BS EN 60666-2010 Detection and determination of specified additives in mineral insulating oils《矿物质绝缘油中制定添加剂的探测和测定》.pdf

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1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationDetection and determination of specified additives in mineral insulating oilsBS EN 60666:2010National forewordThis British Standard is the UK implementation of EN 60666:2010. It

2、is identical to IEC 60666:2010. It supersedes BS 5984:1980 which is withdrawn.The UK participation in its preparation was entrusted to Technical CommitteeGEL/10, Fluids for electrotechnical applications.A list of organizations represented on this committee can be obtained onrequest to its secretary.

3、This publication does not purport to include all the necessary provisions of acontract. Users are responsible for its correct application. BSI 2010ISBN 978 0 580 58307 0ICS 17.220.99; 29.040.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was p

4、ublished under the authority of the StandardsPolicy and Strategy Committee on 31 August 2010.Amendments issued since publicationAmd. No. Date Text affectedBRITISH STANDARDBS EN 60666:2010EUROPEAN STANDARD EN 60666 NORME EUROPENNE EUROPISCHE NORM July 2010 CENELEC European Committee for Electrotechni

5、cal Standardization Comit Europen de Normalisation Electrotechnique Europisches Komitee fr Elektrotechnische Normung Management Centre: Avenue Marnix 17, B - 1000 Brussels 2010 CENELEC - All rights of exploitation in any form and by any means reserved worldwide for CENELEC members. Ref. No. EN 60666

6、:2010 E ICS 17.220.99; 29.040.10 Supersedes HD 415 S1:1981English version Detection and determination of specified additives in mineral insulating oils (IEC 60666:2010) Dtection et dosage dadditifs spcifiques prsents dans les huiles minrales isolantes (CEI 60666:2010) Nachweis und Bestimmung spezifi

7、zierter Additive in Isolierflssigkeiten auf Minerallbasis (IEC 60666:2010) This European Standard was approved by CENELEC on 2010-07-01. CENELEC members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a nati

8、onal standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Central Secretariat or to any CENELEC member. This European Standard exists in three official versions (English, French, German). A version i

9、n any other language made by translation under the responsibility of a CENELEC member into its own language and notified to the Central Secretariat has the same status as the official versions. CENELEC members are the national electrotechnical committees of Austria, Belgium, Bulgaria, Croatia, Cypru

10、s, the Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, the Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN 60666:2010EN 60666:2010

11、- 2 - Foreword The text of document 10/803/FDIS, future edition 2 of IEC 60666, prepared by IEC TC 10, Fluids for electrotechnical applications, was submitted to the IEC-CENELEC parallel vote and was approved by CENELEC as EN 60666 on 2010-07-01. This European Standard supersedes HD 415 S1:1981. The

12、 main changes with respect to HD 415 S1:1981 are listed below: a change in the title from “Detection and determination of specified anti-oxidant additives in insulating oils” to “Detection and determination of specified additives in mineral insulating oils”. The previous edition only addressed the d

13、etection and determination of anti-oxidant additives, with particular regard to the DBPC, phenolic inhibitors and anthranilic acid; more advanced methods for the determination of such anti-oxidant additives; new Annexes B and C which provide methods for the determination of two additives different f

14、rom the anti-oxidants. In particular, Annex B contains a method for the determination of the concentration in used and unused insulating mineral oils of passivators of the family of derivatives of benzotriazole. Annex C contains a method for the qualitative identification of pour point depressants u

15、sed in some commercially available paraffinic oils to improve their low temperature properties. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and CENELEC shall not be held responsible for identifying any or all such patent r

16、ights. The following dates were fixed: latest date by which the EN has to be implemented at national level by publication of an identical national standard or by endorsement (dop) 2011-04-01 latest date by which the national standards conflicting with the EN have to be withdrawn (dow) 2013-07-01 Ann

17、ex ZA has been added by CENELEC. _ Endorsement notice The text of the International Standard IEC 60666:2010 was approved by CENELEC as a European Standard without any modification. In the official version, for Bibliography, the following notes have to be added for the standards indicated: 3 IEC 6042

18、2 NOTE Harmonized as EN 60422. 5 IEC 61198 NOTE Harmonized as EN 61198. _ BS EN 60666:2010- 3 - EN 60666:2010 Annex ZA (normative) Normative references to international publications with their corresponding European publications The following referenced documents are indispensable for the applicatio

19、n of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. NOTE When an international publication has been modified by common modifications, indicated by (mod), the relevant EN/HD

