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    IEC TR 62036-2007 Mineral insulating oils - Oxidation test method based on differential scanning calorimetry (DSC)《矿物绝缘油.基于差示扫描量热法(DSC)的氧化试验法》.pdf

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    IEC TR 62036-2007 Mineral insulating oils - Oxidation test method based on differential scanning calorimetry (DSC)《矿物绝缘油.基于差示扫描量热法(DSC)的氧化试验法》.pdf

    1、 TECHNICAL REPORT IECCEIRAPPORT TECHNIQUE TR 62036First editionPremire dition2007-04Mineral insulating oils Oxidation stability test method based on differential scanning calorimetry (DSC) Huiles minrales isolantes Mthode dessai pour valuer la stabilit doxydation fonde sur lanalyse calorimtrique dif

    2、frentielle par balayage Reference number Numro de rfrence IEC/CEI/TR 62036:2007 THIS PUBLICATION IS COPYRIGHT PROTECTED Copyright 2007 IEC, Geneva, Switzerland All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, elec

    3、tronic or mechanical, including photocopying and microfilm, without permission in writing from either IEC or IECs member National Committee in the country of the requester. If you have any questions about IEC copyright or have an enquiry about obtaining additional rights to this publication, please

    4、contact the address below or your local IEC member National Committee for further information. Droits de reproduction rservs. Sauf indication contraire, aucune partie de cette publication ne peut tre reproduite ni utilise sous quelque forme que ce soit et par aucun procd, lectronique ou mcanique, y

    5、compris la photocopie et les microfilms, sans laccord crit de la CEI ou du Comit national de la CEI du pays du demandeur. Si vous avez des questions sur le copyright de la CEI ou si vous dsirez obtenir des droits supplmentaires sur cette publication, utilisez les coordonnes ci-aprs ou contactez le C

    6、omit national de la CEI de votre pays de rsidence. IEC Central Office 3, rue de Varemb CH-1211 Geneva 20 Switzerland Email: inmailiec.ch Web: www.iec.ch About the IEC The International Electrotechnical Commission (IEC) is the leading global organization that prepares and publishes International Stan

    7、dards for all electrical, electronic and related technologies. About IEC publications The technical content of IEC publications is kept under constant review by the IEC. Please make sure that you have the latest edition, a corrigenda or an amendment might have been published. Catalogue of IEC public

    8、ations: www.iec.ch/searchpub The IEC on-line Catalogue enables you to search by a variety of criteria (reference number, text, technical committee,). It also gives information on projects, withdrawn and replaced publications. IEC Just Published: www.iec.ch/online_news/justpub Stay up to date on all

    9、new IEC publications. Just Published details twice a month all new publications released. Available on-line and also by email. Customer Service Centre: www.iec.ch/webstore/custserv If you wish to give us your feedback on this publication or need further assistance, please visit the Customer Service

    10、Centre FAQ or contact us: Email: csciec.ch Tel.: +41 22 919 02 11 Fax: +41 22 919 03 00 A propos de la CEI La Commission Electrotechnique Internationale (CEI) est la premire organisation mondiale qui labore et publie des normes internationales pour tout ce qui a trait llectricit, llectronique et aux

    11、 technologies apparentes. A propos des publications CEI Le contenu technique des publications de la CEI est constamment revu. Veuillez vous assurer que vous possdez ldition la plus rcente, un corrigendum ou amendement peut avoir t publi. Catalogue des publications de la CEI: www.iec.ch/searchpub/cur

    12、_fut-f.htm Le Catalogue en-ligne de la CEI vous permet deffectuer des recherches en utilisant diffrents critres (numro de rfrence, texte, comit dtudes,). Il donne aussi des informations sur les projets et les publications retires ou remplaces. Just Published CEI: www.iec.ch/online_news/justpub Reste

    13、z inform sur les nouvelles publications de la CEI. Just Published dtaille deux fois par mois les nouvelles publications parues. Disponible en-ligne et aussi par email. Service Clients: www.iec.ch/webstore/custserv/custserv_entry-f.htm Si vous dsirez nous donner des commentaires sur cette publication

    14、 ou si vous avez des questions, visitez le FAQ du Service clients ou contactez-nous: Email: csciec.ch Tl.: +41 22 919 02 11 Fax: +41 22 919 03 00 TECHNICAL REPORT IECCEIRAPPORT TECHNIQUE TR 62036First editionPremire dition2007-04Mineral insulating oils Oxidation stability test method based on differ

