Soil, treated biowaste and sludge - Determination of dioxins and furans and dioxin-like polychlorinated biphenyls by gas chromatography with high resolution mass selective detection (HR GC-MS)

This draft European Standard specifies a method for quantitative determination of 17 2,3,7,8-chlorine substituted dibenzo-p-dioxins and dibenzofurans and dioxin-like polychlorinated biphenyls in sludge, treated biowaste and soil using liquid column chromatographic clean-up methods and GC/HRMS.
The analytes to be determined with this European Standard are listed in Table 1.
(...)
The limit of detection depends on the kind of sample, the congener, the equipment used and the quality of chemicals used for extraction and clean-up. Under the conditions specified in this European Standard, limits of detection better than 1 ng/kg (expressed as dry matter) can be achieved.
This method is "performance based". It is allowed to modify the method if all performance criteria given in this method are met.
NOTE   In principle this method can also be applied for sediments, mineral wastes and for vegetation. It is the responsibility of the user of this European Standard to validate the application for these matrices. For measurement in complex matrices like fly ashes adsorbed on vegetation it can be necessary to further improve the clean-up. This can also apply to sediments and mineral wastes.

Boden, behandelter Bioabfall und Schlamm - Bestimmung von Dioxinen und Furanen sowie Dioxin-vergleichbaren polychlorierten Biphenylen mittels Gaschromatographie und hochauflösender massenspektrometrischer Detektion (HR GC-MS)

Dieses Dokument legt ein Verfahren fest zur quantitativen Bestimmung von 17 2,3,7,8 chlorsubstituierten Dibenzo p dioxinen und Dibenzofuranen sowie dioxinähnlichen polychlorierten Biphenylen in Schlamm, behandeltem Bioabfall und Boden mittels flüssigchromato¬graphischer Reinigungsverfahren und GC/HRMS.
Die nach diesem Dokument zu bestimmenden Analyten enthält Tabelle 1.

Sols, bio-déchets traités et boues - Dosage des dioxines et furanes et polychlorobiphényles de type dioxine par chromatographie en phase gazeuse avec spectrométrie de masse à haute résolution (HR CG-SM)

Le présent document définit une méthode pour le dosage de 17 polychlorodibenzo-p-dioxines et polychlorodibenzofuranes substitués par des atomes de chlore en 2,3,7,8 et de polychlorobiphényles de type dioxine dans les boues, les biodéchets traités et les sols à l’aide de méthodes de purification chromatographique sur colonne et d’analyse par chromatographie en phase gazeuse avec spectrométrie de masse à haute résolution (CG/SMHR).
Les analytes devant être dosés selon le présent document sont répertoriés dans le Tableau 1.
(Tableau 1) ...
La limite de détection dépend du type d’échantillon, du congénère, de l’équipement utilisé et de la qualité des produits chimiques utilisés pour l’extraction et la purification. Dans les conditions spécifiées dans le présent document, des limites de détection supérieures à 1 ng/kg (exprimées en matière sèche) peuvent être atteintes.
Cette méthode est « basée sur la performance ». Il est permis de modifier la méthode si tous les critères de performance donnés dans cette méthode sont remplis.
NOTE   En principe, cette méthode peut être également appliquée pour les sédiments, les déchets minéraux et les végétaux. Il appartient à l’utilisateur du présent document de valider l’application pour ces matrices. Pour les mesures dans les matrices complexes telles que les cendres volantes d’incinération adsorbées sur des végétaux, une amélioration de la purification peut s’avérer nécessaire. Ceci peut également s’appliquer aux sédiments et aux déchets minéraux.

Tla, obdelani biološki odpadki in blato - Določevanje dioksinov in furanov ter dioksinom podobnih polikloriranih bifenilov s plinsko kromatografijo z masno selektivnim detektorjem visoke ločljivosti (HR GC/MS)