20、 applies. Publication Year Title EN/HD Year IEC 60296 - Fluids for electrotechnical applications - Unused mineral insulating oils for transformers and switchgear EN 60296 - IEC 60475 - Method of sampling liquid dielectrics - - ISO 5725 Series Accuracy (trueness and precision) of measurement methods

21、and results - - BS EN 60666:2010 2 60666 IEC:2010 CONTENTS INTRODUCTION.6 1 Scope.7 2 Normative references .7 3 Methods for the determination of anti-oxidant additives 7 3.1 Determination of phenolic and amine-based antioxidants by infrared (IR) spectrophotometry Method A 7 3.1.1 Introductory remark

22、 .7 3.1.2 Equipment, materials and solvents 8 3.1.3 Sample preparation .8 3.1.4 Calibration.8 3.1.5 Analysis.9 3.1.6 Calculation 9 3.1.7 Precision .10 3.1.8 Repeatability .10 3.1.9 Reproducibility.10 3.1.10 Report .10 3.2 Determination of 2,6-di-tert-butyl-para-cresol by IR spectrophotometry Method

23、B.10 3.2.1 Calibration.11 3.2.2 Sample test New or used oil .11 3.2.3 Precision .11 3.2.4 Repeatability .11 3.2.5 Reproducibility.11 3.2.6 Report .12 3.3 Determination of 2,6-di-tert-butyl-para-cresol (DBPC) by high performance liquid chromatography (HPLC).12 3.3.1 Introductory remark .12 3.3.2 Mate

24、rials and equipment .12 3.3.3 Reagents and solvents 12 3.3.4 Solid-liquid extraction 12 3.3.5 Analysis of the extract .12 3.3.6 Calculation 13 3.3.7 Precision .13 3.3.8 Repeatability .13 3.3.9 Reproducibility.13 3.3.10 Report .13 3.4 Determination of phenolic inhibitors by gas chromatography Mass sp

25、ectrometry (GC-MS).14 3.4.1 Summary of method 14 3.4.2 Example of instrument parameters 14 3.4.3 GC accessories .14 3.4.4 Calibration standard solutions .14 3.4.5 Internal standard solutions 14 3.4.6 Preparation of samples and calibration standards15 3.4.7 Analytical procedure15 3.4.8 Calculation of

26、 results .15 3.4.9 Precision .16 BS EN 60666:201060666 IEC:2010 3 3.4.10 Report .16 Annex A (informative) Detection of anti-oxidant additives by thin layer chromatography (TLC) 17 Annex B (informative) Analysis method for determination of passivators in mineral oils by high performance liquid chroma

27、tography (HPLC) .22 Annex C (informative) Determination of pour point depressants by gel permeation chromatography30 Bibliography32 Figure A.1 Typical infrared spectrum to determine DBPC content 19 Figure A.2 Typical infrared spectrum with 0,3 % DBPC 20 Figure A.3 Typical HPLC chromatogram to determ

28、ine DBPC content .21 Figure B.1 UV spectra of TTAA (in blue) and BTA (in red)26 Table B.1 Examples of separation conditions.26 Table B.2 Repeatability29 Table B.3 Reproducibility .29 BS EN 60666:2010 6 60666 IEC:2010 INTRODUCTION General caution, health, safety and environmental protection This Inte

29、rnational Standard does not purport to address all the safety problems associated with its use. It is the responsibility of the user of the standard to establish appropriate health and safety practices and determine the applicability of regulatory limitations prior to use. The mineral oils which are

30、 the subject of this standard should be handled with due regard to personal hygiene. Direct contact with eyes may cause slight irritation. In the case of eye contact, irrigation with copious quantities of clean running water should be carried out and medical advice sought. Some of the tests specifie

31、d in this standard involve the use of processes that could lead to a hazardous situation. Attention is drawn to the relevant standard for guidance. This standard involves mineral oils, chemicals and used sample containers. The disposal of these items should be carried out in accordance with current

32、national legislation with regard to the impact on the environment. Every precaution should be taken to prevent the release into the environment of mineral oil. BS EN 60666:201060666 IEC:2010 7 DETECTION AND DETERMINATION OF SPECIFIED ADDITIVES IN MINERAL INSULATING OILS 1 Scope The methods described

33、 in this International Standard concern the detection and determination of specified additives in unused and used mineral insulating oils. The detection methods may be applied to assess whether or not a mineral insulating oil contains an additive as specified by the supplier. The determination metho

