1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN 15934:2012Sludge, treated biowaste,soil and waste Calculationof dry matter fraction afterdetermination of dry residue orwater contentBS EN 15934:2012 BRITISH STANDARDNation
2、al forewordThis British Standard is the UK implementation of EN 15934:2012.The UK participation in its preparation was entrusted to TechnicalCommittee H/-/4, Environmental testing programmes.A list of organizations represented on this committee can beobtained on request to its secretary.This publica
3、tion does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2012. Published by BSI StandardsLimited 2012ISBN 978 0 580 70593 9ICS 13.030.01; 13.080.05Compliance with a British Standard cannot confer i
4、mmunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Strategy Committee on 30 September 2012.Amendments issued since publicationDate Text affectedBS EN 15934:2012EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15934 August 2012 ICS 13.
5、030.01 English Version Sludge, treated biowaste, soil and waste - Calculation of dry matter fraction after determination of dry residue or water content Boues, bio-dchets traits, sols et dchets - Calcul de la teneur en matire sche par dtermination du rsidu sec ou de la teneur en eau Schlamm, behande
6、lter Bioabfall, Boden und Abfall - Berechnung des Trockenmassenanteils nach Bestimmung des Trockenrckstands oder des Wassergehalts 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 g
7、iving 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 Management Centre or to any CEN member. This European Standard exists in three o
8、fficial 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 as the official versions. CEN members are the national standards bodies
9、 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, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spai
10、n, 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 exploitation in any form and by any means reserved worldwide for CEN nat
11、ional Members. Ref. No. EN 15934:2012: EBS EN 15934:2012EN 15934:2012 (E) 2 Contents Page Foreword 3Introduction .41 Scope 52 Normative references 53 Terms and definitions .54 Principle 54.1 General 54.2 Principle of Method A Drying at 105 C (dry residue) .64.3 Principle of Method B Direct Karl-Fisc
12、her-titration (water content) 65 Sample preparation .66 Method A Drying at 105 C .66.1 General 66.2 Interferences 66.3 Hazards .66.4 Apparatus .66.5 Procedure .76.6 Calculation of results 77 Method B Direct Karl-Fischer-titration (volumetric/coulometric detection)87.1 Interferences 87.2 Reagents .87
13、.3 Apparatus .87.4 Procedure .87.4.1 Determination of the equivalence factor .87.4.2 Analysis of liquid samples 97.4.3 Analysis of solid samples .98 Calculation of dry matter fraction . 109 Precision 1010 Test report . 10Annex A (informative) Repeatability and reproducibility . 11A.1 Performance cha
14、racteristics . 11A.2 Types of samples and sample preparation 12A.3 Homogeneity and stability . 13A.4 Dry matter fraction results by different methods 14Annex B (informative) Azeotropic distillation with toluene . 15B.1 General . 15B.2 Interferences . 15B.3 Hazards 15B.4 Reagents 15B.5 Apparatus 15B.
15、6 Procedure 16B.7 Calculation of results . 16B.8 System performance check . 16B.9 Performance data 17Annex C (informative) Summary of general requirements and recommendations . 19BS EN 15934:2012EN 15934:2012 (E) 3 Foreword This document (EN 15934:2012) has been prepared by Technical Committee CEN/T
16、C 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 publication of an identical text or by endorsement, at the latest by February 2013,
17、 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 shall not be held responsible for identifying any or all such patent rights.
18、 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 (Mandate M/330), which assigned the development of standards on sampling and anal
19、ytical 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. According to the CEN/CENELEC Internal Regulations, the national standards organi
20、zations 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, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, M
21、alta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. BS EN 15934:2012EN 15934:2012 (E) 4 Introduction In case of analysis of solids and sludge water is usually not considered as part of the sample and results are general
22、ly related to dry matter, which can be calculated by determination of the dry residue (dry matter fraction). For this purpose, and for the determination of the water content, two methods are described in this European Standard. The choice of the method depends on the type of sample and its content o
23、f volatile substances excluding water. As a result of the validation study, the determination of water content by azeotropic distillation has been replaced by Karl-Fischer-titration. Nevertheless, the distillation may be useful in certain cases. This method is described in Annex B (informative). Thi
24、s 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 applicable and validated Matrix Materials used for validation Sludge (only method A) Munici
25、pal sludge Biowaste (only method A) Fresh compost Soil (only method A) Sludge amended soil Waste (method A and B) Contaminated soil, Dredged sludge, Nickel sludge, Filter cake, Distillation residue, Drilling emulsion WARNING Persons using this European Standard should be familiar with usual laborato
26、ry 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 abs
27、olutely essential that tests conducted according to this European Standard be carried out by suitably trained staff. BS EN 15934:2012EN 15934:2012 (E) 5 1 Scope This European Standard specifies methods for the calculation of the dry matter fraction of sludge, treated biowaste, soil and waste for whi
28、ch the results of performed analysis are to be calculated to the dry matter basis. Depending on the nature and origin of the sample, the calculation is based on a determination of the dry residue (Method A) or a determination of the water content (Method B). It applies to samples containing more tha
