1、 INTERNATIONAL STANDARD IECCEINORME INTERNATIONALE60450Edition 2.12007-07Measurement of the average viscometric degree of polymerization of new and aged cellulosic electrically insulating materials Mesure du degr de polymrisation moyen viscosimtrique des matriaux isolants cellulosiques neufs et viei
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15、0Edition 2.12007-07Measurement of the average viscometric degree of polymerization of new and aged cellulosic electrically insulating materials Mesure du degr de polymrisation moyen viscosimtrique des matriaux isolants cellulosiques neufs et vieillis usage lectrique Commission Electrotechnique Inter
16、nationaleInternational Electrotechnical Commission For price, see current cataloguePour prix, voir catalogue en vigueur CE PRICE CODE CODE PRIX Edition 2:2004 consolidated with amendment 1:2007 Edition 2:2004 consolide par lamendement 1:2007 2 60450 IEC:2004+A1:2007 CONTENTS FOREWORD.3 INTRODUCTION.
17、5 1 Scope.6 2 Normative references .6 3 Terms, definitions and symbols 6 3.1 Terms and definitions 6 3.2 Symbols 7 4 Principle .8 5 Apparatus and reagents .8 6 Specimens .9 6.1 Preparation of specimens9 7 Experimental procedure10 7.1 Measurement of water content of paper.10 7.2 Determination of visc
18、osity .10 8 Test report16 Annex A (normative) Cuen solution17 Annex B (normative) Preparation of Cuen solution.18 Annex C (normative) Procedure for the verification of the ratio CuEnccof the Cuen solution21 Annex D (informative) Numerical values of the product .c as a function of saccording to Marti
19、ns formula 22 Bibliography23 Table 1 Symbols 7 Table 2 vDP values of specimen .10 Table D.1 .c as a function of s (k = 0,14).22 Figure 1 Chemical structure of cellulose 6 Figure 2 Ubbelohde viscometer tube14 60450 IEC:2004+A1:2007 3 INTERNATIONAL ELECTROTECHNICAL COMMISSION MEASUREMENT OF THE AVERAG
20、E VISCOMETRIC DEGREE OF POLYMERIZATION OF NEW AND AGED CELLULOSIC ELECTRICALLY INSULATING MATERIALS FOREWORD 1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising all national electrotechnical committees (IEC National Committees). The objec
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29、e 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 indispensable for the correct application of this publication. 9) Attention is drawn to the possibility that
30、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. International Standard IEC 60450 has been prepared by subcommittee 15E: Methods of test, of IEC technical committee 15: Insulating materi
31、als. This second edition cancels and replaces the first edition, published in 1974, and constitutes a technical revision. Experience has indicated the need for improved description of the ex-perimental method. It describes a revised procedure that overcomes the limitations of the first edition. This
32、 consolidated version of IEC 60450 consists of the second edition (2004) documents 15E/229/FDIS and 15E/235/RVD and its amendment 1 (2007) documents 112/49/CDV and 112/66/RVC. The technical content is therefore identical to the base edition and its amendment(s) and has been prepared for user conveni
33、ence. It bears the edition number 2.1. 4 60450 IEC:2004+A1:2007 A vertical line in the margin shows where the base publication has been modified by amendment 1. This publication has been drafted in accordance with the ISO/IEC Directives, Part 3. The committee has decided that the contents of the bas
34、e publication and its amendments will remain unchanged until the maintenance result date indicated 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 amende
35、d. 60450 IEC:2004+A1:2007 5 INTRODUCTION Experience has indicated the need for an improved description of the experimental method for the reproducible determination of the average viscometric degree of polymerization of new and aged cellulosic electrically insulating material. The major error appear
