BS EN 12766-3-2004 Petroleum products and used oils Determination of PCBs and related products Determination and quantification of polychlorinated terphenyls (PCT) and polychlorinat.pdf

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1、BRITISH STANDARDBS EN 12766-3:2004BS 2000-462.3:2004Incorporating corrigendum no. 1Petroleum products and used oils Determination of PCBs and related products Part 3: Determination and quantification of polychlorinated terphenyls (PCT) and polychlorinated benzyl toluenes (PCBT) content by gas chroma

2、tography (GC) using an electron capture detector (ECD)The European Standard EN 12766-3:2004 has the status of a British StandardICS 75.080; 75.100g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3

3、g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58Licensed Copy: Wang Bin, na, Wed Sep 26 07:59:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSIBS EN 12766-3:2004This British Standard was published under the authority of the Standards Policy and Strategy Committee on 7 December 2004 BSI 7 December 2007ISBN

4、 978 0 580 59190 7National forewordThis British Standard is the official UK version of EN 12766-3:2004, incorporating corrigendum February 2007.The start and finish of text introduced or altered by corrigendum is indicated in the text by tags . Text altered by CEN corrigendum February 2007 is indica

5、ted in the text by .The UK participation in its preparation was entrusted to Technical Committee PTI/13, Petroleum testing and terminology. A list of organizations represented on this committee can be obtained on request to its secretary.Energy Institute, under the brand of IP, publishes and sells a

6、ll Parts of BS 2000, and is all BS EN petroleum test methods that would be Part of BS 2000, both in its annual publication “Standard methods for analysis and testing of petroleum and related products and British Standard 2000 Parts” and individually.Further information is available from: Energy Inst

7、itute, 61 New Cavandish Street, London W1G 7AR. Tel: 020 7467 7100. Fax: 020 7255 1472.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Compliance with a British Standard does cannot confer immunity from legal

8、obligations.Amendments issued since publicationAmd. No. Date Comments17068Corrigendum No. 129 June 2007 See updated national forewordLicensed Copy: Wang Bin, na, Wed Sep 26 07:59:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 12766-3November 2004ICS 75

9、.080; 75.100English versionPetroleum products and used oils - Determination of PCBs andrelated products - Part 3: Determination and quantification ofpolychlorinated terphenyls (PCT) and polychlorinated benzyltoluenes (PCBT) content by gas chromatography (GC) using anelectron capture detector (ECD)Pr

10、oduits ptroliers et huiles usages - Dtermination desPCB et produits connexes - Partie 3: Dtermination etquantification des polychloroterphnyles (PCT) et despolychlorobenzyltolunes (PCBT) par chromatographie enphase gazeuse (CPG) avec utilisation dun dtecteur capture dlectrons (DCE)Minerallerzeugniss

11、e und Gebrauchtle - Bestimmung vonPCBs und verwandten Produkten - Teil 3: Bestimmung undBerechnung der Gehalte von polychlorierten Terphenylen(PCT) und polychlorierten Benzyltoluolen (PCBT) mittelsGaschromatographie unter Verwendung einesElektroneneinfang-detektors (ECD)This European Standard was ap

12、proved by CEN on 14 October 2004.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 nationa

13、lstandards may be obtained on application to the Central Secretariat 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

14、 to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, N

15、orway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2004 CEN All rights of exploitation in any form and by an

16、y means reservedworldwide for CEN national Members.Ref. No. EN 12766-3:2004: EIncorporating corrigendum February 2007Licensed Copy: Wang Bin, na, Wed Sep 26 07:59:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 12766-3:2004 (E) 2 Contents page Foreword3 1 Scope 4 2 Normative references 5 3 Terms and

17、 definitions .5 4 Principle6 5 Reagents and materials 6 5.1 Reagents and materials for the sample preparation (clean-up) .6 5.2 Reagents and materials for the GC analysis 7 5.3 Standard and reference solutions7 5.4 Base oil .7 5.5 Check sample.8 6 Apparatus .8 6.1 General provisions 8 6.2 Gas chroma