29、n 1 % (mass fraction) of dry residue or more than 1 % (mass fraction) of water. Method A applies to sludge, treated biowaste, soil and solid waste. Method B applies to liquid waste and to samples which are suspected or known to contain volatiles except for water. 2 Normative references The following
30、 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 document (including any amendments) applies. EN 15002, Characteri
31、zation of waste Preparation of test portions from the laboratory sample 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 dry residue remaining mass fraction of a samp
32、le after a drying process at 105 C under specified conditions 3.2 water content mass fraction of water in a sample determined by the method after drying at 105 C or by Karl-Fischer-titration under specified conditions 3.3 dry matter fraction mass fraction of a sample excluding water expressed as mas
33、s fraction calculated by determination of dry residue or water content 4 Principle 4.1 General Depending on the origin (sludge, biowaste, soil, waste) and the nature of the sample (liquid, solid or multiphase) either the water content or the dry residue is to be determined. The results from the dete
34、rmination of water content or dry residue are used to calculate the dry matter fraction. In case of multiphase (waste) samples these samples shall be homogenized. If homogenization is not possible, a phase separation according to EN 15002 shall be applicable and the phases are analysed separately. B
35、S EN 15934:2012EN 15934:2012 (E) 6 4.2 Principle of Method A Drying at 105 C (dry residue) The sample is dried to a constant mass at 105 C. This method applies to solid samples and samples which become solid during the drying process. The method generally applies to soil, sludge and treated biowaste
36、. Solid samples containing amounts of volatiles which are expected to affect the results shall be analysed by Method B. 4.3 Principle of Method B Direct Karl-Fischer-titration (water content) The method usually applies to liquid samples and homogenised multiphase samples. It can also be used for sol
37、id samples in case the “water content” is of interest and in case volatiles are expected to interfere with the determination according to Method A. The water content of a sample is determined by direct Karl-Fischer-titration and either volumetric or coulometric detection. Liquid samples are directly
38、 added to the cell, while solid samples are extracted by use of methanol. 5 Sample preparation Pretreat the samples according to EN 16179 or EN 15002, if not otherwise specified. 6 Method A Drying at 105 C 6.1 General When performing any kind of analysis on samples, the dry matter fraction shall be
39、determined simultaneously on identical test portions, in order to base all other test results on the determined dry matter content of each individual sample. 6.2 Interferences The samples can change during the drying process, e.g. by absorption of carbon dioxide in the case of alkaline samples, or o
40、f oxygen by reducing substances. Volatile compounds evaporating at 105 C are measured as water using this procedure. NOTE For alkaline samples or samples susceptible to oxidation the drying can be carried out in a nitrogen atmosphere. 6.3 Hazards Flammable or explosive gases may be released in the d
41、rying process. 6.4 Apparatus 6.4.1 Drying system thermostatically controlled and capable of maintaining a temperature of (105 5) C; e.g. drying oven, infrared system, halogen lamp system. 6.4.2 Desiccator with an active drying agent such as silica gel. 6.4.3 Precision balance with an accuracy of 1 m
42、g or better. 6.4.4 Evaporating dish or crucible. Temperature tolerant laboratory vessel withstanding 105 C. Suitable materials are metallic, ceramic, borosilicate glass or quartz. NOTE 1 If the sample is to be ashed following this procedure, it should be ensured that the material will withstand the
43、elevated temperatures. BS EN 15934:2012EN 15934:2012 (E) 7 NOTE 2 The material of the evaporating dish or crucible should be compatible with the nature of the sample to avoid interferences upon weighing due to possible oxidations. 6.5 Procedure Place an evaporating dish or crucible (6.4.4) in the dr
44、ying system (6.4.1) set at (105 5) C for a minimum of 30 min. After cooling in the desiccator (6.4.2) to ambient temperature, weigh the basin to the nearest 1 mg. Depending on the expected dry residue, weigh into the evaporating dish or crucible (6.4.4) a suitable amount of material so that the resi
45、due obtained has a weight of at least 0,5 g. Weigh the loaded basin to the nearest 1 mg. Place the evaporating dish or crucible (6.4.4) containing the sample in the drying system (6.4.1) set at (105 5) C until the residue appears dry, typically overnight. NOTE For some samples e.g. sludge, there is
46、a risk of formation of a cake surface, which hinders an even drying. To avoid this, a glass rod can be weighed along with the dish. If cake formation occurs during drying, the glass rod is used to stir the sample, to break up the cake. This should be repeated as necessary. The rod should be reweighe
47、d afterwards. After cooling in the desiccator (6.4.2) weigh the evaporating dish or crucible and contents for the first time. The dry residue shall be regarded as constant if the mass obtained after further 1 h of drying does not differ by more than 0,5 % of the previous value or 2 mg whichever is t
48、he greater. Otherwise repeat the drying process. In case of weight inconstancy after three cycles the drying process may be stopped (after at least 16 h). The result of the last weighing shall be recorded in the test report. A drying period of 16 h is sufficient. In case of infrared or halogen lamp
49、drying systems the corresponding manufacturers instructions apply. The technique of choice shall be recorded in the test report. Other techniques than oven drying, infrared or halogen lamp drying are allowed, provided they are proven to give comparable results. 6.6 Calculation of results The dry residue is calculated according to Formula (1): fmmmmw =abacdr(1) where wdris the dry residue of the sample, expressed as mass fraction in percent
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