SIST EN 14346:2007
(Main)Characterization of waste - Calculation of dry matter by determination of dry residue or water content
Characterization of waste - Calculation of dry matter by determination of dry residue or water content
This European Standard specifies methods for the calculation of the dry matter of samples for which the results of performed analysis are to be calculated to the dry matter basis. Depending on the nature 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 than 1 % (m/m) of dry residue or more than 1 % (m/m) of water.
Charakterisierung von Abfällen - Berechnung der Trockenmasse durch Bestimmung des Trockenrückstandes oder des Wassergehaltes
Diese Europäische Norm legt Verfahren zur Bestimmung des Trockenrückstandes und des Wassergehaltes von Abfällen mit einem Anteil an Trockenrückstand oder einem Wassergehalt von mehr als 1 % fest. Sie regelt die Auswahl des jeweils zutreffenden Verfahrens und der Berechnung der Trockenmasse aus den einzelnen Ergebnissen.
ANMERKUNG Im Fall von Altöl sollte die Norm ENV ISO 12937 (zu Mineralölerzeugnissen) oder EN ISO 9029 (zu Rohöl) angewendet werden.
Caractérisation des déchets - Calcul de la teneur en matiere seche par détermination du résidu sec ou de la teneur en eau
La présente Norme européenne spécifie une méthode de calcul de la matiere seche sur la base de la détermination de la teneur en eau et du résidu sec. Elle est applicable aux déchets contenant plus de 1 % (m/m) de résidu sec ou d'eau.
NOTE Dans le cas d'huile usagée, il convient d'appliquer les normes sur les produits pétroliers (ENV ISO 12937) ou sur le pétrole brut (EN ISO 9029).
Karakterizacija odpadkov - Izračun suhe snovi z določitvijo suhega ostanka ali vode
General Information
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.YRGHCharakterisierung von Abfällen - Berechnung der Trockenmasse durch Bestimmung des Trockenrückstandes oder des WassergehaltesCaractérisation des déchets - Calcul de la teneur en matiere seche par détermination du résidu sec ou de la teneur en eauCharacterization of waste - Calculation of dry matter by determination of dry residue or water content13.030.01Odpadki na splošnoWastes in generalICS:Ta slovenski standard je istoveten z:EN 14346:2006SIST EN 14346:2007en,fr,de01-april-2007SIST EN 14346:2007SLOVENSKI
STANDARD
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 14346December 2006ICS 13.030.01 English VersionCharacterization of waste - Calculation of dry matter bydetermination of dry residue or water contentCaractérisation des déchets - Calcul de la teneur enmatière sèche par détermination du résidu sec ou de lateneur en eauCharakterisierung von Abfällen - Berechnung derTrockenmasse durch Bestimmung des Trockenrückstandesoder des WassergehaltesThis European Standard was approved by CEN on 25 November 2006.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2006 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 14346:2006: E
EN 14346:2006 (E) 2 Contents Page Foreword.3 Introduction.4 1 Scope.5 2 Normative references.5 3 Terms and definitions.5 4 Principle.5 5 Sample preparation and storage.6 6 Method A — Drying at 105 °C.6 7 Method B — Direct Karl-Fischer-titration (volumetric/coulometric detection).8 8 Performance characteristics.10 9 Calculation of dry matter.11 10 Test report.12 Annex A (informative)
Additional validation data.13 Annex B (informative)
Azeotropic distillation with toluene.16 Annex C (informative)
Summary of general requirements and recommendations.20
EN 14346:2006 (E) 3 Foreword This document (EN 14346:2006) has been prepared by Technical Committee CEN/TC 292 “Characterization of waste”, the secretariat of which is held by NEN. 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 June 2007, and conflicting national standards shall be withdrawn at the latest by June 2007. Anyone dealing with waste and sludge analysis should be aware of the typical risks of that kind of material irrespective of the parameter to be determined. Waste and sludge samples may contain hazardous (e.g. toxic, reactive, flammable, infectious) substances, which can be liable to biological and/or chemical reaction. Consequently these samples should be handled with special care. Gases which may be produced by microbiological or chemical activity are potentially flammable and will pressurise sealed bottles. Bursting bottles are likely to result in hazardous shrapnel, dust and/or aerosol. National regulations should be followed with respect to all hazards associated with this method. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EN 14346:2006 (E) 4 Introduction In case of waste analysis water is usually not considered as part of the sample and results are generally related to dry matter, which can be calculated from the water content or the dry residue. For this purpose two methods are described in this European Standard. The choice of the method depends on the type of sample and its content of 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).
EN 14346:2006 (E) 5 1 Scope This European Standard specifies methods for the calculation of the dry matter of samples for which the results of performed analysis are to be calculated to the dry matter basis. Depending on the nature 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 than 1 % (m/m) of dry residue or more than 1 % (m/m) of water. 2 Normative references The following referenced documents are indispensable for the application of this document. 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 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. NOTE These definitions only apply to waste. In standards dealing with other matrices other terms and definitions exist for technical reasons. 3.1 dry residue wdr remaining mass fraction of a sample after a drying process at 105 °C as specified in this European Standard 3.2 water content ww mass fraction of water in a sample determined by Karl-Fischer-titration as specified in this European Standard 3.3 dry matter wdm mass fraction of a sample excluding water expressed as a percentage by mass calculated by determination of dry residue or water content according to this European Standard 4 Principle 4.1 General Depending on 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 determination of water content or dry residue are used to calculate the dry matter. In case of multiphase 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.