36、s to arise from oxidative degradation occurring during processing and effluxing. Other significant factors include the need to ensure that all of the material is dissolved and used, as well as the effect of the speed of effluxing. 6 60450 IEC:2004+A1:2007 MEASUREMENT OF THE AVERAGE VISCOMETRIC DEGRE
37、E OF POLYMERIZATION OF NEW AND AGED CELLULOSIC ELECTRICALLY INSULATING MATERIALS 1 Scope This International standard describes a standardized method for the determination of the average viscometric degree of polymerization (DP ) of new and aged cellulosic electrically insulating materials. It may be
38、 applied to all cellulosic insulating materials such as those used in transformer, cable or capacitor manufacturing. The methods described can also be used for the determination of the intrinsic viscosity of solutions of chemically modified kraft papers, provided that these dissolve completely in th
39、e selected solvent. Caution should be taken if the method is applied to loaded kraft papers. NOTE Within a sample of material, all the cellulose molecules do not have the same degree of polymerization so that the mean value measured by viscometric methods is not necessarily the same as that which ma
40、y be obtained by, for instance, osmotic or ultra centrifuging methods. 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 references, the latest edition of the referenced
41、document (including any amendments) applies. IEC 60814, Insulating liquids Oil-impregnated paper and pressboard Determination of water by automatic coulometric Karl Fischer titration ISO 287, Paper and board Determination of moisture content Oven-drying method ISO 3105, Glass capillary kinematic vis
42、cometers Specifications and operating instructions 3 Terms, definitions and symbols For the purposes of this document, the following terms, definitions and symbols apply. 3.1 Terms and definitions 3.1.1 degree of polymerization of a cellulose molecule number of anhydrous-glucose monomers, C6H10O5, i
43、n the cellulose molecule NOTE Figure 1 shows the chemical structure of cellulose. CH2OHOHOHOOHOHOOHOOOCH2OHCH2OHHOOHOHn 2IEC 424/04Figure 1 Chemical structure of cellulose 60450 IEC:2004+A1:2007 7 3.1.2 Cuen 1 mol/l aqueous solution of bis(ethylenediamine)copper(II) hydroxide Cu(H2NCH2CH2NH2)2(OH)2.
44、 CAS 14552-35-31NOTE In some countries the abbreviation CED is used for bis(ethylenediamine)copper(II) hydroxide. 3.1.3 paper cellulosic electrically insulating material, such as paper, presspaper, pressboard and components made thereof NOTE In the present document such paper is termed “paper”. 3.2
45、Symbols Symbols used in this standard are shown in Table 1. Table 1 Symbols Symbol Definition Mark Houwink constant of the cellulose monomer cCuMolarity of copper in Cuen solution cEnMolarity of ethylenediamine in Cuen solution C0, C1and C2Constants for viscometer tubes 0, 1 and 2 respectively c Con
46、centration of solution DP Average viscometric degree of polymerization Kinematic viscosity of solution v0Kinematic viscosity of solvent K Mark Houwink characteristic constant of the polymer/solvent system k Constant in Martins formula mDMass of dry paper mTMass of swollen paper in tared vessel mH2OM
47、ass of added water H2ODensity of water vH2OVolume of added water vCuVolume of added Cuen Intrinsic viscosity vsSpecific viscosity t1A, t1BEfflux time for tests A and B on dissolved specimen 1 t2A, t2BEfflux time for tests A and B on dissolved specimen 2 t0A, t0BEfflux time for tests A and B on pure
48、solvent t0Efflux time for diluted Cuen solvent (50 % Cuen and 50 % water) tSEfflux time for Cuen dissolved specimen 1Chemical Abstracts Service (CAS) Registry numbers 8 60450 IEC:2004+A1:2007 4 Principle The specific viscosity s of a solution of the paper in Cuen is determined. From this result the
49、intrinsic viscosity of the solution is deduced, and from this the degree of polymerization is calculated. NOTE Solutions of cellulose are non-Newtonian fluids. Their viscosity decreases as the flow velocity increases (sometimes known as “structural viscosity”). Although the viscosity of dilute solutions varies only slightly w
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