SIST EN 15934:2012
(Main)Sludge, treated biowaste, soil and waste - Calculation of dry matter fraction after determination of dry residue or water content
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 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.
Schlamm, behandelter Bioabfall, Boden und Abfall - Berechnung des Trockenmassenanteils nach Bestimmung des Trockenrückstands oder des Wassergehalts
Diese Europäische Norm legt ein Verfahren zur Bestimmung der Trockenmasse auf Grundlage der Masse in folgenden Materialien fest:
- Schlämme einschließlich flüssiger, pastöser oder fester Schlämme;
- alle Arten luftgetrockneter Bodenproben und feldfeuchter Bodenproben;
- Sediment;
- Abfälle; und
- behandelter Bioabfall.
ANMERKUNG Nach diesem Verfahren ist die Bestimmung des Wassergehalts einer Probe unter der Voraussetzung möglich, dass der beim Trocknen bei 105 °C auftretende Masseverlust überwiegend auf Wasser zurückzuführen ist und andere Verbindungen keinen signifikanten Betrag beisteuern.
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
Relations
Buy Standard
Standards Content (Sample)
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
...
SLOVENSKI STANDARD
oSIST prEN 15934:2011
01-januar-2011
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VXKHJDRVWDQNDLQYRGH
Sludge, treated biowaste, soil and waste - Calculation of dry matter by determination of
dry residue or water content
Schlamm, behandelter Bioabfall, Boden und Abfall - Berechnung der Trockenmasse
durch Bestimmung des Trockenrückstands oder des Wassergehalts
Boue, biodéchet traité, sol et déchets - Calcul de la teneur en matière sèche par
détermination du résidu sec ou de la teneur en eau
Ta slovenski standard je istoveten z: prEN 15934
ICS:
13.030.20 7HNRþLRGSDGNL%ODWR Liquid wastes. Sludge
oSIST prEN 15934:2011 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 15934:2011
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oSIST prEN 15934:2011
EUROPEAN STANDARD
DRAFT
prEN 15934
NORME EUROPÉENNE
EUROPÄISCHE NORM
December 2010
ICS 13.030.01
English Version
Sludge, treated biowaste, soil and waste - Calculation of dry
matter by determination of dry residue or water content
Boue, biodéchet traité, sol et déchets - Calcul de la teneur Schlamm, behandelter Bioabfall, Boden und Abfall -
en matière sèche par détermination du résidu sec ou de la Berechnung der Trockenmasse durch Bestimmung des
teneur en eau Trockenrückstands oder des Wassergehalts
This draft European Standard is submitted to CEN members for second enquiry. It has been drawn up by the Technical Committee
CEN/TC 400.
If this draft becomes a European Standard, 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.
This draft European Standard was established by CEN 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 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are aware and to
provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without notice and
shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2010 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 15934:2010: E
worldwide for CEN national Members.
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oSIST prEN 15934:2011
prEN 15934:2010 (E)
Contents Page
Foreword .3
Introduction .4
1 Scope .5
2 Normative references .5
3 Terms and definitions .5
4 Principle .6
4.1 General .6
4.2 Principle of Method A — Drying at 105 °C (dry residue) .6
4.3 Principle of Method B — Direct Karl-Fischer-titration (water content) .6
5 Sample preparation .6
6 Method A — Drying at 105 °C .6
6.1 General .6
6.2 Interferences .6
6.3 Hazards .6
6.4 Apparatus .6
6.5 Procedure .7
6.6 Calculation of results .7
7 Method B — Direct Karl-Fischer-titration (volumetric/coulometric detection).8
7.1 Interferences .8
7.2 Reagents .8
7.3 Apparatus .8
7.4 Procedure .8
7.4.1 Determination of the equivalence factor .8
7.4.2 Analysis of liquid samples .9
7.4.3 Analysis of solid samples .9
8 Calculation of dry matter . 10
9 Precision . 11
10 Test report . 11
Annex A (informative) Repeatability and reproducibility . 12
A.1 Performance characteristics . 12
A.2 Types of samples and sample preparation . 13
A.3 Homogeneity and stability . 14
A.4 Dry matter results by different methods . 15
Annex B (informative) Azeotropic distillation with toluene . 16
B.1 General . 16
B.2 Interferences . 16
B.3 Hazards . 16
B.4 Reagents . 16
B.5 Apparatus . 16
B.6 Procedure . 16
B.7 Calculation of results . 17
B.8 System performance check . 17
B.9 Performance data. 18
Annex C (informative) Summary of general requirements and recommendations . 20
2
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oSIST prEN 15934:2011
prEN 15934:2010 (E)
Foreword
This document (prEN 15934:2010) 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 document is currently submitted to the second CEN Enquiry.