18、tograph.8 6.3 Columns8 7 Sampling and sample preparation.8 8 Clean-up procedure.8 9 Operating conditions for the GC apparatus9 9.1 Setting up the GC apparatus 9 9.2 Injectors 9 9.3 Oven temperature programme .9 9.4 Carrier gas flow rate 9 9.5 Electron capture detector settings 10 10 Check on instrum

19、ental performance and resolution .10 11 Calibration 10 11.1 General10 11.2 Determination of experimental relative retention times (ERRTi) 10 11.3 Determination of experimental relative response factors (ERRFi,j ) for PCT .11 11.4 Determination of experimental relative response factors (ERRFi) for PC

20、BT 12 12 Measurement12 13 Calculation of results 13 13.1 Calculation of PCTs.13 13.2 Calculation of PCBTs 13 14 Calculation of the total content of PCB and PCB related products .14 15 Precision.15 15.1 General Information.15 15.2 Repeatability.15 15.3 Reproducibility.15 16 Test report 16 Annex A (no

21、rmative) Typical chromatograms.17 Bibliography 23 2 egaP4002:366721 NEEN 127663:2004Licensed Copy: Wang Bin, na, Wed Sep 26 07:59:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 12766-3:2004 (E) 3 Foreword This document (EN 12766-3:2004) has been prepared by Technical Committee CEN/TC 19 “Petroleum

22、products, lubricants and related products”, 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 May 2005, and conflicting national standards shall be withdrawn

23、 at the latest by May 2005. EN 12766 consists of the following parts under the general title 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)

24、 Part 2: Calculation of polychlorinated biphenyl (PCB) content Part 3: Determination and quantification of polychlorinated terphenyls (PCT) and polychlorinated benzyl toluenes (PCBT) content by gas chromatography (GC) using an electron capture detector (ECD) According to the CEN/CENELEC Internal Reg

25、ulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands,

26、Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. 3 egaP4002:366721 NEEN 127663:2004Licensed Copy: Wang Bin, na, Wed Sep 26 07:59:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 12766-3:2004 (E) 4 1 Scope This document specifies a method of test for the det

27、ermination of polychlorinated terphenyls (PCT) and polychlorinated benzyl toluenes (PCBT) in petroleum products and related materials by means of a specified gas chromatographic separation procedure. Following the gas chromatographic separation, quantification procedures are described for PCT Aroclo

28、r 5442, PCT Aroclor 5460 and PCBT (Ugilec 141). This document is applicable to unused, used and treated (e.g. dechlorinated) petroleum products including synthetic lubricating oils, to petroleum products and synthetic lubricating oils suitably recovered from other materials (e.g. from waste material

29、s) and to mixtures of vegetable oils. NOTE 1 This document has been developed as an extension of EN 12766 Parts 1 and 2 to provide a method of determining the total PCB content in accordance with Articles 2, 3 and 4 of EC Directive 96/59/EC 1. The total PCB content is calculated by summation of PCB

30、content, determined according to EN 12766-2, and PCTs and PCBTs according to this document. The three classes of materials measured in this standard can be quantified if they occur at concentrations greater than given in Table 1. Table 1 Concentrations for quantification Class of material Minimum co

31、ncentration Method applied 8 mg / kg (EN 12766-2 Method A) PCB, polychlorinated biphenyls 4 mg / kg (EN 12766-2 Method B) PCT 10 mg / kg (EN 12766-3) PCBT 5 mg / kg (EN 12766-3) Total PCB and related products a25 mg / kg (EN 12766-2 and EN 12766-3) aThis value is only a best estimate. Real field con

32、ditions may, depending on the concentrations in the three different classes, result in other, more limited or more improved application ranges. It is the users responsibility to demonstrate that the analysis has been performed in a valid calibrated concentration range. NOTE 2 In order to simplify an

33、d rationalize the analytical operations required for an effective, fast and economic inventory of equipment containing liquids classified as PCBs (as defined by Directive 96/59/EC 1), it is recommended firstly to determine, using an appropriate screening method, the total chlorine content (in mg/kg)

