Sludge, treated biowaste and soil - Determination of adsorbable organically bound halogens (AOX)

This European Standard specifies an empirical method for the direct determination of organically bound chlorine, bromine and iodine (but not fluorine) adsorbed and occluded to the sample matrix. Non-volatile organically bound halogens adsorbable on activated carbon present in the aqueous phase of the sample prior to drying or adsorbed to sample surface are included in the determination. This European Standard is intended for analysis of sludge, treated biowaste or soil in concentrations ranging from 5 mg/kg dry matter to approximately 6 g/kg dry matter. The exact concentration range covered depends on the instrument used for determination.

Schlamm, behandelter Bioabfall und Boden - Bestimmung von adsorbierbaren organisch gebundenen Halogenen (AOX)

Diese Europäische Norm beschreibt ein empirisches Verfahren zur direkten Bestimmung von organisch gebundenem Chlor, Brom und Iod (nicht jedoch von Fluor), die in der Probenmatrix adsorbiert und eingeschlossen sind. Bei dieser Bestimmung werden auch nichtflüchtige organisch gebundene Halogene oder an der Probenoberfläche adsorbierte Halogene erfasst, indem der Probe in der wässrigen Phase vor dem Trocknen Aktivkohle zugegeben wird, an die sich die Halogene anlagern können.
Diese Europäische Norm ist für die Untersuchung von Schlamm, behandeltem Bioabfall oder Boden in Konzentrationen von 5 mg/kg Trockenmasse bis etwa 6 g/kg Trockenmasse vorgesehen. Der tatsächlich erfasste Konzentrationsbereich hängt vom verwendeten Gerät ab.

Boue, biodéchet traité et sol - Détermination des composés organiques halogénés adsorbables (AOX)

La présente Norme européenne spécifie une méthode empirique pour la détermination directe des composés organiques contenant du chlore, du brome et de l'iode (mais pas de fluor) adsorbés sur et inclus dans la matrice de l'échantillon. Les composés organiques halogénés non volatils adsorbables sur charbon actif, présents dans la phase aqueuse de l'échantillon avant le séchage ou adsorbés sur la surface de l'échantillon sont inclus dans la détermination.
La présente Norme européenne est destinée à l'analyse des boues, des biodéchets traités ou des sols dont les concentrations sont comprises entre 5 mg/kg et 6 g/kg de matière sèche environ. La gamme exacte de concentrations couverte dépend de l'appareillage utilisé pour la détermination.

Blato, obdelani biološki odpadki in tla - Določevanje organsko vezanih halogenov, sposobnih adsorpcije (AOX)

Ta evropski standard določa empirično metodo za neposredno določevanje organsko vezanega klora, broma in joda (ne pa fluora), adsorbiranih in vezanih v matrico vzorca. V določevanje so vključeni nehlapni organsko vezani halogeni, sposobni adsorbcije na aktiviran ogljik v vodni fazi vzorca pred sušenjem ali adsorbirani na površino vzorca. Namen tega evropskega standarda je analiza blata, obdelanih bioloških odpadkov ali tal v koncentracijah od 5 mg/kg do približno 6 g/kg suhe snovi. Natančno območje koncentracije je odvisno od instrumentov, uporabljenih za določevanje.

General Information

Status
Published
Public Enquiry End Date
19-Feb-2011
Publication Date
20-Jan-2013
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
07-Jan-2013
Due Date
14-Mar-2013
Completion Date
21-Jan-2013

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Schlamm, behandelter Bioabfall und Boden - Bestimmung von adsorbierbaren organisch gebundenen Halogenen (AOX)Boue, biodéchet traité et sol - Détermination des composés organiques halogénés adsorbables (AOX)Sludge, treated biowaste and soil - Determination of adsorbable organically bound halogens (AOX)13.080.10Chemical characteristics of soils13.030.20Liquid wastes. SludgeICS:Ta slovenski standard je istoveten z:EN 16166:2012SIST EN 16166:2013en,fr,de01-februar-2013SIST EN 16166:2013SLOVENSKI

