SIST EN 15308:2017
(Main)Characterization of waste - Determination of selected polychlorinated biphenyls (PCB) in solid waste by gas chromatography with electron capture or mass spectrometric detection
Characterization of waste - Determination of selected polychlorinated biphenyls (PCB) in solid waste by gas chromatography with electron capture or mass spectrometric detection
This draft European Standard specifies a method for quantitative determination 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 PCB-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 amounts 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 12766-1 and EN ISO 6468 respectively.
The method 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.
Charakterisierung von Abfällen - Bestimmung ausgewählter polychlorierter Biphenyle (PCB) in festem Abfall unter Anwendung der Kapillar-Gaschromatographie mit Elektroneneinfang-Detektion oder massenspektrometrischer Detektion
Diese Europäische Norm legt ein Verfahren zur quantitativen Bestimmung von sieben polychlorierten Biphenyl-Kongeneren (PCB 28, PCB 52, PCB 101, PCB 118, PCB 138, PCB 153 und PCB 180) in festem Abfall unter Anwendung der hochauflösenden Gaschromatographie mit Elektroneneinfang- oder massenspektro¬metri¬scher Detektion fest. Der Inhalt dieser Norm entspricht grundsätzlich dem der horizontalen PCB Norm und ist daher auch auf Boden, Schlamm und behandelten biogenen Abfall anwendbar. Die Detektion und die Quantifizierungsgrenzen in diesem Verfahren sind von der Probenaufnahme, dem Interferenzniveau sowie den instrumentellen Beschränkungen abhängig. Unter den in dieser Norm festgelegten Bedingungen können typischerweise Mindestmengen einzelner PCB-Kongenere von 0,01 mg/kg Trockenmasse oder darüber bestimmt werden, wenn keine Interferenzen vorliegen.
ANMERKUNG Für die Analyse von PCB in Isolierflüssigkeiten, Mineralölerzeugnissen, Gebrauchtölen und wässrigen Proben wird jeweils auf EN 61619, EN 12766 1 und EN ISO 6468 verwiesen.
Das Verfahren darf auf die Analyse weiterer, nicht im Anwendungsbereich festgelegter, PCB-Kongenere angewendet werden, seine Anwendbarkeit sollte jedoch mit geeigneten laborinternen Validierungs-untersuchungen nachgewiesen werden.
Caractérisation des déchets - Détermination de polychlorobiphényles (PCB) sélectionnés dans les déchets solides par chromatographie en phase gazeuse avec détection par capture d'électrons ou spectrométrie de masse
La présente Norme européenne décrit une méthode de détermination quantitative de sept congénères de polychlorobiphényles (PCB-28, PCB-52, PCB-101, PCB-118, PCB-138, PCB-153 et PCB-180) dans les déchets solides, par chromatographie en phase gazeuse haute résolution avec détection par capture d’électrons ou spectrométrie de masse. Le contenu de base de la présente norme est identique à celui de la norme horizontale sur les PCB et s'applique, par conséquent, également aux sols, aux boues et aux déchets biologiques traités. Les limites de détection et de quantification de la présente méthode dépendent de la prise d’essai, du niveau des interférences ainsi que des limitations liées aux instruments. Dans les conditions définies par la présente norme, il est possible de déterminer des quantités minimales de congénères individuels de PCB supérieures ou égales à 0,01 mg/kg de matière sèche sans interférences.
NOTE Pour l’analyse des PCB dans les liquides isolants, les produits pétroliers, les huiles usagées et les échantillons aqueux, se référer respectivement aux normes EN 61619, EN 12766-1 et EN ISO 6468.
La méthode peut être appliquée à l'analyse de PCB congénères autres que ceux décrits dans le domaine d’application, mais il convient d’en définir l’applicabilité par des tests de validation internes adaptés.
Karakterizacija odpadkov - Določevanje izbranih polikloriranih bifenilov (PCB) v trdnih odpadkih s (kapilarno) plinsko kromatografijo z detektorjem z zajemom elektronov (ECD) ali z masno spektrometrično detekcijo
Ta osnutek evropskega standarda določa metodo za kvantitativno določevanje sedmih analogov polikloriranih bifenilov (PCB-28, PCB-52, PCB-101, PCB-118, PCB-138, PCB-153 in PCB-180) v trdnih odpadkih z visokoločljivostno plinsko kromatografijo z detektorjem z zajemom elektronov ali z masno spektrometrično detekcijo. Osnovna vsebina tega standarda je enaka vsebini horizontalnega standarda za poliklorirane bifenile, zato se standard uporablja tudi za prst, blato in obdelane biološke odpadke. Način odkrivanja in količinske omejitve te metode so odvisni od količine vzorca, ravni motenj ter omejitev instrumentov. Pod pogoji, določenimi v tem standardu, se minimalne količine posameznih analogov polikloriranih bifenilov, ki so enake ali večje od 0,01 mg/kg suhe snovi, navadno lahko določi brez prisotnih motenj.