This draft European Standard prEN 15934 was completely technically and editorially revised following the
comments made during the first CEN-Enquiry in 2009 and the discussions from CEN/TC 400/WG 4 "Inorganic
elements and compounds".
This European Standard is part of a modular horizontal approach in which this document belongs to the
analytical step.
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.
Until now, test methods determining properties of materials within the environmental area were prepared in
Technical Committees (TCs) working on specific products/matrices (e. g. soil, waste, sludge). However, it is
understood that many steps within individual test procedures may also be used for the analysis of various
other materials. By careful determination of these steps and selection of specific questions within these steps,
elements of the test procedure can be described in a way that can be used for a variety of matrices and
materials with certain specifications. This optimization is in line with the development among end-users of
standards. A majority of routine environmental analyses are carried out by institutions and laboratories
working under a scope that is not limited to one single environmental matrix but covers a wide variety of
matrices. Availability of standards covering more matrices contributes to the optimization of laboratory
procedures and standard maintenance costs, e. g. costs related to accreditation and recognition.
A horizontal modular approach was developed in the project 'Horizontal'. 'Modular' means that a test standard
developed in this approach concerns a specific step in assessing a property and not the whole ”chain of
measurement” (from sampling to analyses). A beneficial feature of this approach is that individual “modules”
can be replaced by improved ones without jeopardizing the standard “chain”.
The results of the desk study as well as the evaluation and validation studies have been subject to
discussions with all parties concerned in the CEN structure during the development by project 'Horizontal'.
The results of these consultations with interested parties in the CEN structure have been presented to and
discussed in CEN/TC 400.
Based on data from interlaboratory studies and consultations with interested parties within CEN member
bodies, it has been concluded that this draft standard prEN 15934 is acceptable for its intended use and is
ready for CEN enquiry.
It is recognized that standardization in the environmental field in most national standardization bodies is
organized in national standardization committees that mirror the vertical structure of technical committees in
the environmental field in CEN. The present CEN enquiry therefore asks for special attention by the NSBs to
assure that the relevant and interested parties are consulted during the CEN enquiry, i. e. to assure that one
single consolidated enquiry reply on this draft standard prEN 15934 can be presented by the NSB that covers
the entire scope of this draft standard.
3
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oSIST prEN 15934:2011
prEN 15934:2010 (E)
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 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).
This European Standard is (applicable and) validated for several types of matrices as indicated below (see
also Annex A for the results of the validation):
Table 1 — Matrices for which this European Standard is (applicable and) validated
Matrix Validated for
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
4
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oSIST prEN 15934:2011
prEN 15934:2010 (E)
WARNING — Persons using this European Standard should be familiar with normal 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.
1 Scope
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 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
prEN WI 00400022, Sludge, treated biowaste and soil — Guidance for sample pre-treatment
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
dry residue
w
dr
remaining mass fraction of a sample after a drying process at 105 °C under specified conditions
3.2
water content
w
w
mass fraction of water in a sample determined by Karl-Fischer-titration under specified conditions
3.3
dry matter
w
dm
mass fraction of a sample excluding water expressed as mass fraction calculated by determination of dry
residue or water content
5
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oSIST prEN 15934:2011
prEN 15934:2010 (E)
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. 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.
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. The method generally applies to soil, sludge and
treated bio waste. 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 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. 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
Samples should be pretreated according to prEN WI 00400022, if necessary.
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 Apparatus
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
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oSIST prEN 15934:2011
prEN 15934:2010 (E)
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 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 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 ± 3) °C for a minimum of
...
