SIST EN 16166:2022

SLOVENSKI STANDARD
SIST EN 16166:2022
01-marec-2022
Nadomešča:
SIST EN 16166:2013
Tla, obdelani biološki odpadki in blato - Določevanje adsorbiranih organsko
vezanih halogenov (AOX)
Soil, treated biowaste and sludge - Determination of adsorbed organically bound
halogens (AOX)
Boden, behandelter Bioabfall und Schlamm - Bestimmung von adsorbierten organisch
gebundenen Halogenen (AOX)
Boues, biodéchets traités, sols et sédiments - Détermination des composés organiques
halogénés adsorbables (AOX)
Ta slovenski standard je istoveten z: EN 16166:2021
ICS:
13.030.20 Tekoči odpadki. Blato Liquid wastes. Sludge
13.080.10 Kemijske značilnosti tal Chemical characteristics of
soils
SIST EN 16166:2022 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN 16166:2022

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SIST EN 16166:2022


EN 16166
EUROPEAN STANDARD

NORME EUROPÉENNE

December 2021
EUROPÄISCHE NORM
ICS 13.030.01; 13.080.10 Supersedes EN 16166:2012
English Version

Soil, treated biowaste and sludge - Determination of
adsorbed organically bound halogens (AOX)
Boues, biodéchets traités, sols et sédiments - Boden, behandelter Bioabfall und Schlamm -
Détermination des composés organiques halogénés Bestimmung von adsorbierten organisch gebundenen
adsorbables (AOX) Halogenen (AOX)
This European Standard was approved by CEN on 22 November 2021.

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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.





EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2021 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 16166:2021 E
worldwide for CEN national Members.

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SIST EN 16166:2022
EN 16166:2021 (E)
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 5
4 Principle . 5
5 Interferences . 5
6 Reagents . 6
7 Apparatus . 7
7.1 Apparatus for combustion and detection . 7
7.2 Equipment for adsorption . 7
7.3 Equipment for sample preparation . 7
8 Sample storage and pretreatment . 8
8.1 Sampling and storage . 8
8.2 Sample pretreatment . 8
9 Procedure . 8
9.1 General. 8
9.2 Adsorption and inorganic halide removal . 8
9.3 Combustion . 9
9.4 Chlorine determination, preliminary tests and daily checks . 9
9.5 Blank determination . 10
10 Calculation . 11
10.1 Mass concentration of adsorbed organically bound halogens [ρ (AOX)] in dried
Cl
sample . 11
10.2 Expression of results . 11
11 Precision . 11
12 Test report . 12
Annex A (informative) Repeatability and reproducibility data . 13
A.1 Materials used in the interlaboratory comparison study . 13
A.2 Interlaboratory comparison results . 14
Annex B (informative) Storage of activated carbon . 15
Bibliography . 16

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SIST EN 16166:2022
EN 16166:2021 (E)
European foreword
This document (EN 16166:2021) has been prepared by Technical Committee CEN/TC 444
“Environmental characterization of solid matrices”, 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 2022, and conflicting national standards shall be
withdrawn at the latest by June 2022.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes EN 16166:2012.
In comparison with the previous edition, the following technical modifications have been made:
— Calculation harmonized with EN ISO 9562;
— Initial check and daily check procedure harmonized with EN ISO 9562 and extended to include full
measuring process.
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organisations of the
following countries are bound to implement this European Standard: 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, Republic of North
Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United
Kingdom.
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SIST EN 16166:2022
EN 16166:2021 (E)
Introduction
This document is applicable and validated for several types of matrices as indicated in Table 1 (see also
Annex A for the results of the validation).
NOTE This method can also be applied to other environmental solid matrices, provided the user has verified
the applicability.
Table 1 — Matrices for which this document 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 document should be familiar with usual laboratory practice. This
document 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 document be carried out
by suitably trained staff.
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SIST EN 16166:2022
EN 16166:2021 (E)
1 Scope
This document specifies an operationally defined method for the direct determination of organically
bound halogens (chlorine, bromine and iodine) adsorbed and occluded to the sample matrix. AOX being
a methodologically defined parameter, it is essential that the procedure is applied without any
modification.
This document is intended for analysis of sludge, treated biowaste or soil in concentrations ranging from
5 mg/kg dry matter. The upper limit and exact concentration range covered depend on the
instrumentation used for determination.
NOTE This method can also be applied to other environmental solid matrices, provided the user has verified
the applicability.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at https://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp/ui
3.1
adsorbed organically bound halogens, AOX
amount of chlorine, bromine, and iodine contained as organic compounds in the sample matrix, expressed
as chloride, when determined according to this document
Note 1 to entry: This includes halogenated organic compounds adsorbed at the dry sample matrix as well as water
soluble halogenated compounds that can be adsorbed on to activated carbon.
4 Principle
Activated carbon is added to a dried, homogenized 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 the determination of the halide ions, for
example, by microcoulometric titration. The result is expressed as the mass fraction of chloride.
5 Interferences
Sparingly soluble or occluded inorganic halides are included in the determination and can, if present, give
a significant positive bias. Adequate washing is essential to remove inorganic interference.
Iodide contained in the sample can be adsorbed to the active carbon and not be washed off, thus leading
to positive bias.
Organic bromine and iodine compounds can, 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 can be incomplete, thus leading to negative bias.
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SIST EN 16166:2022
EN 16166:2021 (E)
For samples with significant amounts of volatile, purgeable organic halogen compounds negative bias can
occur. In this case, the sample is to be suspended in water and purged with oxygen at 60 °C for 30 min.
The purged gases are analysed by the analytical instrument. The resulting portion of purgeable organic
halogens is added to the result of the regular determination.
6 Reagents
Use only reagents of recognized analytical grade. Water should be of high purity.
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 9.5).
6.1 Activated carbon, grain size approximately 10 µm to 50 µm.
For information for the storage of activated carbon, see Annex B.
The blank value of the activated carbon, expressed as chloride, shall be less than 15 µg per gram of
activated carbon.
6.2 Nitric acid, HNO , ρ = 1,4 g/ml, 65 % solution.
3
6.3 Hydrochloric acid, c(HCl) = 0,010 mol/l.
6.4 Sulfuric acid, H SO , ρ = 1,84 g/ml.
2 4
6.5 Gases for combustion, e.g. oxygen (O ), or a mixture of oxygen and an inert gas.
2
6.6 Sodium nitrate, NaNO , for the preparation of stock solution.
3
6.7 Nitrate stock solution, acidified, c(NaNO ) = 0,2 mol/l.
3
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.
If stored in a brown glass bottle, the solution is stable for three months.
6.8 Nitrate washing solution, c(NaNO ) = 0,01 mol/l.
3
Pipette 50 ml of the nitrate stock solution (6.7) in a 1 000 ml volumetric flask, and make up to volume
with water.
If stored in a brown glass bottle, the solution is stable for three months.
6.9 4-chlorophenol, stock solution, ρ (AOX) = 200 mg/l.
Cl
Dissolve 72,5 mg of 4-chlorophenol (C H ClO) in water in a 100 ml volumetric flask and make up to
6 5
volume with water.
If stored at (5 ± 3) °C the solution is stable for one month.
6.10 2-Chlorobenzoic acid, stock solution ρ (AOX) = 250 mg/l.
Cl
Dissolve 110,4 mg 2-chlorobenzoic acid in a 100 ml volumetric flask in water and mak
...