Ta osnutek evropskega standarda določa metodo za kvantitativno določevanje 17 2,3,7,8-klor substituiranih dibenzo-p-dioksinov in dibenzofuranov ter dioksinom podobnih polikloriranih bifenilov v blatu, obdelanih bioloških odpadkih in tleh z metodami kromatografskega čiščenja v koloni, napolnjeni s tekočino, in plinsko kromatografijo/masno spektrometrijo visoke ločljivosti (GC/HRMS).
Analiti, ki jih je treba določiti s tem evropskim standardom, so navedeni v tabeli 1.
(...)
Meja detekcije je odvisna od vrste vzorca, kongenerja, uporabljene opreme in kakovosti kemikalij, uporabljenih pri ekstrakciji in čiščenju. Pod pogoji, določenimi v tem evropskem standardu, je mogoče doseči meje detekcije, boljše od 1 ng/kg (izraženo kot suha snov).
Ta metoda »temelji na učinkovitosti«. Metodo je dovoljeno spremeniti, če so izpolnjena vsa merila učinkovitosti, ki so v njej navedena.
OPOMBA:   Načeloma je to metodo mogoče uporabiti tudi za sedimente, mineralne odpadke in rastlinje. Uporabnik tega evropskega standarda mora poskrbeti za potrditev uporabe teh matric. Pri meritvah v kompleksnih matricah, kot je elektrofiltrski pepel, adsorbiran v rastlinju, je mogoče potrebno dodatno izboljšanje čiščenja. To lahko velja tudi za sedimente in mineralne odpadke.

General Information

Status
Published
Public Enquiry End Date
02-Jan-2018
Publication Date
30-Jan-2019
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
29-Jan-2019
Due Date
05-Apr-2019
Completion Date
31-Jan-2019

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Boden, behandelter Bioabfall und Schlamm - Bestimmung von Dioxinen und Furanen sowie Dioxin-vergleichbaren polychlorierten Biphenylen mittels Gaschromatographie und hochauflösender massenspektrometrischer Detektion (HR GC-MS)Sols, bio-déchets traités et boues - Dosage des dioxines et furanes et polychlorobiphényles de type dioxine par chromatographie en phase gazeuse avec spectrométrie de masse à haute résolution (HR CG-SM)Soil, treated biowaste and sludge - Determination of dioxins and furans and dioxin-like polychlorinated biphenyls by gas chromatography with high resolution mass selective detection (HR GC-MS)71.040.50Fizikalnokemijske analitske metodePhysicochemical methods of analysis13.080.10Chemical characteristics of soils13.030.20Liquid wastes. SludgeICS:Ta slovenski standard je istoveten z:EN 16190:2018SIST EN 16190:2019en,fr,de01-marec-2019SIST EN 16190:2019SLOVENSKI

STANDARDSIST-TS CEN/TS 16190:20121DGRPHãþD
SIST EN 16190:2019
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16190
December 2018 ICS 13.030.01; 13.080.10 Supersedes CEN/TS 16190:2012
English Version

Soil, treated biowaste and sludge - Determination of dioxins and furans and dioxin-like polychlorinated biphenyls by gas chromatography with high resolution mass selective detection (HR GC-MS)

Sols, bio-déchets traités et boues - Dosage des dioxines et furanes et polychlorobiphényles de type dioxine par chromatographie en phase gazeuse avec spectrométrie de masse à haute résolution (HR CG-SM)

Boden, behandelter Bioabfall und Schlamm - Bestimmung von Dioxinen und Furanen sowie Dioxin-vergleichbaren polychlorierten Biphenylen mittels Gaschromatographie und hochauflösender massenspektrometrischer Detektion (HR GC-MS) This European Standard was approved by CEN on 23 October 2018.

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.

This document was corrected and reissued by the CEN-CENELEC Management Centre on 22 January 2019.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Rue de la Science 23,

B-1040 Brussels © 2018 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16190:2018 E SIST EN 16190:2019