    15、ential scanning calorimetry (DSC) Huiles minrales isolantes Mthode dessai pour valuer la stabilit doxydation fonde sur lanalyse calorimtrique diffrentielle par balayage PRICE CODE CODE PRIX M For price, see current cataloguePour prix, voir catalogue en vigueur Commission Electrotechnique Internation

    16、aleInternational Electrotechnical Commission 2 TR 62036 IEC:2007 CONTENTS FOREWORD.3 INTRODUCTION.5 1 Scope.6 2 General remarks.6 3 Effect of temperature on oxidation induction time .6 3.1 Isothermal .6 3.2 Temperature-programmed runs .7 4 Effect of sample size on oxidation induction time7 4.1 Inhib

    17、ited oil .7 4.2 Uninhibited oil .7 5 Other factors effecting oxidation induction time 8 6 Reliability of method.8 7 Different instruments 8 8 Interpretation of curves.9 9 Conclusion .9 Bibliography13 Table 1 Oxidation induction time of oil samples at different temperature programmes10 Table 2 Oxidat

    18、ion induction time of oil samples at different sample weight.10 Table 3 Repeatability of oxidation induction time by PDSC 10 Table 4 Reproducibility of oxidation induction time by PDSC11 Table 5a DSC Results analyzed at different laboratories Uninhibited oil12 Table 5b DSC Results analyzed at differ

    19、ent laboratories Inhibited oil12 TR 62036 IEC:2007 3 INTERNATIONAL ELECTROTECHNICAL COMMISSION _ MINERAL INSULATING OILS OXIDATION STABILITY TEST METHOD BASED ON DIFFERENTIAL SCANNING CALORIMETRY (DSC) FOREWORD 1) The International Electrotechnical Commission (IEC) is a worldwide organization for st

    20、andardization comprising all national electrotechnical committees (IEC National Committees). The object of IEC is to promote international co-operation on all questions concerning standardization in the electrical and electronic fields. To this end and in addition to other activities, IEC publishes

    21、International Standards, Technical Specifications, Technical Reports, Publicly Available Specifications (PAS) and Guides (hereafter referred to as “IEC Publication(s)”). Their preparation is entrusted to technical committees; any IEC National Committee interested in the subject dealt with may partic

    22、ipate in this preparatory work. International, governmental and non-governmental organizations liaising with the IEC also participate in this preparation. IEC collaborates closely with the International Organization for Standardization (ISO) in accordance with conditions determined by agreement betw

    23、een the two organizations. 2) The formal decisions or agreements of IEC on technical matters express, as nearly as possible, an international consensus of opinion on the relevant subjects since each technical committee has representation from all interested IEC National Committees. 3) IEC Publicatio

    24、ns have the form of recommendations for international use and are accepted by IEC National Committees in that sense. While all reasonable efforts are made to ensure that the technical content of IEC Publications is accurate, IEC cannot be held responsible for the way in which they are used or for an

    25、y misinterpretation by any end user. 4) In order to promote international uniformity, IEC National Committees undertake to apply IEC Publications transparently to the maximum extent possible in their national and regional publications. Any divergence between any IEC Publication and the corresponding

    26、 national or regional publication shall be clearly indicated in the latter. 5) IEC provides no marking procedure to indicate its approval and cannot be rendered responsible for any equipment declared to be in conformity with an IEC Publication. 6) All users should ensure that they have the latest ed

    27、ition of this publication. 7) No liability shall attach to IEC or its directors, employees, servants or agents including individual experts and members of its technical committees and IEC National Committees for any personal injury, property damage or other damage of any nature whatsoever, whether d

    28、irect or indirect, or for costs (including legal fees) and expenses arising out of the publication, use of, or reliance upon, this IEC Publication or any other IEC Publications. 8) Attention is drawn to the Normative references cited in this publication. Use of the referenced publications is indispe

    29、nsable for the correct application of this publication. 9) Attention is drawn to the possibility that some of the elements of this IEC Publication may be the subject of patent rights. IEC shall not be held responsible for identifying any or all such patent rights. The main task of IEC technical comm

    30、ittees is to prepare International Standards. However, a technical committee may propose the publication of a technical report when it has collected data of a different kind from that which is normally published as an International Standard, for example “state of the art“. IEC 62036, which is a tech

    31、nical report, has been prepared by IEC technical committee 10: Fluids for electrotechnical applications. 4 TR 62036 IEC:2007 The text of this technical report is based on the following documents: Enquiry draft Report on voting 10/676/DTR 10/690/RVC Full information on the voting for the approval of

    32、this technical report can be found in the report on voting indicated in the above table. This publication has been drafted in accordance with the ISO/IEC Directives, Part 2. The committee has decided that the contents of this publication will remain unchanged until the maintenance result date indica

