EN 61619-1997 en Insulating Liquids - Contamination by Polychlorinated Biphenyls (PCBs) Method of Determination by Capillary Column Gas Chromatography《绝缘液体 多氯联苯污染度 毛细管气相色谱测定法 IEC 6.pdf

1、 STD-BSI BS EN bLbL7-ENGL 1777 W ib2Libb7 b2bbLi5 317 W BRITISH STANDARD Insulating liquids - Contamination by polychlorinated biphenyls (PCBS) - Method of determination by capillary column gas chromatography The European Standard EN 61619 : 1997 has the status of a British Stanard ICs 29.035.40 BS

2、EN 61619 : 1997 IEC 1619 : 1997 NO COPYING WTHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW - BS EN 61619 : 1997 irection of the Elecrotechnical hd. No. Da Sector Board, was pubiished under the authority of the Standards Board and comes into effect on 15 July 1997 O BSI 1997 National forew

3、ord Text affected This British Standard is the English language version of EN 61619 : 1997. It is identical with IEC 1619 : 1997. The UK participation in its preparation was entsusted to Technical Committee GEUlO, Fluids for electrotechnical applications, which has the responsibility to: - aid enqui

4、rers to understand the text; - present to the responsible inteniationavEuropean committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; - monitor related intemational and European developments and promulgate them in the UK. A list of organizations

5、represented on this committee can be obtained on request to its secretary. Cross-references Attention is drawn to the fact that annex ZA lists normative references to international publications with their corresponding European publications. The British Standards which implement these international

6、or European publications may be found in the BSI Standards Catalogue under the section entitled International Standards Correspondence Index, or using the Find facility of the BSI Standards Electronic Catalogue. Compliance with a British Standard does not of itself confer immunity from legal obligat

7、ions. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 33, a blank page, an inside back cover and a back cover. ISBN O 680 27781 X - STD-BSI BS EN bLbL7-ENGL 1797 IB1 lb24bb7 b26647 LL E EUROPEAN STANDARD NORME EUROPENNE EUROPAISCHE NORM EN

8、 61619 April 1997 ICs 29.036.4 Descriptors: Electrical insulating matarialS. liquid aloctrical insulating materiels, contamination, polychorinated biphenyls. determination, gar chromatography, capillary columns English version Insulating liquids - Contamination by polychlorinated biphenyls (PCBs) Me

9、thod of determination by capillary column gas chromatography (IEC 61 61 9:1997) Isolants liquides - Contamination par les polychlorobiphnyles (PCB) - Mthode de dtermination par chromatographie en phase gazeuse sur colonne capillaire (CE1 61 61 9: 1997) Isolierflssigkeiten - Verunreinigung durch poly

10、chlorierte Biphenyle (PCBs) Verfahren zur Bestimmung mittels Kapillar-Gaschromatographie (IEC 61 61 9:1997) * * IB This European Standard was approved by CENELEC on 1997-03-1 1. CENELEC members are bound to comply with the CENICENELEC Internai Regulations which stipulate the conditions for giving th

11、is European Standard the status of a national standard without any alteration. Up-to-date lists and bibiiographical references concerning such national standards may be obtained on application to the Central Secretariat or to any CENELEC member. This Euopson Standard exists in three official version

12、s (English, French, German). A version in any other language made by translation under the responsibility of a CENELEC member into its own language and notitkd to tho Central Secretariat has the sama statua as the official verrions. CENUK: members am the national electrotechnical committees of Austr

13、ia, Belgium, Denmark, Finland, Franca, germ, Grme, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain. Sweden, Switzerland and United Kingdom. CENELEC European Committee for Electrotechnical Standardization Comit Europen de Normalisation Electrotechnique Europisches Komitee fr

14、 Elektrotechnische Normung Centrd Secretariat: rue de Stassart 36, B - 1050 Brurads * 1997 CENELEC - All rights of exploitation in any form and by any means reserved worldwide for CENELEC members. Ref. No. EN 61619:1997 E _ _ STD-BSI BS EN bLbLS-ENGL 1777 Lb24bb9 062bb48 028 W Page 2 EN 61619 : 1997

15、 Foreword The text of document 10/379/FDIS, future edition 1 of IEC 61619, prepared by IEC TC 10, Fluids for electrotechnical applications, was submitted to the IEC-CENELEC parallel vote and was approved by CENELEC as EN 61 61 9 on 1997-03-1 1. The following dates were fixed: - latest date by which

16、the EN has to be implemented at national level by publication of an identical national standard or by endorsement (dopl 1998-01 -01 - latest date by which the national standards conflicting with the EN have to be withdrawn (daw) 1 998-0 1 -0 1 Annexes designated “normative“ are part of the body of t

17、he standard. Annexes designated “informative“ are given for information only. In this standard, annexes A and ZA are normative and annexes B and C are informative. Annex ZA has been added by CENELEC. Endorsement notice The text of the International Standard IEC 61619:1997 was approved by CENELEC as

18、a European Standard without any modification. In the official version, for annex C, Bibliography, the following note has to be added for the standard indicated: IEC 00567 NOTE: Harmonized as EN 00567:1992 (not modifid). Page 3 EN 61619 : 1997 CONTENTS Clause Page 1 2 3 4 5 6 7 8 9 10 11 12 13 14 Sco

19、pe and object Normative reference . . . . ._ . . _. _._._. ._. . ._. . . . . _ ._ ._. . ._. ._ Definitions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . , . . . . Principle . . . . . . . . . , . . . _ . . ._. . . . . . _ . . . . . . , .

