EN 15308:2008

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Charakterisierung von Abfällen - Bestimmung ausgewählter polychlorierter Biphenyle (PCB) in festem Abfall unter Anwendung der Kapillar-Gaschromatographie mit Elektroneneinfang-Detektion oder massenspektrometrischer DetektionCaractérisation des déchets - Détermination de polychlorobiphényles (PCB) sélectionnés dans les déchets solides par chromatographie en phase gazeuse capillaire avec détection par capture d'électrons ou spectrométrie de masseCharacterization of waste - Determination of selected polychlorinated biphenyls (PCB) in solid waste by using capillary gas chromatography with electron capture or mass spectrometric detection71.040.50Fizikalnokemijske analitske metodePhysicochemical methods of analysis13.030.10Trdni odpadkiSolid wastesICS:Ta slovenski standard je istoveten z:EN 15308:2008SIST EN 15308:2008en,fr,de01-julij-2008SIST EN 15308:2008SLOVENSKI
STANDARD
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 15308February 2008ICS 13.030.10; 13.030.20; 13.080.10 English VersionCharacterization of waste - Determination of selectedpolychlorinated biphenyls (PCB) in solid waste by using capillarygas chromatography with electron capture or massspectrometric detectionCaractérisation des déchets - Détermination depolychlorobiphényles (PCB) sélectionnés dans les déchetssolides par chromatographie en phase gazeuse capillaireavec détection par capture d'électrons ou spectrométrie demasseCharakterisierung von Abfällen - Bestimmung ausgewählterpolychlorierter Biphenyle (PCB) in festem Abfall unterAnwendung der Kapillar-Gaschromatographie mitElektroneneinfang-Detektion odermassenspektrometrischer DetektionThis European Standard was approved by CEN on 28 December 2007.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN 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 translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, 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 and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2008 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15308:2008: ESIST EN 15308:2008

Examples of GC/MS chromatograms of a calibration standard solution and a contaminated soil sample.23 Annex B (informative)
Examples of GC-ECD chromatograms of a calibration standard solution and a cable shredder sample.30 Annex C (informative)
Additional validation data.33 C.1 General.33 C.2 Type of samples and sample preparation.33 C.3 Homogeneity and stability.34 C.4 Extraction.35 C.5 Clean-up.35 C.6 Detection.35 C.7 PCB standard solution.35 Annex D (informative)
Summary of general requirements and recommendations.37 Bibliography.38
()()bjbiRiRjs2wwttR+−= (1) where tRj and tRi are the retention times of the two peaks i and j (sec), and wbi and wbj are the peak widths of i and j (sec) at base 4 Principle 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 cleanup 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 analyzed by gas chromatography with either mass spectrometric (GC-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 analyzed using two columns of different polarity. Quantification is conducted by the internal standard method. NOTE 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. 5 Reagents 5.1 General All reagents shall be of recognized analytical grade. Running a blank determination as described in 11.1 shall check the purity of the reagents used. 5.2 Reagents for extraction and drying 5.2.1 Acetone. 5.2.2 Hexane like solvents with a boiling range of 36 °C to 98 °C, e. g. petroleum ether, n-hexane, n-heptane. SIST EN 15308:2008

(CAS number: 7012-37-5);  PCB-52: 2,2',5,5'-tetrachlorobiphenyl
(CAS number: 35693-99-3);  PCB-101: 2,2',4,5,5'-pentachlorobiphenyl
(CAS number: 37680-37-2);  PCB-118: 2,3',4,4',5-pentachlorobiphenyl
(CAS number: 31508-00-6);  PCB-138: 2,2',3,4,4',5'-hexachlorobiphenyl
(CAS number: 35056-28-2);
1) Florisil is a trade name for a prepared diatomaceous substance, mainly consisting of anhydrous magnesium silicate. This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of this product . Equivalent products may be used if it can be shown to lead to comparable results. SIST EN 15308:2008