EN 16190:2018 (E) 2 Contents Page European foreword ....................................................................................................................................................... 4 Introduction .................................................................................................................................................................... 5 1 Scope .................................................................................................................................................................... 6 2 Normative references .................................................................................................................................... 7 3 Terms and definitions ................................................................................................................................... 7 4 Abbreviations ................................................................................................................................................... 7 5 Principle ............................................................................................................................................................. 8 6 Reagents ............................................................................................................................................................. 8 7 Apparatus and materials .............................................................................................................................. 9 8 Sample storage and sample pretreatment .......................................................................................... 10 8.1 Sample storage .............................................................................................................................................. 10 8.2 Sample pretreatment .................................................................................................................................. 10 9 Extraction and clean-up ............................................................................................................................. 11 9.1 General ............................................................................................................................................................. 11 9.2 Extraction ........................................................................................................................................................ 11 9.3 Clean-up ........................................................................................................................................................... 13 9.3.1 General ............................................................................................................................................................. 13 9.3.2 Gel permeation chromatography ........................................................................................................... 13 9.3.3 Multilayer column ........................................................................................................................................ 13 9.3.4 Sulphuric acid treatment ........................................................................................................................... 13 9.3.5 Activated carbon column ........................................................................................................................... 13 9.3.6 Aluminium oxide column .......................................................................................................................... 13 9.3.7 Removal of sulphur ..................................................................................................................................... 13 9.4 Final concentration of cleaned sample extract ................................................................................. 13 9.5 Addition of recovery standard ................................................................................................................ 14 10 HRGC/HRMS analysis .................................................................................................................................. 14 10.1 General ............................................................................................................................................................. 14 10.2 Gas chromatographic analysis ................................................................................................................ 15 10.3 Mass spectrometric detection ................................................................................................................. 15 10.4 Minimum requirements for identification of PCDF/PCDD and PCB .......................................... 16 10.5 Minimum requirements for quantification of PCDF/PCDD and PCB ......................................... 17 10.6 Calibration of the HRGC/HRMS system ................................................................................................ 18 10.6.1 General ............................................................................................................................................................. 18 10.6.2 Calibration for 2,3,7,8-congeners ........................................................................................................... 18 10.6.3 Calibration for sum of homologue groups .......................................................................................... 19 10.7 Quantification of HRGC/HRMS results .................................................................................................. 20 10.7.1 Quantification of concentrations of 2,3,7,8-congeners .................................................................. 20 10.7.2 Quantification of recovery rates of 13C-labelled standards .......................................................... 20 10.7.3 Quantification of sum of homologue groups ...................................................................................... 21 10.7.4 Calculation of the toxic equivalent......................................................................................................... 21 10.7.5 Calculation of the limit of detection and the limit of quantification .......................................... 22 11 Expression of results ................................................................................................................................... 22 SIST EN 16190:2019

EN 16190:2018 (E) 3 12 Precision .......................................................................................................................................................... 22 13 Test report ...................................................................................................................................................... 23 Annex A (informative)

Toxic equivalency factor (TEF).................................................................................. 24 Annex B (informative)

Examples of extraction and clean-up methods .................................................... 26 B.1 Example A ........................................................................................................................................................ 26 B.1.1 General ............................................................................................................................................................. 26 B.1.2 Chemicals ......................................................................................................................................................... 26 B.1.3 Procedure ........................................................................................................................................................ 27 B.2 Example B: Approved clean-up methods ............................................................................................. 32 Annex C (informative)

Examples of operation of GC/HRMS determination — Example ................... 34 C.1 General ............................................................................................................................................................. 34 C.2 Gas chromatographic analysis ................................................................................................................. 34 C.3 Mass spectrometric detection .................................................................................................................. 35 Annex D (informative)

Repeatability and reproducibility data .................................................................. 38 D.1 Materials used in the interlaboratory comparison study .............................................................. 38 D.2 Interlaboratory comparison results ...................................................................................................... 38 D.3 Calculation of toxicity factors on the basis of interlaboratory data ........................................... 43 Bibliography ................................................................................................................................................................. 45

SIST EN 16190:2019

EN 16190:2018 (E) 4 European foreword This document (EN 16190:2018) 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 document shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by June 2019, and conflicting national standards shall be withdrawn at the latest by June 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 CEN/TS 16190:2012. 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 SIST EN 16190:2019

EN 16190:2018 (E) 5 Introduction Two groups of related chlorinated aromatic ethers are known as polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs); they consist of a total of 210 individual substances (congeners): 75 PCDD and 135 PCDF. A group of chlorinated aromatic compounds similar to polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) is known as polychlorinated biphenyls (PCBs) which consist of 209 individual substances. PCDD and PCDF can form in the combustion of organic materials; they also occur as undesirable by-products in the manufacture or further processing of chlorinated organic chemicals. PCDD/PCDF enter the environment via these emission paths and through the use of contaminated materials. In fact, they are universally present at very small concentrations. The 2,3,7,8-substituted congeners are toxicologically significant. Toxicologically much less significant than the tetrachlorinated to octachlorinated dibenzo-p-dioxins/dibenzofurans are the 74 monochlorinated to trichlorinated dibenzo-p-dioxins/dibenzofurans. PCB have been produced over a period of approximately 50 years until the end of the 1990s for the purpose of different use in open and closed systems, e.g. as electrical insulators or dielectric fluids in capacitors and transformers, as specialized hydraulic fluids, as a plasticizer in sealing material. Worldwide more than one million tons of PCB were produced. PCDD/PCDF as well as PCB are emitted during thermal processes as e.g. waste incineration. In 1997 a group of experts of the World Health Organization (WHO) fixed toxicity equivalent factors (TEF) for PCDD and twelve PCB, known as dioxin-like PCB (see Annex A). These twelve dioxin-like PCB consist of four non-ortho PCB and eight mono-ortho PCB (no or only one chlorine atoms in 2-, 2’-, 6- and 6’-position), having a planar or mostly planar structure. Dioxin-like PCB can contribute considerably to the total WHO-TEQ. Only skilled operators who are trained in handling highly toxic compounds should apply the method described in this document. This document is applicable for several types of matrices and validated for municipal sludge (see also Annex A for the results of the validation). WARNING — Persons using this document should be familiar with normal 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. SIST EN 16190:2019

