Sludge, treated biowaste, soil and waste - Calculation of dry matter fraction after determination of dry residue or water content

This European Standard specifies methods for the calculation of the dry matter of sludge, treated biowaste, soil and waste for which 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 than 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.

Schlamm, behandelter Bioabfall, Boden und Abfall - Berechnung des Trockenmassenanteils nach Bestimmung des Trockenrückstands oder des Wassergehalts

Diese Europäische Norm legt Verfahren zur Berechnung des Trockenmassenanteils von Schlamm,
behandeltem Bioabfall, Boden und Abfall fest, bei denen die Ergebnisse der durchgeführten Analyse auf
wasserfreier Bezugsbasis zu berechnen sind. In Abhängigkeit vom Charakter und Herkunft der Probe erfolgt
die Berechnung auf der Basis der Bestimmung des Trockenrückstandes (Verfahren A) oder des
Wassergehaltes (Verfahren B). Sie gilt für Proben mit einem Trockenrückstand oder einem Wassergehalt von
mehr als 1 % (Massenanteil).
Verfahren A ist anwendbar auf Schlamm, behandelten Bioabfall, Boden und feste Abfälle. Verfahren B ist
anwendbar auf flüssige Abfälle und auf Proben, die vermutlich oder nachweislich flüchtige Stoffe, mit
Ausnahme von Wasser, enthalten.

Boues, bio-déchets traités, sols et déchets - Calcul de la teneur en matière sèche par détermination du résidu sec ou de la teneur en eau

La présente Norme européenne spécifie des méthodes de calcul de la fraction de matière sèche des boues, biodéchets traités, sols et déchets pour lesquels les résultats de l'analyse réalisée doivent être rapportés à la matière sèche. Selon la nature et l'origine de l'échantillon, le calcul est basé sur une détermination du résidu sec (méthode A) ou une détermination de la teneur en eau (méthode B). Elle s'applique à des échantillons contenant plus de 1 % (fraction massique) de résidu sec ou plus de 1 % (fraction massique) d'eau.
La méthode A s'applique aux boues, biodéchets traités, sols et déchets solides, la méthode B s'applique aux déchets liquides et aux échantillons suspectés ou connus pour contenir des substances volatiles autres que l'eau.

Blato, obdelani biološki odpadki, tla in odpadki - Izračun suhe snovi z določevanjem suhega ostanka ali vsebnosti vode

Ta evropski standard določa metode za izračun deleža suhe snovi v blatu, predelanih bioloških odpadkih, prsti in smeteh, za katere se rezultati izvedene analize izračunajo na podlagi suhe snovi. Glede na lastnosti in izvor vzorca temelji izračun na določitvi suhega ostanka (metoda A) ali določitvi vsebnosti vode (metoda B). Velja za vzorce, ki vsebujejo več kot 1 % (masni delež) suhega ostanka ali več kot 1 % (masni delež) vode. Metoda A velja za blato, predelane biološke odpadke, prst in trdne odpadke. Metoda B velja za tekoče odpadke in vzorce, za katere se sumi ali za katere je znano, da vsebujejo hlapne tekočine (razen vode).

General Information

Status
Published
Publication Date
21-Aug-2012
Current Stage
9093 - Decision to confirm - Review Enquiry
Due Date
04-Mar-2018
Completion Date
17-May-2018

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Schlamm, behandelter Bioabfall, Boden und Abfall - Berechnung des Trockenmassenanteils nach Bestimmung des Trockenrückstands oder des WassergehaltsBoues, bio-déchets traités, sols et déchets - Calcul de la teneur en matière sèche par détermination du résidu sec ou de la teneur en eauSludge, treated biowaste, soil and waste - Calculation of dry matter fraction after determination of dry residue or water content13.030.20Liquid wastes. SludgeICS:Ta slovenski standard je istoveten z:EN 15934:2012SIST EN 15934:2012en,fr,de01-december-2012SIST EN 15934:2012SLOVENSKI

STANDARD
SIST EN 15934:2012
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15934
August 2012 ICS 13.030.01 English Version

Sludge, treated biowaste, soil and waste - Calculation of dry matter fraction after determination of dry residue or water content

Boues, bio-déchets traités, sols et déchets - Calcul de la teneur en matière sèche par détermination du résidu sec ou de la teneur en eau

Schlamm, behandelter Bioabfall, Boden und Abfall - Berechnung des Trockenmassenanteils nach Bestimmung des Trockenrückstands 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 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 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 has 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, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR 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 15934:2012: ESIST EN 15934:2012

EN 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-Fischer-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 .................................................................................................................................................87.3 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 characteristics ............................................................................................................. 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.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 ................................... 19 SIST EN 15934:2012

EN 15934:2012 (E) 3 Foreword This document (EN 15934:2012) 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 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. 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 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 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 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, 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, Sweden, Switzerland, Turkey and the United Kingdom.

SIST EN 15934:2012

EN 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 generally 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 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). 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 applicable and validated Matrix Materials used for validation Sludge

(only method A) Municipal 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 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 regulatory conditions. IMPORTANT — It is absolutely essential that tests conducted according to this European Standard be carried out by suitably trained staff. SIST EN 15934:2012

EN 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 which 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 than 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 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, Characterization 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 sample 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 mass 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 determination 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. SIST EN 15934:2012

EN 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. 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 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. 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. 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 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 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 can be carried out in a nitrogen atmosphere. 6.3 Hazards Flammable or explosive gases may be released in the drying 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 mg 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 elevated temperatures. SIST EN 15934:2012

EN 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 drying 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 residue 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 a risk of formation of a cake surface, which hinders an even drying. To avoid this, a glass rod can be weighe

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