DIN EN 12766-1-2000 Petroleum products and used oils - Determination of PCBs and related products - Part 1 Separation and determination of selected PCB congeners by gas chromatogra.pdf

1、ICS 75.080; 75.100Minerallerzeugnisse und Gebrauchtle Bestimmung von PCBs und verwandten Produkten Teil 1:Trennung und Bestimmung von ausgewhlten PCB-Congeneren mittels Gaschromatographie (GC) unterVerwendung eines Elektroneneinfang-Detektors (ECD)European Standard EN 12766-1 : 2000 has the status o

2、f a DIN Standard.A comma is used as the decimal marker.National forewordThis standard has been prepared by CEN/TC 19 Petroleum products, lubricants and related products(Secretariat: The Netherlands).The responsible German body involved in its preparation was the Normenausschuss Materialprfung(Materi

3、als Testing Standards Committee), Technical Committee Minerallerzeugnisse, Schmierstoffe undverwandte Produkte.DIN EN ISO 3170, DIN 51750-1, DIN 51750-2 and DIN EN ISO 3171 are the standards corresponding toEuropean Standards ISO 3170 and ISO 3171, respectively, referred to in clause 2 of the EN.Nat

4、ional Annex NAStandards referred to(and not included in Normative references)DIN 51750-1 Sampling of petroleum products GeneralDIN 51750-2 Sampling of liquid petroleum productsRef. No. DIN EN 12766-1 : 2000-11English price group 14 Sales No. 111404.01DEUTSCHE NORM November 2000EN 12766-1Continued ov

5、erleaf.EN comprises 31 pages. No part of this standard may be reproduced without the 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).Petroleum products and used oilsDetermin

6、ation of PCBs and related productsPart 1: Separation and determination of selected PCB congeners by gaschromatography (GC) using an electron capture detector (ECD)English version of DIN EN 12766-1English versionICS 75.080; 75.100Descriptors:Petroleum products and used oilsDetermination of PCBs and r

7、elated productsPart 1: Separation and determination of selected PCB congeners by gaschromatography (GC) using an electron capture detector (ECD) 2000. CEN All rights of exploitation in any form and by any meansreserved worldwide for CEN national members.Ref. No. EN 12766-1 : 2000 EMinerallerzeugniss

8、e undGebrauchtle Bestimmung vonPCBs und verwandten Produkten Teil 1: Trennung und Bestimmungvon ausgewhlten PCB-Congenerenmittels Gaschromatographie (GC)unter Verwendung eines Elektronen-einfang-Detektors (ECD)This European Standard was approved by CEN on 2000-01-20.CEN members are bound to comply w

9、ith the CEN/CENELEC Internal Regulationswhich stipulate the conditions for giving this European Standard the status of anational standard without any alteration.Up-to-date lists and bibliographical references concerning such national stand-ards may be obtained on application to the Central Secretari

10、at or to anyCEN member.The European Standards exist in three official versions (English, French, German).A version in any other language made by translation under the responsibility of aCEN member into its own language and notified to the Central Secretariat has thesame status as the official versio

11、ns.CEN members are the national standards bodies of Austria, Belgium, the CzechRepublic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy,Luxembourg, the Netherlands, Norway, Portugal, Spain, Sweden, Switzerland,and the United Kingdom.EN 12766-1March 2000Central Secretariat: rue de

12、 Stassart 36, B-1050 BrusselsEuropean Committee for StandardizationComit Europen de NormalisationEuropisches Komitee fr Normung|Produits ptroliers et huiles usages Dtermination des PCBs et produitsconnexes Partie 1: Sparation etdosage dune slection de congnresde PCB par chromatographie enphase gazeu

13、se (CG) avec utilisationdun dtecteur capture dlectrons(ECD)Page 2EN 12766-1 : 2000Page 3EN 12766-1 : 2000Page 4EN 12766-1 : 2000Page 5EN 12766-1 : 2000Page 6EN 12766-1 : 2000Page 7EN 12766-1 : 2000Page 8EN 12766-1 : 200025 mg samplein 250 ml solvent solution2,5 ml solvent0,5 g SiO2/H2SO4+0,5 g benze