34、. Examples for analytical procedures to determine total chlorine content in fresh, used, or treated insulating oils are: i) pre-dosed colorometric kits to measure 25 mg/kg or 50 mg/kg total chlorine (ref: US EPA SW-846 Method 9079); ii) electrochemical methods in the range 2 mg/kg to 2 000 mg/kg of

35、total chlorine (ref: DEXSILL-2000 DXC - US EPA SW-846 Method 9079 and US EPA SW-846 Method 9078); iii) wavelength dispersive X-ray fluorescence; or iv) oxidative microcoulometry or other scientifically validated analytical methods. From the total chlorine measured for a specific sample, a theoretica

36、l maximum equivalent PCB content can be calculated. When this maximum equivalent PCB content is significantly lower than the limit prescribed by Directive 96/59/EC 1 (50 mg/kg total PCBs) or by local standards (e.g. 25 mg/kg total PCBs), the sample may be considered as “PCB-free“. NOTE 3 When the to

37、tal chlorine content in a sample is higher than the limits described above, it becomes necessary to proceed with gas chromatographic analysis in accordance with this document using the total chlorine content as: i) a guide to establish the level of dilution necessary to operate within the linear ran

38、ge of the ECD detector (EN 12766-1:2000, 10.3.2); 4 egaP4002:366721 NEEN 127663:2004Licensed Copy: Wang Bin, na, Wed Sep 26 07:59:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 12766-3:2004 (E) 5 ii) a method of calculating the ratio between total chlorine content and total PCB for quality control

39、purposes; iii) a method for the classification of the hazard posed by the oil (e.g. at the end of its life cycle, for regeneration, use as fuel and/or disposal in accordance with local regulations). NOTE 4 For the purposes of this document, the terms “% (m/m)” and “% (V/V)” are used to represent res

40、pectively the mass fraction and the volume fraction. WARNING The use of this document can involve hazardous materials, operations and equipment. This document does not purport to address all the safety problems associated with its use. It is the responsibility of the user of this document to establi

41、sh appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated refer

42、ences, the latest edition of the referenced document (including any amendments) applies. 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 chromatography (GC) using an electron captur

43、e 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 ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987) 3 Terms and definitions As define

44、d in several regulations and legislation, the term “PCB” includes “PCT” and also “PCBT”. For the purposes of this document, however, “PCB” is defined on a molecular, chemical basis and its measurement and quantification is described in EN 12766 Part 1 and Part 2. Also, the terms “PCT” and “PCBT” are

45、 defined in chemical terms, and this document describes their measurement and quantification. For analytical results to comply with Directive 96/59/EC, the total sum of PCB obtained from EN 12766-2 and PCT plus PCBT obtained from this document is required. For the purposes of this document, the foll

46、owing terms and definitions apply. 3.1 polychlorinated biphenyl PCB biphenyl substituted by one to 10 chlorine atoms NOTE For legal purposes, congeners with one, two or ten chlorine atoms may be excluded from this definition. 3.2 polychlorinated terphenyl PCT terphenyl substituted by one to 14 chlor

47、ine atoms NOTE There are 8 557 possible congeners of polychlorinated terphenyls. 5 egaP4002:366721 NEEN 127663:2004Licensed Copy: Wang Bin, na, Wed Sep 26 07:59:00 GMT+00:00 2007, Uncontrolled Copy, (c) BSIEN 12766-3:2004 (E) 6 3.3 polychlorinated benzyl toluene PCBT family of compounds monomethyl-p

48、olychlorobiphenyl methane 3.4 congener any chlorinated derivative of biphenyl or terphenyl irrespective of the number of chlorine atoms 3.5 decachlorobiphenyl DCB PCB congener 209 NOTE This congener is used as reference and as an internal standard. 4 Principle A sample preparation (clean-up) procedu

49、re is used to remove most of the impurities likely to interfere with the determination. The clean-up procedure is chosen according to the type of sample. A range of clean-up procedures is described in EN 12766-1:2000, Clause 8 and B.1 to B.5. Groups of PCT and PCBT congeners are determined by gas chromatography using a high efficiency narrow-bore capillary column, an electron capture detector and an internal standard. PCBT and PCT are separated into groups of overlapping congeners and the types of gas chromatograms obt