion and the 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 orga

21、nic determinants, 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: A

22、ustria, Belgium, 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, Sw

23、eden, Switzerland, Turkey and the United Kingdom. DIN EN 15936:2012-11EN 15936:2012 (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 Europe

24、an Standard is applicable and validated Matrix Materials used for validation Sludge Municipal sludge Biowaste Compost, 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 s

25、hould 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. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regul

26、atory conditions. IMPORTANT It is absolutely essential that tests conducted according to this European Standard be carried out by suitably trained staff. DIN EN 15936:2012-11EN 15936:2012 (E) 5 1 Scope This European Standard specifies two methods for the determination of total organic carbon (TOC) i

27、n sludge, treated biowaste, soil, waste and sediment samples containing more than 1 g carbon per kg of dry matter (0,1 %). 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 documen

28、t 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 15002, Characterization of waste Preparation of test portions from the laboratory sample EN

29、15934, Sludge, treated biowaste, soil and waste Calculation of dry matter fraction after determination of dry residue 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 defin

30、itions apply. 3.1 total carbon TC quantity of carbon present in the sample in the form of organic, inorganic and elementary 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

31、 into carbon dioxide by combustion and which is not liberated as carbon dioxide by acid treatment 4 Principle 4.1 Method 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

32、is converted to carbon dioxide by combustion in an oxygen-containing gas flow free of carbon dioxide. To ensure complete combustion, catalysts and/or modifiers can be used. The released amount of carbon dioxide is measured by infrared spectrometry, thermal conductivity detection, flame ionisation de

33、tection after reduction to methane, or by gravimetry, coulometry, conductometry after absorption. DIN EN 15936:2012-11EN 15936:2012 (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 o

34、ne of the techniques mentioned above. Alternatively, for soil the total organic carbon content may be calculated by determining 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

35、) In this procedure, the carbonates present in the sample are previously removed by treating the sample with acid. The carbon 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 Me

36、thods A and B have the same applicability for the determination of TOC and/or the determination of the TIC to TOC ratio. In 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 s

37、ubstances that evaporate during the acidification (e.g. volatile hydrocarbons from sludge of oil separators); side reactions 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,

38、 especially regarding the steps before the determination of TOC. Use of automatic dispensing units regarding removal of carbonates 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, t

39、he carbon content resulting from volatile organic substances shall be determined separately. Depending on the laboratory experience 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 det

40、ection method used, different interferences may occur, for instance: the presence of cyanide may interfere with the coulometric 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 us

41、ed; in some cases the classical silver or copper trap can be insufficient to absorb all halides. When present, elementary carbon, carbides, cyanides, cyanates, isocyanates, isothiocyanates and thiocyanates are determined as organic carbon using the methods described in this European Standard. An int

42、erpretation of the measured value may therefore be problematic in cases where the sample contains relevant levels of the above-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 carbo

43、n, determined separately, may be subtracted if required for the sample. If this is done this shall be reported by the laboratory. DIN EN 15936:2012-11EN 15936:2012 (E) 7 6 Reagents Use only reagents of recognized analytical grade, unless otherwise specified. Hygroscopic substances shall be stored in

44、 a desiccator. 6.1 Calcium carbonate, CaCO3. 6.2 Sodium carbonate, Na2CO3, anhydrous. 6.3 Tetrasodium ethylenediamine tetraacetate-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

45、 cases, the composition of the control mixtures has to be recalculated accordingly (see also 6.10 and 6.11). 6.4 Potassium hydrogen 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

46、, neutral, granular size 200 m, annealed at 600 C. 6.10 Control mixture A prepared from sodium carbonate (6.2), Na4-EDTA 4 H2O (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 sod

47、ium carbonate, 18,83 g Na4-EDTA 4 H2O, 37,04 g of aluminium oxide). 6.11 Control mixture B prepared from sodium salicylate (6.8), 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

48、/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 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 organic impurities in accordance