DIN EN 15308-2016 Characterization of waste - Determination of selected polychlorinated biphenyls (PCB) in solid waste by gas chromatography with electron capture or mass spectrome.pdf

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1、December 2016 English price group 19No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 13.030.10; 13.030.20; 13.080.10

2、!%hK“2596940www.din.deDIN EN 15308Characterization of waste Determination of selected polychlorinated biphenyls (PCB) in solid waste by gas chromatography with electron capture or mass spectrometric detection;English version EN 15308:2016,English translation of DIN EN 15308:2016-12Charakterisierung

3、von Abfllen Bestimmung ausgewhlter polychlorierter Biphenyle (PCB) in festem Abfall mittels Gaschromatographie mit ElektroneneinfangDetektion oder massenspektrometrischer Detektion;Englische Fassung EN 15308:2016,Englische bersetzung von DIN EN 15308:2016-12Caractrisation des dchets Dtermination de

4、polychlorobiphnyles (PCB) slectionns dans les dchets solides par chromatographie en phase gazeuse avec dtection par capture dlectrons ou spectromtrie de masse;Version anglaise EN 15308:2016,Traduction anglaise de DIN EN 15308:2016-12SupersedesDIN EN 15308:200805www.beuth.deDocument comprises 51 page

5、sDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.12.16 DIN EN 15308:2016-12 2 A comma is used as the decimal marker. National foreword This document (EN 15308:2016) has been prepared by Technical Committee CEN/TC 444 “Test methods f

6、or the characterization of solid matrices” (Secretariat: NEN, Netherlands). The responsible German body involved in its preparation was DIN-Normenausschuss Wasserwesen (DIN Standards Committee Water Practice), Working Committee NA 119-01-02-02 UA Chemische und physikalische Verfahren, Working Group

7、NA 119-01-02-02-05 AK Organische Analytik. Expert assistance and specialized laboratories will be required to perform the analyses described in this standard. The DIN Standards corresponding to the International Standards referred to in this document are as follows, whereby EN ISO Standards are only

8、 listed below if these have not been published as DIN EN ISO Standards with the same number: ISO 11464 DIN 19747 ISO 14507 DIN 19747 ISO 22892 DIN EN ISO 22892 Amendments This standard differs from DIN EN 15308:2008-05 as follows: a) a new calculation method for the estimation of the total PCB conte

9、nt has been added in Annex D; b) the standard has been editorially revised. Previous editions DIN EN 15308: 2008-05 National Annex NA (informative) Bibliography 1 DIN 19747, Investigation of solids Pre-treatment, preparation and processing of samples for chemical, biological and physical investigati

10、ons 2 DIN EN ISO 22892, Soil quality Guidelines for the identification of target compounds by gas chromatography and mass spectrometry EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15308 October 2016 ICS 13.030.10; 13.030.20; 13.080.10 Supersedes EN 15308:2008English Version Characterization

11、of waste - Determination of selected polychlorinated biphenyls (PCB) in solid waste by gas chromatography with electron capture or mass spectrometric detection Caractrisation des dchets - Dtermination de polychlorobiphnyles (PCB) slectionns dans les dchets solides par chromatographie en phase gazeus

12、e avec dtection par capture dlectrons ou spectromtrie de masse Charakterisierung von Abfllen - Bestimmung ausgewhlter polychlorierter Biphenyle (PCB) in festem Abfall mittelsGaschromatographiemit Elektroneneinfang-Detektion oder massenspektrometrischer Detektion This European Standard was approved b

13、y CEN on 21 September 2016. 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 st

14、andards 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

15、 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, Hungar

16、y, 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 COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELE

17、C Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15308:2016 EEN 15308:2016 (E) 2 Contents Page European foreword . 4 Introduction 5 1 Scope 6 2 Normative references 6 3 Ter