OPOMBA: Za analizo polikloriranih bifenilov v izolacijskih tekočinah, naftnih proizvodih, rabljenih oljih in vodnih vzorcih se standard sklicuje na standarde EN 61619, EN 12766-1 in EN ISO 6468.
Metoda se lahko uporablja za analize drugih analogov polikloriranih bifenilov, ki ne spadajo na področje uporabe tega standarda, vendar je treba njeno ustreznost dokazati s primernimi internimi poskusi za validacijo.
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Standards Content (Sample)
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 avec détection par capture d'électrons ou spectrométrie de masseCharacterization of waste - Determination of selected polychlorinated biphenyls (PCB) in solid waste by 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 15308:2016SIST EN 15308:2017en01-maj-2017SIST EN 15308:2017SLOVENSKI
STANDARDSIST EN 15308:20081DGRPHãþD
SIST EN 15308:2017
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15308
October
t r s x ICS
s uä r u rä s râ
s uä r u rä t râ
s uä r z rä s r Supersedes EN
s w u r zã t r r zEnglish Version
Characterization of waste æ Determination of selected chromatography with electron capture or mass spectrometric detection Caractérisation des déchets æ Détermination de déchets solides par chromatographie en phase gazeuse avec détection par capture d 5électrons ou spectrométrie de masse
Charakterisierung von Abfällen æ Bestimmung festem Abfall unter Anwendung der KapillaræGaschromatographie mit ElektroneneinfangæDetektion oder massenspektrometrischer Detektion This European Standard was approved by CEN on
t s September
t r s xä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
9
t r s x CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s w u r zã t r s x ESIST EN 15308:2017
EN 15308:2016 (E) 2 Contents Page European foreword . 4 Introduction . 5 1 Scope . 6 2 Normative references . 6 3 Terms 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 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 10.2 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 H2SO4 clean-up . 15 11.3.5 Florisil® clean-up . 15 11.3.6 TBA clean-up . 16 11.3.7 Pyrogenic copper clean-up . 16 SIST EN 15308:2017
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 chromatographic 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 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 . 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 . 49
SIST EN 15308:2017
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 national 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 patent 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, 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, Switzerland, Turkey and the United Kingdom. SIST EN 15308:2017
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 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). Taking 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 Mass Spectrometry and Electron Capture is possible. Two different extraction 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 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). SIST EN 15308:2017
EN 15308:2016 (E) 6 1 Scope This European Standard specifies a method for quantitative determination 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 PCB-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 amounts 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 12766–1 and EN ISO 6468 respectively. The method 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 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 12766-1, Petroleum products and used oils - Determination of PCBs and related products - Part 1: Separation and determination 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 - Calculation 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, class 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. SIST EN 15308:2017
EN 15308:2016 (E) 7 3.3 calibration standard solution 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 samples 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 response 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 Rs difference in retention times between the maxima of the two peaks 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: ()()−=+RjRisbibj2ttRww (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 clean-up 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-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. SIST EN 15308:2017
EN 15308:2016 (E) 8 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 (2-propanone), (CH3)2CO. 5.2.2 Hexane like solvents with a boiling range of 36 °C to 98 °C, e.g. petroleum ether, n-hexane, n-heptane. 5.2.3 Anhydrous sodium sulfate, heated for at least 6 h to 550 °C ± 20 °C, cooled to about 200 °C in the furnace and then to ambient temperature in a desiccator containing magnesium perchlorate or another suitable drying reagent. The anhydrous sodium sulfate shall be kept carefully sealed. 