CEN/TS 16183:2012
(Main)Sludge, treated biowaste and soil - Determination of selected phthalates using capillary gas chromatography with mass spectrometric detection (GC-MS)
Sludge, treated biowaste and soil - Determination of selected phthalates using capillary gas chromatography with mass spectrometric detection (GC-MS)
This Technical Specification specifies a method for the determination of selected phthalates in sludge, treated biowaste and soil, after extraction and gas chromatographic analysis with mass spectrometric detection.
The method is applicable for the determination of phthalates (see Table 2) at the lowest mass content of 0,1 mg/kg to 0,5 mg/kg (expressed as dry matter), depending on the individual substance.
The applicability of the method to other phthalates not specified in Table 2 is not excluded except the isomeric mixtures e.g. DiNP (Di-isononylphthalate), but shall be verified in each case.
Schlamm, behandelter Bioabfall und Boden - Bestimmung ausgewählter Phthalate mittels kapillarer Gaschromatographie mit massenspektrometrischer Detektion (GC-MS)
Diese Technische Spezifikation legt ein Verfahren zur Bestimmung ausgewählter Phthalate in Schlamm,
behandeltem Bioabfall und Boden nach Extraktion und gaschromatographischer Analyse mit
massenspektrometrischer Detektion fest.
Das Verfahren ist für die Bestimmung von Phthalaten (siehe Tabelle 2) mit einem Mindestmassengehalt von
0,1 mg/kg bis 0,5 mg/kg (angegeben als Trockenmasse), geeignet, abhängig von der jeweiligen Substanz.
Die Anwendbarkeit des Verfahrens auf weitere, in Tabelle 2 nicht angegebene Phthalate, ist bis auf die
Isomerengemische, wie z. B. DINP (Di-isononylphthalat), nicht ausgeschlossen, muss aber für jeden Fall
nachgewiesen werden.
Boues, biodéchets traités et sols - Détermination de certains phtalates par chromatographie en phase gazeuse capillaire avec détection par spectrométrie de masse (CG-SM)
La présente Spécification technique spécifie une méthode pour la détermination de certains phtalates dans
les boues, les biodéchets traités et les sols, après extraction et analyse par chromatographie en phase
gazeuse/spectrométrie de masse.
La méthode est applicable pour la détermination de phtalates (voir Tableau 2) à la plus faible teneur massique
de 0,1 mg/kg à 0,5 mg/kg (exprimée en teneur en matière sèche), selon la substance individuelle.
L'applicabilité de la méthode à d'autres phtalates non spécifiés dans le Tableau 2 n'est pas exclue, à
l'exception des mélanges isomériques tels que DiNP (Di-isononylphtalate), mais elle doit être vérifiée dans
chaque cas.
Blato, obdelani biološki odpadki in tla - Določevanje izbranih ftalatov s kapilarno plinsko kromatografijo z masno selektivno detekcijo (GC/MS)
Ta tehnična specifikacija opredeljuje metodo za določevanje izbranih ftalatov v blatu, obdelanih bioloških odpadkih in tleh po ekstrakciji in plinski kromatografiji z masno selektivno detekcijo. Ta metoda se uporablja za določevanje ftalatov (glejte preglednico 2) pri najnižji masni vsebnosti od 0,1 mg/kg do 0,5 mg/kg (izraženo kot suha snov), odvisno od posamezne snovi. Uporabnost metode pri drugih ftalatih, ki niso navedeni v preglednici 2, ni izključena, razen pri mešanicah izomerov, npr. DiNP (di-izononilftalat), vendar mora biti preverjena pri vsakem posameznem primeru.
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-junij-2012
%ODWRREGHODQLELRORãNLRGSDGNLLQWOD'RORþHYDQMHL]EUDQLKIWDODWRYVNDSLODUQR
SOLQVNRNURPDWRJUDILMR]PDVQRVHOHNWLYQRGHWHNFLMR *&06
Sludge, treated biowaste and soil - Determination of selected phthalates using capillary
gas chromatography with mass spectrometric detection (GC-MS)
Schlamm, behandelter Bioabfall und Boden - Bestimmung ausgewählter Phthalate
mittels kapillarer Gaschromatographie mit massenspektrometrischer Detektion (GC-MS)
Boues, bio-déchets traités et sols - Détermination de certains phtalates par
chromatographie en phase gazeuse capillaire avec détection par spectrométrie de
masse (CG-SM)
Ta slovenski standard je istoveten z: CEN/TS 16183:2012
ICS:
13.030.20 7HNRþLRGSDGNL%ODWR Liquid wastes. Sludge
13.080.10 .HPLMVNH]QDþLOQRVWLWDO Chemical characteristics of
soils
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
TECHNICAL SPECIFICATION
CEN/TS 16183
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
February 2012
ICS 13.030.01
English Version
Sludge, treated biowaste and soil - Determination of selected
phthalates using capillary gas chromatography with mass
spectrometric detection (GC-MS)
Boues, biodéchets traités et sols - Détermination de Schlamm, behandelter Bioabfall und Boden - Bestimmung
certains phtalates par chromatographie en phase gazeuse ausgewählter Phthalate mittels kapillarer
capillaire avec détection par spectrométrie de masse (CG- Gaschromatographie mit massenspektrometrischer
SM) 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 16183:2012: E
worldwide for CEN national Members.
