SIST EN 16167:2018+AC:2019
(Main)Soil, treated biowaste and sludge - Determination of polychlorinated biphenyls (PCB) by gas chromatography with mass selective detection (GC-MS) and gas chromatography with electron-capture detection (GC-ECD)
Soil, treated biowaste and sludge - Determination of polychlorinated biphenyls (PCB) by gas chromatography with mass selective detection (GC-MS) and gas chromatography with electron-capture detection (GC-ECD)
This draft European Standard specifies a method for quantitative determination of seven selected polychlorinated biphenyls (PCB28, PCB52, PCB101, PCB118, PCB138, PCB153 and PCB180) in sludge, treated biowaste and soil using GC-MS and GC-ECD (see Table 2).
The limit of detection depends on the determinants, the equipment used, the quality of chemicals used for the extraction of the sample and the clean-up of the extract.
Under the conditions specified in this European Standard, limit of application of 1 μg/kg (expressed as dry matter) can be achieved.
Sludge and treated biowaste may differ in properties and also in the expected contamination levels of PCBs and presence of interfering substances. These differences make it impossible to describe one general procedure. This European Standard contains decision tables based on the properties of the sample and the extraction and clean-up procedure to be used.
Boden, behandelter Bioabfall und Schlamm - Bestimmung von polychlorierten Biphenylen (PCB) mittels Gaschromatographie mit Massenspektrometrie-Kopplung (GC-MS) und Gaschromatographie mit Elektroneneinfangdetektion (GC-ECD)
Die vorliegende Europäische Norm legt ein Verfahren für die quantitative Bestimmung von sieben ausgewählten polychlorierten Biphenylen (PCB 28, PCB 52, PCB 101, PCB 118, PCB 138, PCB 153 und PCB 180) in Schlamm, behandeltem Bioabfall und Boden unter Anwendung der GC MS und GC ECD fest (siehe Tabelle 2).
Sols, biodéchets traités et boues - Dosage des polychlorobiphényles (PCBs) par chromatographie en phase gazeuse-spectrométrie gazeuse couplée avec un détecteur de masse (CG-SM) ou un détecteur par capture d'électrons (CG-ECD)
Tla, obdelani biološki odpadki in blato - Določevanje polikloriranih bifenilov (PCB) s plinsko kromatografijo z masno selektivnim detektorjem (GC/MS) in s plinsko kromatografijo z detektorjem z zajetjem elektronov (GC/ECD) (vključno s popravkom AC)
Ta osnutek evropskega standarda določa metodo za kvantitativno določevanje sedmih izbranih polikloriranih bifenilov (PCB28, PCB52, PCB101, PCB118, PCB138, PCB153 in PCB180) v blatu, obdelanih bioloških odpadkih ter tleh z metodama GC-MS in GC-ECD (glej preglednico 2).
Meja detekcije je odvisna od determinant, uporabljene opreme, kakovosti kemikalij, uporabljenih za ekstrakcijo vzorca in očiščenje izvlečka.
Pod pogoji, določenimi v tem evropskem standardu, je mogoče doseči mejo uporabe 1 μg/kg (izraženo kot suha snov).
Blato in obdelani biološki odpadki se lahko razlikujejo glede lastnosti, predvidenih stopenj onesnaženja s polikloriranimi bifenili ter prisotnosti motečih snovi. Zaradi teh razlik ni možen opis enotnega splošnega postopka. Ta evropski standard vključuje tabele odločanja, ki temeljijo na lastnostih vzorca, ter postopek za ekstrakcijo in očiščenje, ki ga je treba uporabiti.
General Information
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Standards Content (Sample)
SLOVENSKI STANDARD
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Soil, treated biowaste and sludge - Determination of polychlorinated biphenyls (PCB) by
gas chromatography with mass selective detection (GC-MS) and gas chromatography
with electron-capture detection (GC-ECD)
Boden, behandelter Bioabfall und Schlamm - Bestimmung von polychlorierten
Biphenylen (PCB) mittels Gaschromatographie mit Massenspektrometrie-Kopplung (GC-
MS) und Gaschromatographie mit Elektroneneinfangdetektion (GC-ECD)
Sols, biodéchets traités et boues - Dosage des polychlorobiphényles (PCBs) par
chromatographie en phase gazeuse-spectrométrie gazeuse couplée avec un détecteur
de masse (CG-SM) ou un détecteur par capture d'électrons (CG-ECD)
Ta slovenski standard je istoveten z: EN 16167:2018+AC:2019
ICS:
13.030.20 7HNRþLRGSDGNL%ODWR Liquid wastes. Sludge
13.080.10 .HPLMVNH]QDþLOQRVWLWDO Chemical characteristics of
soils
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN 16167:2018+AC
EUROPEAN STANDARD
NORME EUROPÉENNE
January 2019
EUROPÄISCHE NORM
ICS 13.030.01; 13.080.10 Supersedes EN 16167:2018
English Version
Soil, treated biowaste and sludge - Determination of
polychlorinated biphenyls (PCB) by gas chromatography
with mass selective detection (GC-MS) and gas
chromatography with electron-capture detection (GC-
ECD)
Sols, biodéchets traités et boues - Dosage des Boden, behandelter Bioabfall und Schlamm -
polychlorobiphényles (PCBs) par chromatographie en Bestimmung von polychlorierten Biphenylen (PCB)
phase gazeuse-spectrométrie gazeuse couplée avec un mittels Gaschromatographie mit
détecteur de masse (CG-SM) ou un détecteur par Massenspektrometrie-Kopplung (GC-MS) und
capture d'électrons (CG-ECD) Gaschromatographie mit Elektroneneinfangdetektion
(GC-ECD)
This European Standard was approved by CEN on 20 March 2018 and includes the Corrigendum issued by CEN on 30 January
2019.