5.3 Reagents for clean-up procedures 5.3.1 Aluminium oxide clean-up: 5.3.1.1 One of two types of alumina, acidic or basic, which can be used in the clean-up of sample extracts: — acidic alumina, activate by heating to 130 °C for a minimum of 12 h; — basic alumina, activate by heating to 600 °C for a minimum of 24 h. Preparation of deactivated aluminium oxide, the aluminium oxide is deactivated with 10 % water. To 90 g of aluminium oxide (5.3.1.1) add 10 g of water. Shake until all lumps have disappeared. Allow the aluminium oxide to condition before use for some 16 h, sealed from the air. ICN Alumina Super I or an equivalent may be used without activation. 5.3.2 TBA sulfite reagent for sulfur removal: 5.3.2.1 Tetrabutylammonium reagent (TBA sulfite reagent): saturate a solution of tetrabutylammonium hydrogen sulfate in a mixture of equal volumina of water and 2-propanol, c((C4H9)4NHSO4) = 0,1 mol/l, with sodium sulfite. 25 g of sodium sulfite should be sufficient for 100 ml of solution. 5.3.3 Pyrogenic copper for sulfur removal: WARNING — Pyrogenic copper is spontaneously inflammable. Suitable precautions should be taken. 5.3.3.1 Copper-(II)sulfate pentahydrate, CuSO4 · 5 H2O. 5.3.3.2 Hydrochloric acid, c(HCl) = 2 mol/l. 5.3.3.3 Zinc granules, Zn, particle size 0,3 mm to 1,4 mm. SIST EN 15308:2017
EN 15308:2016 (E) 9 5.3.3.4 Anionic detergent aqueous solution (e.g. 35 % m/V n-dodecane-1-sulfonic acid sodium salt (CH3(CH2)11SO3Na)). 5.3.3.5 Deoxygenated water. 5.3.4 Silica – silver nitrate clean up: 5.3.4.1 Silica gel, particle size 60 µm to 200 µm. 5.3.4.2 Silver nitrate, AgNO3. 5.3.4.3 Preparation of silica gel impregnated with silver nitrate. Dissolve 10 g of AgNO3 in 40 ml of water and pour this mixture in portions to 90 g silica. Shake the mixture until it is homogenous and leave standing it for 30 min. Put the mixture into a drying oven at 70 °C. Within 5 h increase the temperature from 70 °C up to 120 °C. Activate the mixture for 15 h at 125 °C. Store the mixture in brown glass bottles. 5.3.5 Commercially available benzenesulfonic acid/silica gel cartridges, 3 ml. 5.3.6 Dimethylsulfoxide/n-hexane partitioning: 5.3.6.1 Dimethylsulfoxide (DMSO). 5.3.6.2 n-Hexane, C6H14. 5.3.7 Sulphuric acid clean-up: 5.3.7.1 Sulphuric acid, H2SO4, 95 % to 97 %. 5.3.8 Silica gel/sulphuric acid clean-up: 5.3.8.1 Silica/H2SO4 44 %: Pour 28 g of activated silica and 22 g of sulfuric acid in a flask, stopper air tight and shake thoroughly until disappearance of all agglomerates. 5.3.8.2 Silica/NaOH 33 % 1 mol/l: pour 33,5 g of activated silica and 16,5 g 1 mol/l NaOH in a flask, stopper air tight and shake thoroughly until disappearance of all agglomerates. 5.3.9 Commercially available silica cartridges, 3 ml or 6 ml. 5.3.10 Florisil clean up: 5.3.10.1 Florisil®1) 100 mesh to 200 mesh, activated by heating to 600 °C for a minimum of 2 h. 5.3.10.2 Iso-octane, C8H18. 5.3.10.3 Iso-octane/Toluene 95/5.
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 15308:2017
EN 15308:2016 (E) 10 5.4 Reagents for gas chromatographic analysis 5.4.1 Operating gases for gas chromatography, of high purity and in accordance with manufacturer's specifications. 5.5 Standard compounds 5.5.1 Calibration standards Use the following PCB for the calibration: — PCB-28: 2,4,4'-trichlorobiphenyl (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); — PCB-153: 2,2',4,4',5,5'-hexachlorobiphenyl (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. 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 SIST EN 15308:2017
EN 15308:2016 (E) 11 — 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). For quantification (internal standard) PCB-198 and PCB-209 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); — PCB-31 – 2,4',5-trichlorobiphenyl (CAS number: 16862-07-4). 6 Apparatus 6.1 Extraction and clean-up procedures 6.1.1 General 6.1.1.1 Customary laboratory glassware. All glassware and material that comes into contact with the sample or extract shall be free of PCB and interfering compounds. 6.1.2 Extraction procedures 6.1.2.1 Glass sample bottles of proper size according to the amount of sample taken with glass stopper or screw top and polytetrafluorethene seal (PTFE). 6.1.2.2 Shaking device. With horizontal movement (200 min «1 to 300 min «1). 6.1.2.3 Water bath, adjustable up to 100 °C. 6.1.2.4 Separatory funnels of appropriate volume. 6.1.2.5 Conical flasks of appropriate volume. 6.1.2.6 Soxhlet extraction apparatus, consisting of round bottom flask e.g.100 ml, Soxhlet extractors and soxhlet thimbles e.g. 27 mm × 100 mm, vertical condensers e.g. 300 mm, with water-bath or heating mantle as heating device. 6.1.2.7 Evaporator. SIST EN 15308:2017
EN 15308:2016 (E) 12 Kuderna Danish or other evaporators, e.g. a rotary evaporator. 6.1.2.8 Analytical balance. 6.1.3 Clean-up procedures 6.1.3.1 Quartz wool or silanized glass wool. WARNING — Working with quartz wool imposes a risk to health through the release of fine quartz particles. Inhalation of these should be prevented by using a fume cupboard and wearing a dust mask. 6.1.3.2 Boiling chips, glass or porcelain beads. 6.1.3.3 Calibrated test tubes with a capacity of 10 ml to 15 ml and ground glass stopper. 6.1.3.4 Glass chromatography columns of e.g. 600 mm length and 5 mm internal diameter. 6.1.3.5 Empty SPE-cartridge of e.g. 6 ml volume. 6.2 Gas chromatograph Equipped with a capillary column, mass spectrometric detector (MS) or electron capture detector (ECD) based
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