20、Reagents and auxiliary materials . . . . Apparatus . . . . , . . . . . . . . . . . . . . . . . . _. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . Sample _ ,. . . . _. ._. . _ _._ . _._ ._. . . . . . .

21、 . . _. _. . . . . . Chromatograph operating conditions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . , . . . . . Data-processing system . . . . . . ._. . . . . . _ _._. . . . . . _. . . . . . . . . Checks of instrumen

22、tal performance . . . Procedure . . . . . ._ . . . . . . . . . . . . . . . . . . . . . . . ._ ._. . ._. , Test report . Detection limit Precision . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . , . . . . . . . . . . . . . . . . . . . . .

23、. . . . . . . . . . . 4 4 4 5 5 6 9 9 10 11 13 18 18 19 Annexes 20 A Test mixtures . B General informations 27 C Bibliography . 32 ZA Normative references to international publications with their corresponding 33 European publications . Page 4 EN 61619 : 1997 INSULATING LIQUIDS - CONTAMINATION BY PO

24、LYCHLORINATED BIPHENYLS (PCBS) - METHOD OF DETERMINATION BY CAPILLARY COLUMN GAS CHROMATOGRAPHY 1 Scope and object This International Standard specifies a method for the determination of polychlorinated biphenyl (PCB) concentration in non-halogenated insulating liquids by high-resolution capillary c

25、olumn gas chromatography using an electron capture detector (ECD). The method gives the total PCB content and is especially useful when a detailed analysis of PCB congeners is necessary. Other methods, such as IEC 60997, may be used when a less detailed analysis is acceptable. The method is applicab

26、le to unused, reclaimed (including dechlorinated and chemically and/or physically treated), or used insulating liquids contaminated by PCBs. 2 Normative reference The following normative document contains provisions which, through reference in this text, constitute provisions of this normative docum

27、ent. At the time of publication, the edition indicated was valid. All normative documents are subject to revision, and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the normative document indicated bel

28、ow. Members of IEC and IS0 maintain registers of current valid International Standards. IEC 60475: 1974, Method of sampling liquid dielectrics 3 Definitions For the purposes of the international Standard, the following definitions apply: 3.1 Polychlorinated biphenyl (PCB) A biphenyl substituted by o

29、ne to ten chlorine atoms. NOTE - For legal purposes, congeners with one, two or ten chlorine atoms may be excluded from this definition. 3.2 Congener All the chlorine derivatives of biphenyl, irrespective of the number of chlorine atoms, are termed congeners. NOTE - There are 209 possible PCB congen

30、ers.These are listed in table 8.1. The congener numbers (IUPAC) are for easy identification; they do not represent the order of chromatographic elution. international Union of Pure and Applied Chemistry. - - STD-BSI BS EN bLbL7-ENGL 1997 M 1b24bb7 Ob2bb51 bL2 M Page 5 EN 61619 : 1997 4 Principle The

31、 PCB congeners are determined by temperature programmed gas chromatography. The chromatograph uses a high-efficiency capillary column to separate the PCBs into single or small groups of overlapping congeners. The sensitivity of the electron capture detector (ECD) may be reduced by the presence of mi

32、neral oil. In this method the sample is diluted 100 times to reduce this effect to a minimum. A sample preparation (clean-up) procedure is used to remove most of the impurities likely to interfere with the determination. Reference compounds are included to enable calculation of experimental relative

33、 retention times (ERRTs) which are compared to a data file of peak ERRTs to identify individual or groups of unresolved congeners. An internal standard is added for quantification. Relative response factors (RRF), taken from the data files (9.1), corrected by experimental relative response factors (

34、ERRFs) obtained from reference compounds, are applied to identified peaks to quantify the individual (or groups of) congeners, and the values summed to give total PCB content. 5 Reagents and auxiliary materials 5.1 Reagents and standards All reagents and materials, including those for clean-up, shal

35、l be free from PCB contamination and compounds responding to the ECD. 5.1.1 Solvent Hexane, heptane, cyclohexane or isooctane (2,2,44rimethylpentane), high purity, free from PCB contamination and low in compounds that respond to the ECD. 5.1.2 Hexachiorobenzene Purity 99 % at least, used for checkin

36、g detector sensitivity. 5.1.3 Insulating liquid An insulating liquid, checked to be free from PCBs or other interfering substances, of the same type as is present in the sample. 5.1.4 Congener 30 solution (C 30) 10 mg/l in solvent (5.1.1) purchased in solution or prepared from pure material (purity