SLOVENSKI STANDARD
oSIST prEN 15934:2009
01-julij-2009
7ODEODWRRGSDGNLLQELRRGSDGNL'RORþHYDQMHVXKHVQRYL*UDYLPHWULMVND
PHWRGD
Soil, sludge, waste, and treated biowaste - Determination of dry matter - Gravimetric
method
Schlamm, Boden, Abfall und behandelter Bioabfall - Bestimmung der Trockenmasse -
Gravimetrisches Verfahren
Sol, boue et biodéchet traité - Détermination de la teneur pondérale en matière sèche -
Méthode gravimétrique
Ta slovenski standard je istoveten z: prEN 15934
ICS:
13.030.01 Odpadki na splošno Wastes in general
oSIST prEN 15934:2009 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 15934:2009
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oSIST prEN 15934:2009
EUROPEAN STANDARD
DRAFT
prEN 15934
NORME EUROPÉENNE
EUROPÄISCHE NORM
April 2009
ICS
English Version
Soil, sludge, waste, and treated biowaste - Determination of dry
matter - Gravimetric method
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee CEN/SS S99.
If this draft becomes a European Standard, 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.
This draft European Standard was established by CEN 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 Management Centre has the
same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, 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.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are aware and to
provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without notice and
shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2009 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 15934:2009: E
worldwide for CEN national Members.
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prEN 15934:2009 (E)
Contents
Foreword .3
Introduction .4
1 Scope .5
2 Normative references .5
3 Terms and definitions .6
4 Safety remarks .6
5 Principle .6
6 Interferences and sources of errors .6
7 Apparatus .7
7.1 Drying oven .7
7.2 Desciccator .7
7.3 Temperature tolerant evaporating dish or crucible .7
7.4 Analytical balance.7
8 Sampling and sample pre-treatment.7
9 Procedure .7
10 Quality control .8
11 Calculation and expression of results .8
12 Precision data .9
13 Test report .9
Annex A (informative) Repeatability and reproducibility data . 10
A.1 Materials used in the interlaboratory study . 10
A.2 Interlaboratory study results . 10
A.3 Repeatability and reproducibility limits. . 11
Annex B (informative) Comparison of validation results with earlier validation studies using
the same method . 12
Bibliography . 14
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Foreword
This document (prEN 15934:2009) has been prepared by Technical Committee CEN/SS S99 "Health,
environment and medical equipment - Undetermined", the secretariat of which is held by CMC.
The document is currently submitted to the CEN Enquiry.
This draft standard has been prepared by the European project «Horizontal » and presented to
CEN/TC BTTF 151 “Horizontal Standards in the Fields of Sludge, Biowaste, and Soil”, the secretariat of
which is held by DS. Standardisation is carried out under mandate M330 given to CEN by the European
Commission, and supports essential requirements of EU Directive(s).
The standard is part of a modular horizontal approach in which this standard belongs to the analytical step.
The results of the desk study as well as the evaluation and validation studies have been subject to
discussions with all parties concerned in the CEN structure during the development by project Horizontal.
The results of these consultations with interested parties in the CEN structure have been presented to and
discussed in CEN BT/TF 151.
Based on data from interlaboratory studies and consultations with interested parties within CEN member
bodies, it has been concluded that the draft standard is acceptable for its intended use and is ready for the
CEN enquiry. The matrix “waste” was included during the entire process of development of the draft
standard and is according to a resolution by TC 292 in 2008 included in the scope of the standard.
It is recognized that standardization in the environmental field in most national standardization bodies is
organized in national standardization committees that mirror the vertical structure of technical committees
in the environmental field in CEN. The present CEN enquiry therefore asks for a special attention by the
NSBs to assure that the relevant and interested parties are consulted during the CEN enquiry, i.e. to
assure that one single consolidated enquiry reply on the draft standard can be presented by the NSB that
covers the entire scope of the draft standard.
The standard is applicable and validated for several types of matrices as indicated below:
Material Validated for Reference:
(type of sample, e.g. municipal
sludge, compost)
Sludge Eight sludge samples EN 12880:2000, Annex
Municipal sludge, North Rhine Horizontal Project Interlab comp.
Westphalia
Soil Soil samples ISO 11465:1993
Sludge amended soil, Barcelona Horizontal Project Interlab comp.
Biowaste Fresh compost, Vienna Horizontal Project Interlab comp.