    33、ted on the IEC web site under “http:/webstore.iec.ch“ in the data related to the specific publication. At this date, the publication will be reconfirmed, withdrawn, replaced by a revised edition, or amended. TR 62036 IEC:2007 5 INTRODUCTION The existing methods to assess oxidation stability of miner

    34、al insulating oil are very time consuming. A faster method is necessary for effective quality control and status monitoring. Differential scanning calorimetry (DSC) as a technique has been used for monitoring grease and lubricants oxidation stability. The use of DSC for evaluation of oil oxidation s

    35、tability was originally suggested to IEC, TC 10 following publication of a literature review of DSC oxidation tests performed on petroleum products (10/367/INF April 1996). During IECs TC 10 meeting in Geneva, 1998, it was decided to set up a working group for development of a standard based on DSC

    36、for rapid evaluation of mineral insulating oil oxidation stability. 6 TR 62036 IEC:2007 MINERAL INSULATING OILS OXIDATION STABILITY TEST METHOD BASED ON DIFFERENTIAL SCANNING CALORIMETRY (DSC) 1 Scope The purpose of IEC 62036, which is a technical report, is to develop a rapid oxidation stability te

    37、st method based on differential scanning calorimetry (DSC) to assess the oxidation stability of mineral insulating oils. 2 General remarks The main function of insulating oil is insulation and cooling. The expected life span of transformer oil is 25 to 40 years, largely depending on operating temper

    38、ature and electrical load. Specifications are prepared and used to fulfil all criteria required for proper functioning of the oil in service. Life expectancy from insulating oil has a large economic impact on the cost of operation of a unit. The oxidation stability test is an important test as this

    39、will evaluate, to some extent, the life of the oil in service. Resistance of an oil oxidation is very much dependant on the refining process and type of crude oil. Both under-refined and over-refined oils may exhibit poor oxidation stability. The complex process of oxidation of in-service oils occur

    40、s slowly at the normal operating temperature of the transformer and is dependant on temperature, oxygen and catalyst. In the first stage of oil oxidation, radicals and peroxides are produced. These compounds are unstable and rapidly convert to volatile and soluble acids and finally producing insolub

    41、le material or sludge. All of these products have an adverse effect on electrical and physical properties of oil. The oil may reach a stage where it is not fit for its intended purpose. To establish a long service life for the oil, an oxidation stability test is performed on the unused oil. There ar

    42、e several standard test methods for evaluation of the oxidation stability of transformer oil. The recommended international test method is IEC 61125. This test involves oxidizing the oil at 120 C for 164 h and then measuring the acidity, sludge and dielectric dissipation factor (DDF). Other national

    43、 test methods are based on the same principal and are time consuming. On delivery, it is required to test the oil for compliance with the specification. As this test is very time consuming, results are usually retrospective. Clearly, existing methods are time consuming and not very sensitive. Althou

    44、gh there is no direct relation between the oil oxidation stability test and service life of the oil, oils that are very stable and resist oxidation are clearly preferred. Therefore, a fast method of determining the oxidation stability is needed for rapid evaluation of the oil and compliance to the s

    45、pecification. In order to evaluate high pressure differential scanning calorimetry (PDSC) as a technique for testing oxidation stability of transformer oil and to establish a suitable method, transformer oil samples were analysed under varying conditions. 3 Effect of temperature on oxidation inducti

    46、on time 3.1 Isothermal Six samples of transformer oil (A-F) were analysed using PDSC at different temperature programmes. Samples B and D were inhibited transformer oil, the remainder were uninhibited and sample F was a used oil. Oxygen at 300 psi was applied in each case and the sample weight was k

    47、ept constant at 4 mg. The results are shown in Table 1. It was found that below 165 C, no phase transition occurred in any of the six samples. Temperatures higher than expected, of up to 260 C were required to give peaks in a reasonable time. At the lower TR 62036 IEC:2007 7 temperature, only sample

    48、 D gave a peak at around 45 min. When this sample was run at 170 C, the peak become sharper and clear and occurred at an onset of around 40 min. At 175 C, the peak occurred at around 30 min and was sharper still. The same trend was observed in sample B, showing decreasing induction time with increas

    49、ing temperature, but oxidation occurred after a slightly longer time. Sample B and D were inhibited oils, which showed a clear and sharp peak following the rapid oxidation and depletion of the inhibitor. 3.2 Temperature-programmed runs The uninhibited oils, A, C, E and F showed no clearly defined peak in the thermograms of isothermal runs. Oxidation did not occur


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