EN 16190:2018 (E) 6 1 Scope This document specifies a method for quantitative determination of 17 2,3,7,8-chlorine substituted dibenzo-p-dioxins and dibenzofurans and dioxin-like polychlorinated biphenyls in sludge, treated biowaste and soil using liquid column chromatographic clean-up methods and GC/HRMS. The analytes to be determined with this document are listed in Table 1. Table 1 — Analytes and their abbreviations Substance Abbreviation Tetrachlorodibenzo-p-dioxin TCDD Pentachlorodibenzo-p-dioxin PeCDD Hexachlorodibenzo-p-dioxin HxCDD Heptachlorodibenzo-p-dioxin HpCDD Octachlorodibenzo-p-dioxin OCDD Tetrachlorodibenzofuran TCDF Pentachlorodibenzofuran PeCDF Hexachlorodibenzofuran HxCDF Heptachlorodibenzofuran HpCDF Octachlorodibenzofuran OCDF Polychlorinated biphenyl PCB Trichlorobiphenyl TCB Tetrachlorobiphenyl TeCB Pentachlorobiphenyl PeCB Hexachlorobiphenyl HxCB Heptachlorobiphenyl HpCB Decachlorobiphenyl DecaCB The limit of detection depends on the kind of sample, the congener, the equipment used and the quality of chemicals used for extraction and clean-up. Under the conditions specified in this document, limits of detection better than 1 ng/kg (expressed as dry matter) can be achieved. This method is “performance based”. It is allowed to modify the method if all performance criteria given in this method are met. NOTE In principle this method can also be applied for sediments, mineral wastes and for vegetation. It is the responsibility of the user of this document to validate the application for these matrices. For measurement in complex matrices like fly ashes adsorbed on vegetation it can be necessary to further improve the clean-up. This can also apply to sediments and mineral wastes. SIST EN 16190:2019

EN 16190:2018 (E) 7 2 Normative references The following documents are referred to in the text in such a way that some or all of their content constitutes requirements of this document. 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 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 http://www.electropedia.org/

ISO Online browsing platform: available at http://www.iso.org/obp 3.1 internal standard 13C12-labelled 2,3,7,8-PCDD/PCDF analogue added to samples prior to extraction against which the concentrations of native PCDD and PCDF are calculated [SOURCE: ISO 18073:2004, 3.1.5] 3.2 recovery standard 13C12-labelled 2,3,7,8-chloro-substituted PCDD/PCDF, added before injection into the GC [SOURCE: ISO 18073:2004, 3.1.12] 4 Abbreviations I-TEF NATO/CCMS International toxic equivalent factor proposed by NATO-CCMS in 1988 (for detailed description, see Annex A) I-TEQ International toxic equivalent obtained by multiplying the mass determined with the corresponding I-TEF including PCDD and PCDF (for detailed description, see Annex A). Should only be used for comparison with older data PCDD/PCDF or PCDD/F Polychlorinated dibenzo-p-dioxins/dibenzofurans WHO-TEF Toxic equivalent factor proposed by WHO in 2005 (for detailed description, see Annex A) WHO-TEQ Toxic equivalent obtained by multiplying the mass determined with the corresponding WHO-TEF including PCDD, PCDF and PCB (for detailed description, see Annex D). WHO-TEQPCB, WHO-TEQPCDD/PCDF should be used to distinguish different compound classes SIST EN 16190:2019