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, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATIO N
EUROPÄISCHES KOMITEE FÜR NORMUN G
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 16167:2018+AC:2019 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and definitions . 6
4 Principle . 7
5 Interferences . 7
5.1 Interference with sampling and extraction . 7
5.2 Interference with GC . 7
6 Safety remarks . 8
7 Reagents . 8
8 Apparatus . 14
9 Sample storage and preservation . 15
9.1 Sample storage . 15
9.2 Sample pretreatment . 15
10 Procedure. 16
10.1 Blank test . 16
10.2 Extraction . 16
10.3 Concentration . 18
10.4 Clean-up of the extract . 19
10.5 Addition of the injection standard . 22
10.6 Gas chromatographic analysis (GC) . 22
10.7 Mass spectrometry (MS) . 23
10.8 Electron capture detection (ECD) . 28
11 Performance characteristics . 30
12 Precision . 30
13 Test report . 30
Annex A (informative) Repeatability and reproducibility data . 31
Annex B (informative) Examples for retention times of PCBs . 33
Annex C (informative) Calculation method for the estimation of total PCB content . 34
Bibliography . 39
European foreword
This document (EN 16167:2018+AC:2019) has been prepared by Technical Committee CEN/TC 444
“Test methods for 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 July 2019, and conflicting national standards shall be
withdrawn at the latest by July 2019.
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 16167:2018™.
This document includes the corrigendum 1 which deletes the mandate information.
The start and finish of text introduced or altered by corrigendum is indicated in the text by tags ˜™
˜deleted text™.
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, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Introduction
Polychlorinated biphenyls (PCB) have been widely used as additives in industrial applications where
chemical stability has been required. This stability on the other hand creates environmental problems
when PCBs are eventually released into the environment. Since some of these PCB compounds are
highly toxic, their presence in the environment (air, water, soil, sediment and waste) is regularly
monitored and controlled. At present determination of PCB is carried out in these matrices in most of
the routine laboratories following the preceding steps for sampling, pretreatment, extraction, clean-up
by measurement of specific PCB by means of gas chromatography in combination with mass
spectrometric detection (GC-MS) or gas chromatography with electron capture detector (GC-ECD).
This European Standard was developed in the European project 'HORIZONTAL'. It is the result of a desk
study “3-12 PCB” and aims at evaluation of the latest developments in assessing PCBs in sludge, soil,
treated biowaste and neighbouring fields. Taken into account the different matrices and possible
interfering compounds, this European Standard does not contain one single possible way of working.
Several choices are possible, in particular relating to clean-up. Detection with both MS-detection and
ECD-detection is possible. Three different extraction procedures are described and 11 clean-up
procedures. The use of internal and injection standards is described in order to have an internal check
on choice of the extraction and clean-up procedure. The method is as far as possible in agreement with
the method described for PAHs (see EN 16181). It has been tested for ruggedness.
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 sewage sludge
Biowaste Compost
Soil Sandy 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.
1 Scope
This draft European Standard specifies a method for quantitative determination of seven selected
polychlorinated biphenyls (PCB28, PCB52, PCB101, PCB118, PCB138, PCB153 and PCB180) in sludge,
treated biowaste and soil using GC-MS and GC-ECD (see Table 2).
Table 2 — Target analytes of this European Standard
Target analyte a
CAS-RN
PCB28 2,4,4'-trichlorobiphenyl 7012–37–5
PCB52 2,2',5,5'-tetrachlorobiphenyl 35693–99–3
PCB101 2,2',4,5,5'-pentachlorobiphenyl 37680–73–2
PCB118 2,3',4,4',5-pentachlorobiphenyl 31508–00–6
PCB138 2,2',3,4,4',5'-hexachlorobiphenyl 35065–28–2
PCB153 2,2',4,4',5,5'-hexachlorobiphenyl 35065–27–1
PCB180 2,2',3,4,4',5,5'-heptachlorobiphenyl 35065–29–3
a
CAS-RN Chemical Abstracts Service Registry Number.
The limit of detection depends on the determinants, the equipment used, the quality of chemicals used
for the extraction of the sample and the clean-up of the extract.
Under the conditions specified in this European Standard, limit of application of 1 µg/kg (expressed as
dry matter) can be achieved.
Sludge and treated biowaste may differ in properties and also in the expected contamination levels of
PCBs and presence of interfering substances. These differences make it impossible to describe one
general procedure. This European Standard contains decision tables based on the properties of the
sample and the extraction and clean-up procedure to be used.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
consti
...
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