STANDARD
SIST EN 16166:2013
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16166
August 2012 ICS 13.030.01; 13.080.10 English Version

Sludge, treated biowaste and soil - Determination of adsorbable organically bound halogens (AOX)

Boues, biodéchets traités et sols - Détermination des composés organiques halogénés adsorbables (AOX)

Schlamm, behandelter Bioabfall und Boden - Bestimmung von adsorbierbaren organisch gebundenen Halogenen (AOX) 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 16166:2012: ESIST EN 16166:2013

EN 16166:2012 (E) 2 Contents Page Foreword ..............................................................................................................................................................3Introduction .........................................................................................................................................................41 Scope ......................................................................................................................................................52 Normative references ............................................................................................................................53 Terms and definitions ...........................................................................................................................54 Principle ..................................................................................................................................................55 Interferences ..........................................................................................................................................56 Reagents .................................................................................................................................................67 Apparatus ...............................................................................................................................................77.1 Apparatus for combustion and detection ...........................................................................................77.2 Equipment for adsorption .....................................................................................................................77.3 Equipment for sample preparation ......................................................................................................78 Sample storage and pretreatment........................................................................................................78.1 Sample storage ......................................................................................................................................78.2 Sample pretreatment .............................................................................................................................89 Procedure ...............................................................................................................................................89.1 General ....................................................................................................................................................89.2 Adsorption and inorganic halide removal ...........................................................................................89.3 Combustion ............................................................................................................................................89.4 Initial calibration ....................................................................................................................................99.4.1 General ....................................................................................................................................................99.4.2 Calibration of the entire system ...........................................................................................................99.4.3 Check of argentometric measuring device ...................................................................................... 109.5 Recalibration ....................................................................................................................................... 109.6 Blank determination ........................................................................................................................... 1010 Calculation ........................................................................................................................................... 1110.1 Method of calculation ......................................................................................................................... 1110.1.1 Entire system calibration (according to 9.4.2) ................................................................................. 1110.1.2 Direct argentometric measurement device calibration (according to 9.4.3) ................................ 1110.2 Expression of results ......................................................................................................................... 1211 Precision .............................................................................................................................................. 1212 Test report ........................................................................................................................................... 12Annex A (informative)

Repeatability and reproducibility data ..................................................................... 13A.1 Materials used in the interlaboratory comparison study ............................................................... 13A.2 Interlaboratory comparison results .................................................................................................. 14Annex B (informative)

Storage of activated carbon ...................................................................................... 15Annex C (informative)

Schematic diagram of an AOX apparatus ............................................................... 16Bibliography ..................................................................................................................................................... 17 SIST EN 16166:2013

EN 16166:2012 (E) 3 Foreword This document (EN 16166:2012) 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 16166:2013

EN 16166:2012 (E) 4 Introduction This document is the result of a desk study "Horizontal European standard for determination of AOX in sewage sludge and comparable matrices" in the project "Horizontal" and aims at evaluating the latest developments in assessing AOX in sludge, soil, treated biowaste and neighbouring fields. After an evaluation study, in which the ruggedness of the method was studied, a European wide validation of the draft standard has taken place. The results of the desk studies as well as the evaluation and validation studies have been subject to discussions with all parties involved in the evaluation. 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 Municipal sludge Compost Fresh compost Compost Soil Sludge amended soil Agricultural soil

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 16166:2013

EN 16166:2012 (E) 5 1 Scope This European Standard specifies an empirical method for the direct determination of organically bound chlorine, bromine and iodine (but not fluorine) adsorbed and occluded to the sample matrix. Non-volatile organically bound halogens adsorbable on activated carbon present in the aqueous phase of the sample prior to drying or adsorbed to sample surface are included in the determination.