EN 16190:2018 (E) 8 5 Principle This document is based on the use of gas chromatography/mass spectrometry combined with the isotope dilution technique to enable the separation, detection and quantification of PCDD/PCDF and dioxin-like PCB in sludge, biowaste and soil. For the isotope dilution method 17 labelled PCDD/PCDF and 12 labelled PCB internal standards are used. The extracts for the GC-MS measurements contain one or two recovery standards. The gas chromatographic parameters offer information which enables the identification of congeners (position of chlorine substitutes) whereas the mass spectrometric parameters enable the differentiation between isomers with different numbers of chlorine substitutes and between dibenzo-p-dioxins, furans and PCB. 13C12-labelled PCDD/PCDF and PCB congeners are added to the sample prior to extraction and HRGC/HRMS measurement. Losses during extraction and clean-up are detected and compensated by using these added congeners as internal standards for quantification together with recovery standards which are added just before the HRGC/HRMS analysis. For the determination of these substances it is necessary to separate PCB from PCDD/PCDF and vice versa. The main purpose of the clean-up procedure of the raw sample extract is the removal of sample matrix components, which may overload the separation method, disturb the quantification or otherwise severely impact the performance of the identification and quantification method and the separation of PCDD/PCDF from dioxin-like PCB. Furthermore, the enrichment of the analytes in the final sample extract is achieved. Extraction procedures are usually based on Soxhlet or equivalent extraction methods of dried, preferably freeze-dried, samples. Sample clean-up is usually carried out by multi-column liquid chromatographic techniques using different adsorbents. The determination of PCDD/PCDF and PCB is based on quantification by the isotope-dilution technique using HRGC/HRMS. 6 Reagents 6.1 Chemicals: Solvents used for extraction and clean-up shall be of pesticide grade or equivalent quality and checked for blanks. Adsorbents like aluminium oxide, silica gel, diatomaceous earth and others used for clean-up shall be of analytical grade quality or better and pre-cleaned and activated if necessary. NOTE See Annex B for a specific list of solvents and chemicals. 6.2 Standards: — 13C-spiking solution for PCDD/PCDF (internal Standard); — 13C-spiking solution for PCB (internal Standard); — calibration solutions PCDD/PCDF; — calibration solutions PCB; — recovery standard PCDD/PCDF; — recovery standard PCB. NOTE See Annex B for examples of concentration of the standard solutions. SIST EN 16190:2019

EN 16190:2018 (E) 9 7 Apparatus and materials The apparatus and materials listed below are meant as minimum requirements for “conventional” sample treatment with Soxhlet extraction and column chromatographic clean-up. Additional apparatus and materials may be necessary due to different methods of sample extraction and clean-up methods. 7.1 Equipment for sample preparation: 7.1.1 Laboratory fume hood, of sufficient size to contain the sample preparation equipment listed below. 7.1.2 Desiccator. 7.1.3 Balances, consisting of an analytical type capable of weighing 0,1 mg and a top-loading type capable of weighing 10 mg. 7.2 Soxhlet extractor: 7.2.1 Soxhlet, 50 mm internal diameter, 150 ml or 250 ml capacity with 500 ml round bottom flask. 7.2.2 Thimble, 43 mm × 123 mm, to fit Soxhlet. 7.2.3 Hemispherical heating mantle, to fit 500 ml round-bottom flask. 7.3 Clean-up apparatus: 7.3.1 Disposable pipettes, either disposable Pasteur pipettes, or disposable serological pipettes. 7.3.2 Glass chromatographic columns of the following sizes: — 150 mm length × 8 mm internal diameter, with coarse-glass frit or glass-wool plug, 250 ml reservoir and glass or polytetrafluoroethylene (PTFE) stopcock; — 200 mm length × 15 mm internal diameter, with coarse-glass frit or glass-wool plug, 250 ml reservoir and glass or PTFE stopcock; — 300 mm length × 25 mm internal diameter, with coarse-glass frit or glass-wool plug, 300 ml reservoir and glass or PTFE stopcock. 7.3.3 Oven, capable of maintaining a constant temperature (±5 °C) in the range of 105 °C to 450 °C for baking and storage of adsorbents. 7.4 Concentration apparatus: 7.4.1 Rotary evaporator, equipped with a variable temperature water bath and: — vacuum source for rotary evaporator equipped with shutoff valve at the evaporator and vacuum gauge; — recirculating water pump and chiller, providing cooling water of (9 ± 4) °C (use of tap water for cooling the evaporator wastes large volumes of water and can lead to inconsistent performance as water temperatures and pressures vary); — round-bottom flask, 100 ml and 500 ml or larger, with ground-glass fitting compatible with the rotary evaporator. SIST EN 16190:2019