(CAS number: 35065-27-1);  PCB-180: 2,2',3,4,4',5,5'-heptachlorobiphenyl (CAS number: 35065-29-3). 5.5.2 Internal and injection standards 5.5.2.1 MS detection The labelled PCB congeners to be considered as internal standards are listed below.  13C-2,4,4’-trichlorobiphenyl (PCB-28);  13C-2,2‘,5,5‘-tetrachlorobiphenyl (PCB-52);  13C-2,2‘,4,5,5‘-pentachlorobiphenyl (PCB-101);  13C-2,3‘,4,4‘,5-pentachlorobiphenyl (PCB-118);  13C-2,2‘,3,4,4‘,5‘-hexachlorobiphenyl (PCB-138);  13C-2,2‘,4,4‘,5,5‘-hexachlorobiphenyl (PCB-153);  13C-2,2‘,3,4,4‘,5,5‘-heptachlorobiphenyl (PCB-180). 13C-2,2',3,3',5,5',6-heptachlorobiphenyl (PCB-178), other 13C-labelled PCB or PCB that are unlikely to be present in waste samples may be used as internal and injection standards as well.
NOTE The application of isotopic dilution mass spectrometry is recommended but adding 13C-labelled internal standards to the test portion before extraction is associated with high costs. Hence, if only an aliquot of the extract is subjected to the clean-up adding 13C-labelled internal standards to this aliquot might be a good option to ensure high quality of the analysis and to reduce costs. 5.5.2.2 ECD detection Also for ECD-detection internal and injection standards shall be added. Use at least one of the following standards unlikely to be present in waste samples and not interfering with the analytes as internal standard  PCB-29 – 2,4,5-trichlorobiphenyl
(CAS number: 15862-07-4);  PCB-30 – 2,4,6-trichlorobiphenyl
(CAS number: 35693-92-6);  PCB-143 - 2,2',3,4,5,6'-hexachlorobiphenyl
(CAS number: 68194-15-0);  PCB-155 - 2,2',4,4',6,6'-hexachlorobiphenyl
(CAS number: 33979-03-2);  PCB-198 - 2,2',3,3',4,5,5’,6,-octachlorobiphenyl
(CAS number: 68194-17-2);  PCB-207 - 2,2',3,3',4,4',5,6,6'-nonachlorobiphenyl
(CAS number: 52663-79-3);  PCB-209 - 2,2',3,3',4,4',5,5’,6,6'-decachlorobiphenyl (CAS number: 2051-24-3). NOTE For quantification (internal standard) PCB198 and PCB209 are recommended because of little interferences found in practice. Use of PCB 30 and PCB 209 for relative retention is recommended see EN 12766-1. 5.5.2.3 PCB congeners for resolution check  PCB-28 – 2,4,4'-trichlorobiphenyl (CAS number: 7012-37-5); SIST EN 15308:2008

Grinding of samples which have a plastic or paste-like consistency requires embrittlement with liquid nitrogen and particle size reduction to less than 0,5 mm, e. g. by using an ultra-centrifugal mill. NOTE In case of plastic materials (e. g. cable shredder) the material to be granulated is poured in portions into liquid nitrogen and ground in a centrifugal mill (10 000 rounds/min to 15 000 rounds/min) cooled with liquid nitrogen. It should be noted that the mill is constantly kept cool by addition of liquid nitrogen in short intervals. The plastic material should be filled into the mill constantly in small portions without causing any significant slowing down of the grinder. 11 Procedure 11.1 Blank Perform a blank determination following the paragraphs of the procedure applied to samples (selected extraction and clean-up). Use the same amounts of reagents that are used for pre-treatment, extraction, clean up and analysis of samples. Analyse the blank immediately prior to analysis of the samples to demonstrate freedom from contamination. 11.2 Extraction 11.2.1 Extraction by shaking or sonification Weigh a test portion of 10 g to 25 g to the nearest 0,1 g in a stoppered flask. Add a definite volume of the internal standard solution. Isotopically labelled internal standards may be added after extraction to an aliquot of the extract where appropriate. Typically the concentration of the individual internal standards in the final extract will be 0,1 µg/ml. Add 50 ml of acetone to the test sample. Extract by shaking thoroughly for 30 min on a shaking device or by sonification. Then add 50 ml of hexane-like solvent (5.2.2) and extract again thoroughly SIST EN 15308:2008

NOTE Commercially available disposable aluminium oxide cartridges may be used as an alternative if found equally suitable. SIST EN 15308:2008
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