14、nesulfonic acid phaseRemoval of hetero compounds,polyaromatichydrocarbons and bases2 0,5 ml solvent0,5 g SiO2-phaseGCmake up 5,0 ml with solventRemoval of polar compoundsand aromaticsa) for the split/splitless injector:splitless mode:split valve closed between:split mode:split ratio:T = 240 C to 280

15、 C0,5 min to 1,5 minT = 250 C to 280 C5:1T: 50 C to 110 C depending on the solvent used.b) for the on-column injector:Page 9EN 12766-1 : 2000Initial isothermal period 1 min or 0,5 minInitial temperature 50 C or 70 CTemperature programm 50 C to 168 C at or 70 C to 130 C at50 C/min 40 C/min168 C to 31

16、0 C at 130 C to 290 C at4,0 C/min 2,5 C/minIsothermal period 10 min or 5 minCool down to 50 C or 70 CThese settings may be varied to obtain the required chromatogram.Page 10EN 12766-1 : 20001300011000900070001 0000,1 1 10 100Sensitivity Sjt 5 % EnvelopeLower limit Linear range Upper limitAmount inje

17、cted mj(pg)Page 11EN 12766-1 : 2000Page 12EN 12766-1 : 2000Identify the peaks by their experimental relative retention times (ERRT) as calculated for each peak using the equation given inclause 10, and the PCB distribution pattern of the example in Annex A.1.Page 13EN 12766-1 : 2000a) the type and i

18、dentification of the sample under test;b) a reference to this European Standard;c) the sampling procedure used (see clause 7);d) the clean-up procedure used (see clause 8);e) the results of the test (see clause 14);f) any deviation from the procedure described and any unusual features noted during t

19、he determinations;g) the date of the test.Page 14EN 12766-1 : 2000(Aroclor 1242/1254/1260 (2:1:1) plus congener 30 and congener 209)Page 15EN 12766-1 : 2000Retention time (min)IntensityPage 16EN 12766-1 : 2000Calibration Congener numberPeak nr. ERRT (example) All probables(IUPAC nr.)All possibles(IU

20、PAC nr.)Page 17EN 12766-1 : 2000Calibration Congener numberPeak nr. ERRT (example) All probables(IUPAC nr.)All possibles(IUPAC nr.)Page 18EN 12766-1 : 2000Calibration Congener numberPeak nr. ERRT (example) All probables(IUPAC nr.)All possibles(IUPAC nr.)Page 19EN 12766-1 : 2000Congener number(IUPAC)

21、Relative retention timeto DCBCongener number(IUPAC)Relative retention timeto DCBPage 20EN 12766-1 : 2000Congener number(IUPAC)Relative retention timeto DCBCongener number(IUPAC)Relative retention timeto DCBPage 21EN 12766-1 : 2000Page 22EN 12766-1 : 2000 RIVM (1989). Werkdocument rondzending analyse

22、s van PCBs in afvalolie volgens de IvM methode, Rijksinstituutvoor Volksgezondheid en Milieuhygiene, Bilthoven. Wegener, J.W.M., P. de Voogt en H. Govers (1987).Voorschrift voor de bepaling van polychloorbifenylen in minerale olien, IvM 87-17, Instituut voor Milieuvraagstukken,Vrije Universiteit van

23、 Amsterdam.Page 23EN 12766-1 : 2000Figure B.1Chromatographic Column 1 for the clean-up andfractionation of the extract (B.1.3.7)Figure B.2Chromatographic Column 1 for the clean-up andfractionation of the extract (B.1.3.8)Page 24EN 12766-1 : 2000Page 25EN 12766-1 : 2000Page 26EN 12766-1 : 2000Nr. Str

24、ucture Nr. Structure Nr. Structure Nr. StructurePage 27EN 12766-1 : 2000Nr. Structure Nr. Structure Nr. Structure Nr. StructurePage 28EN 12766-1 : 2000Producer Country TradenameMonsanto USA and Britain AroclorBayer Germany ClophenProdelec France Phenclor and PyraleneKanegafuchi Japan SantothermMitsubishi Japan SantothermCaffaro Italy Fenclor/ApirolioColumn ManufacturerRtx5 RestexDB5 J & WSPB-5 SupelcoOV-5 Ohio ValleyHP-5, Ultra-Z Hewlett PackardRSL-200 AlltechCP SIL 8CB ChrompackBP5 SGE007-2 QuadrexTRB-5 Teknokrona