EN 16190:2018 (E) 10 7.4.2 Nitrogen blowdown apparatus, equipped with either a water bath controlled in the range of 30 °C to 60 °C or a heated stream of nitrogen or of another suitable inert gas, installed in a fume hood. 7.4.3 Kuderna-Danish1) concentrator. 7.4.4 Sample vials, of the following types: — amber glass, nominated volume 2 ml to 5 ml, with PTFE-lined screw cap; — glass, 0,3 ml, conical, with PTFE-lined screw or crimp cap. 7.5 Other equipment: 7.5.1 Gas chromatograph, equipped with a splitless or on-column or temperature programmed injection port for the use with capillary columns, and an oven temperature programme which enables isothermal hold. 7.5.2 GC column for PCDD/PCDF and for isomer specificity for 2,3,7,8-TCDD (e.g. 60 m length × 0,32 mm internal diameter; 0,25 µm; 5 % phenyl, 94 % methyl, 1 % vinyl silicone bonded-phase fused-silica capillary column). 7.5.3 Mass spectrometer, 28 eV to 80 eV electron impact ionization, capable of repetitively selectively monitoring of twelve exact masses minimum at high resolution (>10 000) during a period of approximately 1 s. 7.5.4 Data system, capable of collecting, recording, and storing mass spectrometric data. 8 Sample storage and sample pretreatment 8.1 Sample storage Samples should be stored in suitable containers with an appropriate closure material such as polytetrafluoroethylene (PTFE). Samples to be frozen may be stored in aluminium containers pre-cleaned by heating to 450 °C for minimum 4 h or by rinsing with a non-chlorinated solvent. Samples should be kept cold (<8 °C) and in the dark. The sample pretreatment should take place within three days of sampling. If not achievable, samples may be frozen (–18 °C) directly after sampling and kept frozen before sample pretreatment. 8.2 Sample pretreatment Drying and homogenization should be carried out according to EN 16179, if not otherwise specified. Store the ground material in a desiccator or a tightly closed glass container. Determination of water content shall be carried out according to EN 15934.

1) Kuderna Danish is an example of a suitable product available commercially. This information is given for the convenience of users of this document and does not constitute an endorsement by CEN of this product. SIST EN 16190:2019

EN 16190:2018 (E) 11 9 Extraction and clean-up 9.1 General In this document the minimum requirements for extraction and clean-up to be met are described as well as examples of operation. The analyst may use any of the procedures given below and in Annex C or any suitable alternative procedures. The determination of PCDD/PCDF is based on quantification by the isotope-dilution technique using HRGC/HRMS. 13C12-labelled 2,3,7,8-chlorine substituted PCDD/PCDF congeners are added at different stages of the whole method. Losses during extraction and clean-up can be detected and compensated by using these added congeners as internal standards for quantification together with recovery standards which are added just before the HRGC/HRMS analysis. However, due to possible differences in the binding and adsorption characteristics between the native PCDD/PCDF and the 13C12-labelled congeners, which are added during analysis, complete substantiation of the extraction efficiency and compensation of losses during clean-up is not ensured. Therefore, in addition the applied methods shall be validated thoroughly. Examples of well-proven extraction and clean-up methods are given in Annex C. The main purpose of the clean-up procedure of the raw sample extract is the removal of sample matrix components, which may overload the separation method, disturb the quantification or otherwise severely impact the performance of the identification and quantification method and to separate dioxin-like PCB from PCDD/PCDF. Furthermore, an enrichment of the analytes in the final sample extract is achieved. Extraction procedures are normally based on soxhlet extraction of the < 2 mm fraction of the dry and ground or sieved solid sample. Sample clean-up is usually carried out by multi-column liquid chromatographic techniques using different adsorbents. In principle any clean-up method can be used which recovers the analytes in sufficient quantities. Furthermore, the final sample extract shall not affect adversely the performance of the analytical system or the quantification step. However, all applied methods shall be tested thoroughly and shall pass a set of method validation requirements before they can be employed (see Annex D). In addition, the verification of the method performance for each single sample shall be part of the applied quality assurance protocol. 9.2 Extraction The sample amount used fo

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