18、ms and definitions . 6 4 Principle . 7 5 Reagents . 8 5.1 General 8 5.2 Reagents for extraction and drying 8 5.3 Reagents for clean-up procedures 8 5.4 Reagents for gas chromatographic analysis . 10 5.5 Standard compounds 10 5.5.1 Calibration standards . 10 5.5.2 Internal and injection standards 10

19、6 Apparatus 11 6.1 Extraction and clean-up procedures . 11 6.1.1 General . 11 6.1.2 Extraction procedures 11 6.1.3 Clean-up procedures . 12 6.2 Gas chromatograph . 12 6.3 Capillary columns 12 7 Safety precautions . 12 8 Interferences . 13 9 Sample storage 13 10 Pretreatment . 13 10.1 General . 13 10

20、.2 Drying . 13 10.3 Particle size reduction 13 11 Procedure 14 11.1 Blank . 14 11.2 Extraction 14 11.2.1 Extraction by shaking or sonification . 14 11.2.2 Soxhlet extraction 14 11.3 Clean-up . 15 11.3.1 General . 15 11.3.2 Aluminium oxide clean-up 15 11.3.3 Silica cartridge clean-up 15 11.3.4 Silica

21、 H2SO4clean-up . 15 11.3.5 Florisilclean-up 15 11.3.6 TBA clean-up 16 11.3.7 Pyrogenic copper clean-up . 16 DIN EN 15308:2016-12 EN 15308:2016 (E) 3 11.3.8 AgNO3/silica clean-up . 16 11.3.9 DMSO/n-hexane partitioning clean-up . 17 11.3.10 Benzenesulfonic acid/silica cartridge clean-up 17 11.4 Gas ch

22、romatographic analysis . 17 11.4.1 General . 17 11.4.2 Optimizing the gas chromatograph 17 11.4.3 Detectors 17 11.4.4 Check on method performance . 18 11.4.5 GC-MS determination 19 11.4.6 GC-ECD determination 21 12 Calculation 22 13 Test report 22 Annex A (informative) Performance characteristics 23

23、 A.1 General . 23 A.2 Type of samples and sample preparation . 23 A.3 Homogeneity and stability 24 A.4 Extraction 25 A.5 Clean-up . 25 A.6 Detection 25 A.7 PCB standard solution 25 Annex B (informative) Examples of GC-MS chromatograms of a calibration standard solution and a contaminated soil sample

24、 29 Annex C (informative) Examples of GC-ECD chromatograms of a calibration standard solution and a cable shredder sample 36 Annex D (normative) Calculation method for the estimation of total PCB content . 39 Annex E (informative) Summary of general requirements and recommendations 48 Bibliography .

25、 49 DIN EN 15308:2016-12 EN 15308:2016 (E) 4 European foreword This document (EN 15308:2016) has been prepared by Technical Committee CEN/TC 444 “Test methods for the characterization of solid matrices”, the secretariat of which is held by NEN. This European Standard shall be given the status of a n

26、ational standard, either by publication of an identical text or by endorsement, at the latest by April 2017, and conflicting national standards shall be withdrawn at the latest by April 2017. Attention is drawn to the possibility that some of the elements of this document may be the subject of paten

27、t rights. CEN shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 15308:2008. According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria

28、, 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, Slovakia, Slovenia, Spain, Sweden,

29、Switzerland, Turkey and the United Kingdom. DIN EN 15308:2016-12 EN 15308:2016 (E) 5 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

30、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

31、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). Taking into accoun

32、t 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 Mass Spectrometry and Electron Capture is possible. Two different extraction

33、procedures and nine clean-up procedures are described. 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. This European Standard has been validated on seven solid waste which are typically contaminated with

34、PCB (building debris, cable shredder, contaminated soil, electronic waste, sealant waste, shredder light fraction and waste wood). Validation data are given in Annex A (informative). DIN EN 15308:2016-12 EN 15308:2016 (E) 6 1 Scope This European Standard specifies a method for quantitative determina