This European Standard is intended for analysis of sludge, treated biowaste or soil in concentrations ranging from 5 mg/kg dry matter to approximately 6 g/kg dry matter. The exact concentration range covered depends on the instrument used for determination. 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 16179, Sludge, treated biowaste and soil — Guidance for sample pretreatment EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696) EN ISO 5667-15, Water quality — Sampling — Part 15: Guidance on the preservation and handling of sludge and sediment samples (ISO 5667-15) 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 adsorbable organically bound halogens AOX equivalent amount of chlorine, bromine, and iodine contained in organic compounds, expressed as chloride when determined according to this European Standard 4 Principle Activated carbon is added to a dried, homogenised solid sample. Inorganic halides are eluted and at the same time water soluble organic compounds are adsorbed onto the activated carbon by shaking with acidified nitrate solution. The loaded carbon/sample mixture is combusted in an oxygen stream. The hydrogen halides produced are absorbed followed by determination of the halide ions by an argentometric titration, such as microcoulometry. The result is expressed as the mass concentration of chloride. 5 Interferences Sparingly soluble or occluded inorganic halides are included in the determination and may, if present, give a significant positive bias. Adequate washing is essential to remove inorganic interference. NOTE Halogenated substances that volatilise at 105 °C are lost.

Organic bromine and iodine compounds may, during combustion, lead to the formation of elemental bromine or iodine respectively or to the formation of halogen oxides. The determination of these AOX fractions may be incomplete, thus leading to negative bias. SIST EN 16166:2013

EN 16166:2012 (E) 6 6 Reagents Use only reagents of recognised analytical grade and water grade 1 in accordance with EN ISO 3696. The AOX contribution from water, reagents and gases should be significantly lower than the lowest AOX content to be determined. The overall AOX content of water, chemicals, and gases shall be checked by measuring the total blank (see 9.6). 6.1 Activated carbon, grain size approximately 10 µm to 50 µm. For the storage of activated carbon, see Annex B. The blank value of the washed activated carbon shall be less than 15 µg of chloride equivalent per gram of activated carbon. 6.2 Nitric acid, HNO3, ρ = 1,4 g/ml, 65 % (mass fraction) solution. 6.3 Hydrochloric acid, c(HCl) = 0,100 mol/l. The molarity shall be precisely known, since the acid is used for checking the micro-titration (see 9.4.3). 6.4 Sulfuric acid, H2SO4, ρ = 1,84 g/ml. 6.5 Gases for combustion, e.g. oxygen (O2), or a mixture of oxygen and an inert gas. 6.6 Sodium nitrate, NaNO3, for the preparation of stock solution. 6.7 Nitrate stock solution, acidified, c(NaNO3) = 0,2 mol/l. Dissolve 17 g of sodium nitrate (6.6) in water in a 1 000 ml volumetric flask, add 15 ml of nitric acid (6.2), and make up to volume with water. 6.8 Nitrate washing solution, c(NaNO3) = 0,01 mol/l. Pipette 50 ml of the nitrate stock solution (6.7) in a 1 000 ml volumetric flask, and make up to volume with water. 6.9 Methanol, CH3OH. 6.10 4-Chlorophenol stock solution, C6H5ClO, equivalent to AOX = 2,0 g/l. Dissolve 0,725 g of 4-chlorophenol in methanol (6.9) in a 100 ml calibrated flask and make up to volume with methanol (6.9). 6.11 4-Chlorophenol working solutions, equivalent to AOX = 0,1 g/l and 0,5 g/l AOX, respectively. Pipette 5 ml and 25 ml of 4-chlorophenol stock solution (6.10) into two separate 100 ml calibrated flasks, and make up to volume with methanol (6.9). The stock solution (6.10) may be stored for at least one month and the working solutions (6.11) for one week in a refrigerator in glass bottles. SIST EN 16166:2013

EN 16166:2012 (E) 7 7 Apparatus 7.1 Apparatus for combustion and detec
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