Waste Contaminated soil, dredged EN 14346:2006
sludge, nickel sludge
3
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Introduction
This draft standard is one of a number of draft standards developed and validated in the European project
'Horizontal' financed by the EU commission and EU member states. The project “Horizontal” was
conducted by a European Consortium under the management by ECN, The Netherlands. This draft
standard was presented by the project Horizontal to CEN/BT TF 151 in June 2008 with a view to be
formally adopted as European Standard under CEN rules.
The standardisation by CEN is carried out on a mandate by the European Commission (Mandate M/330).
The mandate considers standards on sampling and analytical methods for hygienic and biological
parameters as well as inorganic and organic determinants. It was the aim of the initiative to develop
standards that are suitable for a wide range of environmental materials and lead to equivalent results as far
as this is technically feasible.
Until now test methods determining properties of materials within the environmental area were prepared in
Technical Committees (TCs) working on specific products/matrices (soil, waste, sludge etc). However, it is
recognized that many steps in test procedures can be used in test procedures for other products/matrices.
By careful determination of these steps and selection of specific questions within these steps, elements of
the test procedure can be described in a way that can be used for more matrices and materials with certain
specifications. This optimization is in line with the development among end-users of standards. A majority
of routine environmental analyses are carried out by institutions and laboratories working under a scope
which is not limited to one single environmental matrix but covers a wide variety of matrices. Availability of
standards covering more matrices contributes to the optimization of laboratory procedures and standard
maintenance costs, e.g. cost related to accreditation and recognition.
A horizontal modular approach was developed in the project 'Horizontal'. 'Modular' means that a test
standard developed in this approach concerns a specific step in assessing a property and not the whole ”
chain of measurement” (from sampling to analyses). A beneficial feature of this approach is that “modules”
can be replaced by better ones without jeopardizing the standard “chain”.
The modules that relates to this standard are specified in section 2 - Normative references.
4
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1 Scope
This European Standard specifies a method for the determination of dry matter on a mass basis of samples
of:
sludges, including liquid, paste-like or solid sludges,
all types of air-dried soil samples and field moist soil samples,
sediment
waste and
treated biowaste.
NOTE Determination of water content of a sample using this method is possible provided that other compounds other
than water do not contribute significantly to the weight loss by heating to 105 ºC.
2 Normative references
This European Standard incorporates by dated or undated reference, provisions from other publications.
These normative references are cited at appropriate places in the text and the publications are listed hereafter.
For dated references, subsequent amendments to or revisions of any of these publications apply to this
European Standard only when incorporated in it by amendment or revision. For undated references, the latest
edition of the publication referred to applies (including amendments).
CSS99031, Sludge, treated biowaste, and soils in the landscape – Sampling – Framework for the preparation
and application of a sampling plan
CSS99058, Sludge, treated biowaste, and soils in the landscape – Sampling – Part 1: Guidance on selection
and application of criteria for sampling under various conditions
CSS99057, Sludge, treated biowaste, and soils in the landscape – Sampling – Part 2: Guidance on sampling
techniques
CSS99032, Sludge, treated biowaste, and soils in the landscape – Sampling - Part 3: Guidance on sub-
sampling in the field
CSS99059, Sludge, treated biowaste, and soils in the landscape – Sampling – Part 4: Guidance on
procedures for sample packaging, storage, preservation, transport and delivery
CSS99060, Sludge, treated biowaste, and soils in the landscape – Sampling – Part 5: Guidance on the
process of defining the sampling plan
CSS99035, Soil, sludge, and treated biowaste – Pre-treatment for inorganic and organic characterization
CSS99023, Soil, sludge and treated biowaste – Determination of loss on ignition
5
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3 Terms and definitions
For the purpose of this European Standard, the following terms and definitions apply.
3.1
dry matter w
dm
dry residue after drying according to the specified drying process. It is expressed as a percentage or in grams
per kilogram
3.2
water content w
wc
mass fraction determined as the loss on mass after the specified drying process. It is expressed as a
percentage or in grams per kilogram
3.3
constant mass
mass reached when, during the drying process, the difference between two successive weighings of the
sample at an interval of minimum 1 h, first heated, then cooled to room temperature, does not exceed 0,5 %
(m/m) of the last determined mass or 2 mg, whichever is the greater
NOTE 1 These definitions do not - for technical reasons - apply to samples containing volatile substances.
NOTE 2 Usually 16 h to 24 h are sufficient for most soil, sludge, sediment and waste samples, but certain
...
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