Contents Page
Foreword .3
Introduction .4
1 Scope .5
2 Normative references .5
3 Principle .6
4 Interferences .6
4.1 General .6
4.2 Interferences during sampling .6
4.3 Cross contamination .6
4.4 Interferences in gas chromatography .6
5 Reagents .6
6 Apparatus .8
7 Sampling and sample storage . 10
8 Procedure . 10
8.1 Preparation of glass apparatus . 10
8.2 Drying of the sample . 10
8.2.1 General . 10
8.2.2 Freeze drying . 10
8.2.3 Drying with sodium sulfate (Na SO ) . 11
2 4
8.3 Extraction . 11
8.4 Clean-up . 11
8.5 Gas chromatography . 12
8.6 Blank monitoring . 12
8.7 Identification of individual compounds . 12
9 Calibration . 13
9.1 General . 13
9.2 Calibration with internal standard. 14
9.3 Verification of calibration . 14
10 Calculation . 14
11 Expression of results . 16
12 Precision . 16
13 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 a reference solution for multipoint calibration . 20
Annex C (informative) Examples for gas chromatographic conditions . 22
C.1 Examples for capillary columns . 22
C.2 Example of gas chromatographic conditions . 22
Annex D (informative) Flow scheme of the determination of phthalates . 24
Bibliography . 25
Foreword
This document (CEN/TS 16183:2012) 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
This Technical Specification 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 Technical Specification is applicable and validated
Matrix Materials used for validation
Sludge Municipal sludge
Biowaste Fresh compost
Soil Sludge amended soil
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 selected phthalates in sludge, treated
biowaste and soil, after extraction and gas chromatographic analysis with mass spectrometric detection.
The method is applicable for the determination of phthalates (see Table 2) at the lowest mass content of
0,1 mg/kg to 0,5 mg/kg (expressed as dry matter), depending on the individual substance.
The applicability of the method to other phthalates not specified in Table 2 is not excluded except the isomeric
mixtures e. g. DiNP (Di-isononylphthalate), but shall be verified in each case.
Table 2 — Phthalates that can be determined according to CEN/TS 16183
a
No Name Formula Abbreviation Molar mass CAS-RN
g/mol
1 Dimethylphthalate C H O DMP 194,2 00131-11-3
10 10 4
2 Diethylphthalate C H O DEP 222,2 00084-66-2
12 14 4
3 Dipropylphthalate C H O DPP 250,3 00131-16-8
14 18 4
4 Di-(2-methyl- C H O DiBP 278,4 00084-69-5
16 22 4
propyl)phthalate
5 Dibutylphthalate C H O DBP 278,4 00084-74-2
16 22 4
6 Butylbenzylphthalate C H O BBzP 312,4 00085-68-7
19 20 4
C H O
7 Dicyclohexylphthalate DCHP 330,4 00084-61-7
20 26 4
8 Di-(2-ethylhexyl)phthalate C H O DEHP 390,6 00117-81-7
24 38 4
9 Dioctylphthalate C H O DOP 390,6 00117-84-0
24 38 4
10 Didecylphthalate C H O DDcP 446,7 00084-77-5
28 46 4
11 Diundecylphthalate C H O DUP 474,4 03648-20-2
30 50 4
a CAS-RN Chemical Abstracts Service Registry Number.
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 5667-13, Water quality — Sampling — Part 13: Guidance on sampling of sludges (ISO 5667-13)
EN ISO 5667-15, Water quality — Sampling — Part 15: Guidance on the preservation and handling of sludge
and sediment samples (ISO 5667-15)
EN ISO 22892, Soil quality — Guidelines for the identification of target compounds by gas chromatography
and mass spectrometry (ISO 22892)
ISO 10381-2, Soil quality — Sampling — Part 2: Guidance on sampling techniques
3 Principle
The dried sample, dried by freeze-drying or with sodium sulfate is extracted with ethyl acetate on the shaking
device. An aliquot of the extract is cleaned with aluminium oxide (if necessary) followed by gas
chromatographic separation using capillary columns and identification and quantification of
...
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