34、ds are used for the quantitative determination of additives known to be present or previously detected by the appropriate detection method. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited a

35、pplies. For undated references, the latest edition of the referenced document (including any amendments) applies. IEC 60296, Fluids for electrotechnical applications Unused mineral insulating oils for transformers and switchgear IEC 60475, Method of sampling liquid dielectrics ISO 5725 (all parts),

36、Accuracy (trueness and precision) of measurement methods and results 3 Methods for the determination of anti-oxidant additives 3.1 Determination of phenolic and amine-based antioxidants by infrared (IR) spectrophotometry Method A 3.1.1 Introductory remark This method determines the amount of 2,6-di-

37、tert-butyl-para-cresol (DBPC) in unused and used mineral oils by measurement of the infrared absorption at the (OH) stretching frequency of hindered phenols. It can also be used to determine the amount of 2,6-di-tert-butyl-phenol (DBP), but does not discriminate between them. The previous test metho

38、d in the first edition of IEC 60666 described a procedure for the determination of specific antioxidants using IR techniques. This test method was satisfactory with new oils, where no oxidation by-products interfere with the antioxidant. However, this method was less satisfactory for used oils becau

39、se oxidation by-products may modify the IR baseline, making the detection and quantification of the antioxidants difficult. To overcome this problem, a procedure for preparing a reference oil to be used as a baseline was described. Unfortunately, this procedure was difficult to perform, was time-con

40、suming and did not ensure that the new baseline matched adequately that of the oil to be analysed, because the content of some components of the baseline oil and the analysed oil could be quite different. This new method describes a procedure for preparing reference, antioxidant-free oils by solid p

41、hase extraction (SPE) using silica gel. BS EN 60666:2010 8 60666 IEC:2010 3.1.2 Equipment, materials and solvents The following materials and reagents are used: FT-IR or double-beam IR spectrometer having matched 1 mm sodium chloride cells (other materials are accepted provided they do not absorb IR

42、 radiation in the range 3 000 cm1to 3 800 cm1); 5 ml or 10 ml round-bottom flasks; 5 ml or 10 ml beakers; rotary evaporator; silica gel cartridges (1 g or 2 g size is satisfactory); n-pentane, analytical grade. 3.1.3 Sample preparation Into a beaker pour 1 g of the oil to be analysed for antioxidant

43、s, add 2 ml of analytical grade n-pentane and mix thoroughly. Filter the solution through a silica gel cartridge and recover the eluate in a round-bottom flask. Evaporate the n-pentane in the rotary evaporator. Take a portion large enough to completely fill one IR cell of the oil that remains in the

44、 flask, fill one IR cell and put it on the reference beam of the spectrometer. Fill a second IR cell with the oil to be analysed, which has not been submitted to the filtration process, and insert it on the analytical beam of the spectrometer. Record the IR spectrum as described in 3.1.5. 3.1.4 Cali

45、bration Prepare standard calibration solutions by dissolving weighed amounts of DBP or DBPC inhibitor in weighed amounts of antioxidant-free oil, prepared if necessary from the oil sample under test using the procedure in 3.1.3 (larger cartridges and amounts of oil will be necessary). The maximum li

46、fe of the standard solution shall be six months. NOTE The calibration solutions may be prepared using an unused, inhibitor-free oil, provided the base oil is known to be the same as that under test. The oil should be tested by this procedure to ensure that no inhibitor is detectable. This alternativ

47、e should not be used where the oil under test is heavily aged. Prepare at least five calibration solutions, covering the range 0,02 % to 0,50 % inhibitor by mass. Intermediate standards may be prepared if necessary when the approximate concentration of inhibitor in the sample is known. The absorbanc

48、e (at 3 650 cm1for DBPC) of the calibration solutions is recorded as described in 3.1.5 and a calibration curve of absorbance against per cent inhibitor content produced. The calibration should be a straight line passing through the origin, according to the Beer-Lambert law of absorption: KCDIIA =o1

49、0log where BS EN 60666:201060666 IEC:2010 9 A is the absorbance; Io is the intensity of incident radiation; I is the intensity of transmitted radiation; K is the extinction coefficient (constant for (O-H) of DBPC); C is the concentration of DBPC in percentage by mass; D is the cell path-length. Since K and D are constant for this determination, A is directly proportional to C. 3.1.5 Analysis 1. FT-IR instrument Check the equipment. The quality tests