35、tion of seven polychlorinated biphenyl congeners (PCB-28, PCB-52, PCB-101, PCB-118, PCB-138, PCB-153 and PCB-180) in solid waste using high-resolution gas chromatography with electron capture or mass spectrometric detection. The basic content of this standard is identical to that of the Horizontal P

36、CB-standard and is therefore also applicable to soil, sludge and treated bio-waste. The detection and the quantification limits in this method are dependent on sample intake, the level of interferences as well as instrumental limitations. Under the conditions specified in this standard, minimum amou

37、nts of individual PCB congeners equal or above 0,01 mg/kg dry matter can typically be determined with no interferences present. NOTE For the analysis of PCB in insulating liquids, petroleum products, used oils and aqueous samples is referred to EN 61619, EN 127661 and EN ISO 6468 respectively. The m

38、ethod may be applied to the analysis of other PCB congeners not specified in the scope, but its suitability should be proven by proper in-house validation experiments. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensab

39、le 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 12766-1, Petroleum products and used oils - Determination of PCBs and related products - Part 1: Separation and d

40、etermination of selected PCB congeners by gas chromatography (GC) using an electron capture detector (ECD) EN 12766-2, Petroleum products and used oils - Determination of PCBs and related products - Part 2: Calculation of polychlorinated biphenyl (PCB) content EN 14346, Characterization of waste - C

41、alculation of dry matter by determination of dry residue or water content 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 polychlorinated biphenyl PCB biphenyl substituted by one to ten chlorine atoms 3.2 congener member of the same kind, cla

42、ss or group of chemicals Note 1 to entry: Any one of the two hundred and nine individual PCB. Note 2 to entry: The IUPAC congener numbers are for easy identification; they do not represent the order of chromatographic elution. DIN EN 15308:2016-12 EN 15308:2016 (E) 7 3.3 calibration standard solutio

43、n prepared from a secondary standard and/or stock solutions of native polychlorinated biphenyl congeners (PCB) and used to calibrate the response of the instrument with respect to analyte concentration 3.4 internal standard 13C12-labelled PCB or other PCB that are unlikely to be present in waste sam

44、ples added to the sample before extraction and used for quantification of PCB content 3.5 injection standard 13C12-labelled PCB or other PCB that is unlikely to be present in waste samples added to the sample extract before injection into the gas chromatograph, to monitor variability of instrument r

45、esponse and the recovery of the internal standards 3.6 critical pair pair of congeners that needs to be separated to a predefined degree (e. g. R = 0,5) to ensure chromatographic separation meets minimum quality criteria 3.7 resolution Rsdifference in retention times between the maxima of the two pe

46、aks i and j, which constitute the critical pair, divided by the arithmetic mean of the peak widths of i and j at base, calculated as: ( )( )=+Rj Risbi bj2 ttRww(1) where tRjand tRiare the retention times of the two peaks i and j (sec), and wbiand wbjare the peak widths of i and j (sec) at base 4 Pri

47、nciple A proper test portion is extracted with a mixture of organic solvents by an appropriate extraction technique (e.g. shaking, soxhlet, sonication), partitioned against water and the organic layer separated. The obtained extracts are concentrated and, if appropriate, cleaned-up. Sample clean-up

48、procedures may include sulphuric acid treatment, Dimethylsulfoxide/n-Hexan partitioning, column chromatography on alumina and silica. Tetrabutylammonium sulfite (TBA) or copper may be used to remove sulfur if required. The extract is analysed by gas chromatography with either mass spectrometric (GC-

49、MS) or electron capture detection (GC-ECD). In case of GC-MS analysis quantification is performed by the isotope dilution technique. In case of GC-ECD, extracts are analysed using two columns of different polarity. Quantification is conducted by the internal standard method. In case of plastic shredder a pure non-polar solvent should be used for extraction to prevent dissolving of the polymer matrix as far as possible. DIN EN 15308:2016-12 EN 15308:2016 (E) 8