EN 14346:2006 (E) 6 4.2 Principle of Method A — Drying at 105 °C (dry residue) The sample is dried to a constant mass in an oven at (105 ± 3) °C. This method applies to solid samples and samples which become solid during the drying process. 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 — Karl-Fischer-titration (water content) The water content of a sample is determined by direct Karl-Fischer-titration and either volumetric or coulometric detection. Liquid samples are directly added to the cell, while solid samples are extracted by use of methanol. The method usually applies to liquid samples and homogenised multiphase samples. It could also be used for solid samples in case the “water content” is of interest and in case volatiles are expected to interfere with the determination according to Method A. 5 Sample preparation and storage Specification of sample preparation is not included in this European Standard. As the dry matter content is calculated in order to convert obtained results for a sample to the dry matter basis, the determination of dry residue or water content shall be carried out on the identical portions of the same test sample. By that the sample preparation is as specified in the actual analysis standard. Storage of samples may cause changes as e.g. uptake or liberation of water, carbon dioxide and other volatiles. If it is not possible to carry out the determination of dry residue or water content parallel to the analyses, samples shall be stored in air-tight containers. Biologically active samples shall be stored at about 4 °C and analysed within 3 days. 6 Method A — Drying at 105 °C 6.1 General When carrying out one or more analysis on a sample, the dry matter shall be determined on an identical test portion in parallel in order to recalculate the results of the other analysis to the dry matter basis. 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 of 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 could be carried out in a nitrogen atmosphere. 6.3 Hazards Flammable or explosive gases may be released in the drying process. 6.4 Equipment 6.4.1 Drying system thermostatically controlled and capable of maintaining a temperature of (105 ± 3) °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 Analytical balance with an accuracy of 1 mg or better.
EN 14346:2006 (E) 7 6.4.4 Evaporating dish or crucible. Temperature tolerant laboratory vessel withstanding 105 °C. Suitable materials are metallic or ceramic. NOTE 1 If the sample is to be ashed following this procedure, it should be ensured that the material will withstand the elevated temperatures. NOTE 2 The material of the evaporating dish or crucible should be compatible with the nature of the waste to avoid interferences upon weighing due to possible oxidations. 6.5 Procedure Place an evaporating dish or crucible (6.4.4) in the drying system (6.4.1) set at (105 ± 3) °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 (ma). Depending on the expected dry residue, weigh into the evaporating dish or crucible a suitable amount of material so that the residue obtained has a weight of at least 0,5 g. Weigh the loaded basin to the nearest 1 mg (mb). Place the evaporating dish or crucible (6.4.4) containing the sample in the drying system (6.4.1) set at (105 ± 3) °C until the residue appears dry, typically overnight. NOTE 1 For some samples e.g. sludge, there is 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 reweighed afterwards. After cooling in the desiccator (6.4.2) weigh the evaporating dish or crucible and contents for the first time, (mc). The dry residue (mc – ma) shall be regarded as constant if the mass obtained after a further one hour of drying does not differ by more than 0,5 % of the previous value or 2 mg whichever is the greater. Otherwise repeat the drying process. NOTE 2 In case of weight inconstancy after three cycles the drying process may be stopped (after at least 12 h). The result of the last weighing should be recorded in the test report. In case of infrared or halogen lamp drying systems the corresponding manufacturer’s instructions apply. The technique of choice has to be noted in the test report. Other techniques than oven drying (infrared/halogen) are allowed, provided they are proven to give comparable results. 6.6 Calculation of results The dry residue, expressed as mass fraction in per cent or in grams per kilogram, is calculated according to Equation (1): ()()fmmmmw×−−=abacdr (1) where wdr
is the dry residue of the sample, expressed as mass fraction in per cent [%] or in grams per kilogram [g/kg]; ma
is the mass of the empty dish or crucible, expressed in grams [g];
EN 14346:2006 (E) 8 mb
is the mass of the dish or crucible containing the sample, expressed in grams [g]; mc
is the mass of the dish or crucible containing the dried sample, expressed in grams [g]; f is the conversion factor f = 100 for expression of results as mass fraction in per cent [%] and f = 1 000 for expression of results in grams per kilogram [g/kg]. The analysis is performed at least in duplicate; the mean value is calculated and reported. 7 Method B — Direct Karl-Fischer-titration (volumetric/coulometric detection) 7.1 Interferences Substances like peroxides, oxides, hydroxides, ammonia, carbonates, hydrogen carbonates, disulfites, nitrite, sulfite, thiosulfate, hydrazine and derivatives, iron (II), copper (I), tin (II), silanoles, arsenite, arsenate, selenite, tellurite, phenols, boric compounds, aldehydes, acetone and other reactive ketones may interfere. Especially all reductive or oxidative reagents are potentially interfering. In case of concern about interferences results can be verified by azeotropic distillation (Annex B). Most of the interferences are reduced in case of extraction with methanol before analysis. 7.2 Reagents All reagents used shall be at least an
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