CEN/TS 16182:2012

SLOVENSKI STANDARD
01-junij-2012
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Sludge treated biowaste and soil - Determination of nonylphenols (NP) and nonylphenol-
mono- and diethoxylates using gas chromatography with mass selective detection (GC-
MS)
Schlamm, behandelter Bioabfall und Boden - Bestimmung von Nonylphenolen (NP) und
Nonylphenol-Mono- und Diethoxylaten mittels Gaschromatographie mit massenselektiver
Detektion (GC-MS)
Boues, bio-déchets traités et sols - Détermination des nonylphénols et nonylphénol-
mono- et di-éthoxylates par chromatographie en phase gazeuse avec détection sélective
de masse (GC-MS)
Ta slovenski standard je istoveten z: CEN/TS 16182:2012
ICS:
13.030.20 7HNRþLRGSDGNL%ODWR Liquid wastes. Sludge
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

TECHNICAL SPECIFICATION
CEN/TS 16182
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2012
ICS 13.030.01
English Version
Sludge treated biowaste and soil - Determination of
nonylphenols (NP) and nonylphenol-mono- and diethoxylates
using gas chromatography with mass selective detection (GC-
MS)
Boues, biodéchets traités et sols - Détermination des Schlamm, behandelter Bioabfall und Boden - Bestimmung
nonylphénols et nonylphénol-mono- et di-éthoxylates par von Nonylphenolen (NP) und Nonylphenol-Mono- und
chromatographie en phase gazeuse avec détection Diethoxylaten mittels Gaschromatographie mit
sélective de masse (GC-MS) massenselektiver Detektion (GC-MS)
This Technical Specification (CEN/TS) was approved by CEN on 24 April 2011 for provisional application.

The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.

CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available
promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)
until the final decision about the possible conversion of the CEN/TS into an EN is reached.

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, 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 Ref. No. CEN/TS 16182:2012: E
worldwide for CEN national Members.

Contents Page
Foreword .3
Introduction .4
1 Scope .5
2 Normative references .5
3 Principle .5
4 Interferences .5
4.1 Interferences from sampling .5
4.2 Interferences by GC-MS .6
5 Reagents .6
6 Apparatus .8
7 Sample storage and sample pretreatment .9
7.1 Sample storage .9
7.2 Sample pretreatment .9
8 Procedure .9
8.1 Extraction .9
8.1.1 General .9
8.1.2 Extraction of wet sludge samples . 10
8.1.3 Extraction of freeze-dried sludge samples . 10
8.1.4 Extraction of soil and treated biowaste samples . 10
8.1.5 Extraction of freeze-dried soil and treated biowaste samples . 11
8.2 Concentration (optional) . 11
8.3 Clean-up (optional) . 12
8.4 Derivatization . 12
8.5 Blank test . 12
8.6 GC-MS analysis . 13
8.7 Calibration . 13
8.7.1 General . 13
8.7.2 Initial calibration . 13
8.7.3 Verification of calibration . 14
8.8 Analysis of samples and identification . 14
9 Calculation and expression of results . 14
9.1 General . 14
9.2 Calibration . 15
9.3 Calculation . 15
10 Precision . 16
11 Test report . 16
Annex A (informative) Repeatability and reproducibility data . 17
A.1 Materials used in the interlaboratory comparison study . 17
A.2 Interlaboratory comparison results . 18
Annex B (informative) Example of chromatographic conditions and example of a chromatogram . 19
Bibliography . 21

Foreword
This document (CEN/TS 16182:2012) 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.
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.
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 announce this Technical Specification: 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, Turkey and the United Kingdom.

Introduction
Nonylphenols (NP) are mainly found in the environment as degradation products of nonylphenol
polyethoxylates (NPEO). NPEO have many applications as non-ionic detergents in washing and cleaning
agents.
After use NPEO are degraded by de-ethoxylation, resulting in polyethoxylates with fewer ethoxy-groups.
Nonylphenol-diethoxylates (NP2EO), nonylphenol-monoethoxylates (NP1EO) and nonylphenols (NP) are the
last three products in the degradation chain. Due to their significant presence in sewage sludge, all three
components are included in this Technical Specification.
This Technical Specification is applicable for several types of matrices and validated for municipal sewage
sludge (see also Annex A for the results of the validation).
WARNING — Persons using this Technical Specification should be familiar with usual laboratory
practice. This Technical Specification 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 Technical
Specification be carried out by suitably trained staff.
1 Scope
This Technical Specification specifies a method for the determination of nonylphenols (NP), nonylphenol-
monoethoxylates (NP1EO) and nonylphenol-diethoxylates (NP2EO) in sludge, treated biowaste and soil using
GC-MS.
For sludge a limit of detection of 0,1 mg/kg and for soil and treated biowaste 0,02 mg/kg (expressed as dry
matter) may be achieved.
Lower limits of detection may be achieved by concentrating the extract by solvent evaporation.
NOTE 4-tert-octylphenol can also be analysed with this method.
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 15934, Sludge, treated biowaste, soil and waste — Calculation of dry matter fraction after determination of
dry residue or water content
EN 16179, Sludge, treated biowaste and soil — Guidance for sample pretreatment
EN ISO 16720, Soil quality — Pretreatment of samples by freeze-drying for subsequent analysis (ISO 16720)
EN ISO 22892, Soil quality — Guidelines for the identification of target compounds by gas chromatography
and mass spectrometry (ISO 22892)
ISO 8466-1, Water quality — Calibration and evaluation of analytical methods and estimation of performance
characteristics — Part 1: Statistical evaluation of the linear calibration function
3 Principle
After pretreatment, the test sample is extracted by shaking with a mixture of acetone and petroleum ether
(1:1). If necessary, interfering compounds are removed from the extract by a clean-up on a suitable column.
The extract is treated with N-methyl-N-(trimethylsilyl)-trifluoracetamide (MSTFA) reagent for the derivatization
(silylation) of the analytes, and subsequently analysed by gas chromatography and mass selective detection
(GC-MS).
Nonylphenols and nonylphenol-mono- and diethoxylates are identified from the GC fingerprint, the relative
retention times and the relative intensities of two diagnostic ions. The quantification is based on an internal
13 13
standard procedure. The internal standards ( C-labelled 4-n-NP and C-labelled 4-n-NP2EO) are taken
through the whole analytical procedure.
4 Interferences
4.1 Inter
...