37、99 % at least). 5.1.5 Congener 209 (DCB), decachlorobiphenyi solution 10 mgil in solvent (5.1.1) purchased in solution or prepared from pure material (purity 99% at least). Page 6 EN 61619 : 1997 5.1.6 Calibration solution of selected PCB congeners Certified calibration mixture in solvent (5.1.1) co

38、ntaining at least the following PCB congeners at a concentration of 10 mg/l each: 18, 28, 31, 44, 52, 101, 118, 138, 149, 153, 170, 180, 194 and 209 (see 8.3). 5.2 Commercial PCB standards (see 8.4) 5.2.1 Solutions of Aroclors 1242, 1254 and 1260 in solvent (5.1.1) Concentration required 50 mg/l or

39、more, typically 1000 mg/l. 5.2.2 Solutions of Aroclors 1242, 1254 and 1260 in oil 50 mg/kg solutions of Aroclors 1242, 1254 and 1260 in unused insulating liquid, either purchased as standardized solutions or prepared from pure material. 5.3 Gas chromatography gases 5.3.1 Carrier gas: helium or hydro

40、gen, purity 99,99 % at least. 5.3.2 Make-up gas: argodmethane, 95 % / 5 %. Alternatively, 99,99 % minimum purity nitrogen can be used. 5.4 Internal standewreference solutions . NOTE - Standards should be stored in a cool, dark place 5.4.1 Internal standard solution 2 (IS 2) 2 mg/l C209 (DCB), 2 mg/l

41、 C30. Pipette (5.8.3) 5 ml of DCB solution (5.1.5) and 5 ml C30 solution (5.1.4) into a 25 ml volumetric flask, make up to the mark with solvent (5.1.1). 5.4.2 Internal standard solution 0,s (IS 0,5) 0,5 mg/l C209 (DCB), 0,5 mg/l C30. Follow 5.4.1 using a 100 ml volumetric flask. 5.5 Test mixture so

42、lution (for system evaluation) Into a 20 ml volumetric flask: weigh, to the nearest 0,001 g, 0,50 g of 50 mg/kg AroclorJ 1260, plus 0,50 g of 50 mg/kg Arodor 1254 plus 1,OO g of 50 mg/kg Aroclor 1242 solutions in insulating liquid (5.2.2). Add by pipette 1 ml of IS 2 solution (5.4.1) and make up to

43、volume with solvent. Prior to use this solution shall be treated as per 11.1.3. 5.6 Calibration - congener mix stock solution Into a 20 ml volumetric flask: weigh, to the nearest 0,001 g, 2,O g of insulating liquid (5.1.3) and add 1 ml of the calibration PCB congener mix (5.1.6). Make up to the mark

44、 with solvent (5.1.1). STD-BSI BS EN bLbL7-ENGL 1997 W lb24bb9 Ub2bb53 475 Page 7 EN 61619 : 1997 5.7 Congener mix calibration solution (for response factors) Submit 500 pI of solution (5.6) to the clean-up (11.1.3). The final solution is suitable for the determination of relative factors. Prepare a

45、 fresh solution monthly. 5.8 Glassware 5.8.1 Volumetric flasks 100, 50, 25, 10 and 5 ml (tolerance better than f 0,4%) 5.8.2 Syringes and pipettes: 500 pl f 5 pI syringe or pipette, 1 pI and 5 pI gas chromatography precision syringes. 5.8.3 Bulb pipettes (volumetric) 1, 2 and 5 ml class A 5.9 Column

46、s and accessories for sample preparation 5.9.1 Commercial or self-packed solid-phase extraction columns: 3 ml silica gel column, adsorbent weight 500 mg, particle size 40 pm, 3 ml benzenesulphonic acid column, adsorbent weight 500 mg, particle size 40 pm. 5.9.2 Column adapter, for joining two column

47、s 5.9.3 Vacuum manifold column processor - optional 6 Apparatus 6.1 Gas chromatograph (GC) A high-resolution gas chromatograph with accurately reproducible oven temperature control, capable, when used with the appropriate column and conditions, of resolving the test mixture (5.5) at least as well as

48、 in figure A.l (90 peaks observed) and of reproducing relative retention times to within i 0,0015. The gas lines (carrier gas and make-up gas) shall be fitted with water vapour and oxygen traps. The carrier gas supply system shall be capable of running with a 50 m column at maximum efficiency using

49、He or H2 carrier gas, e.g. adequate column head pressure. The oven temperature programmer shall have a range that can be set to attain the required resolution. 6.1 . 1 Injector Either an “on-column” injector or a “spli/splitless” injector may be used. Page 8 EN 61619 : 1997 6.1.2 Columns Either a cross-linked 5 % phenyl-methyl silicone, stationary phase coated onto fused silica capillary column or a similar chemically bonded phase column. Their dimensions shall be as follows: length = 50m to60m; internal diameter =