BS ISO 12013-2-2012 Paints and varnishes Determination of curing characteristics using a free damped oscillation method Glass transition temperature《涂料和清漆 采用自由阻尼振荡法测定固化特性 玻璃转换温度》.pdf

1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 12013-2:2012Paints and varnishes Determination of curingcharacteristics using a freedamped oscillation methodPart 2: Glass transition temperatureBS ISO 12013-2:2012 BRITIS

2、H STANDARDNational forewordThis British Standard is the UK implementation of ISO 12013-2:2012. The UK participation in its preparation was entrusted to T e c h n i c a l Committee STI/10, Test methods for paints.A list of organizations represented on this committee can be obtained on request to its

3、secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2012. Published by BSI Standards Limited 2012.ISBN 978 0 580 66518 9 ICS 87.040 Compliance with a British Standard c

4、annot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 November 2012.Amendments issued since publicationDate T e x t a f f e c t e dBS ISO 12013-2:2012 ISO 2012Paints and varnishes Determination of cur

5、ing characteristics using a free damped oscillation method Part 2: Glass transition temperaturePeintures et vernis Dtermination des caractristiques de polymrisation par une mthode utilisant un pendule amorti Partie 2: Temprature de transition vitreuseINTERNATIONAL STANDARDISO12013-2First edition2012

6、-10-15Reference numberISO 12013-2:2012(E)BS ISO 12013-2:2012ISO 12013-2:2012(E)ii ISO 2012 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2012All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mec

7、hanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.org

8、Published in SwitzerlandBS ISO 12013-2:2012ISO 12013-2:2012(E) ISO 2012 All rights reserved iiiContents PageForeword ivIntroduction v1 Scope 12 Normative references .13 Terms and definitions .14 Principle .25 Pendulum-damping apparatus 26 Sampling 67 Test panels 67.1 Substrate .67.2 Preparation and

9、coating 67.3 Thickness of coating 68 Procedure 69 Expression of results .710 Precision 710.1 General .710.2 Repeatability limit 810.3 Reproducibility limit.811 Test report .8Annex A (informative) Viscoelastic properties .9Bibliography .10BS ISO 12013-2:2012ISO 12013-2:2012(E)ForewordISO (the Interna

10、tional Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has be

11、en established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical stan

12、dardization.International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for

13、voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all s

14、uch patent rights.ISO 12013-2 was prepared by Technical Committee ISO/TC 35, Paints and varnishes, Subcommittee SC 9, General tests methods for paints and varnishes.ISO 12013 consists of the following parts, under the general title Paints and varnishes Determination of curing characteristics using a

15、 free damped oscillation method: Part 1: Start temperature of the curing reaction Part 2: Glass transition temperatureiv ISO 2012 All rights reservedBS ISO 12013-2:2012ISO 12013-2:2012(E)IntroductionWhen a rigid-body pendulum with a cylindrical edge is placed in contact with a cured coating, the fre

16、e damped oscillation is measured as, due to heating, the viscoelasticity of the paint film changes. The attenuation of the oscillating rigid pendulum on the coating depends on the viscoelasticity of the paint. When the viscoelasticity of the paint changes, the logarithmic damping ratio of the rigid-

17、body pendulum changes. Various paint film properties can be read from a plot of the logarithmic damping ratio versus temperature (see Annex A). ISO 2012 All rights reserved vBS ISO 12013-2:2012BS ISO 12013-2:2012Paints and varnishes Determination of curing characteristics using a free damped oscilla

18、tion method Part 2: Glass transition temperature1 ScopeThis part of ISO 12013 specifies a free damped oscillation method for determining the glass transition temperature of dried and cured films of paints and varnishes.2 Normative referencesThe following referenced documents are indispensable for th

19、e application 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.ISO 1513, Paints and varnishes Examination and preparation of test samplesISO 1514, Paints and varnishes Stan

20、dard panels for testingISO 2808, Paints and varnishes Determination of film thicknessISO 4618, Paints and varnishes Terms and definitionsISO 15528, Paints, varnishes and raw materials for paints and varnishes Sampling3 Terms and definitionsFor the purposes of this document, the terms and definitions

21、 given in ISO 4618 and the following apply.3.1glass transitionreversible change in an amorphous polymer or in amorphous regions of a partially crystalline polymer from (or to) a viscous or rubbery condition to (or from) a hard and relatively brittle oneISO 472:199913.2glass transition temperatureTga

22、pproximate midpoint of the temperature range over which the glass transition takes placeISO 472:19991NOTE 1 The rotational degrees of freedom of a polymer are excited at the glass transition temperature.NOTE 2 The glass transition temperature varies significantly, depending upon the adhesion to the

23、substrate of the cured coating film, as well as the test method and conditions selected to measure it.INTERNATIONAL STANDARD ISO 12013-2:2012(E) ISO 2012 All rights reserved 1BS ISO 12013-2:2012ISO 12013-2:2012(E)3.3glass transition temperature as determined by the pendulum methodTgpglass transition

24、 temperature of dried and cured paints and varnishes determined using a free damped oscillation methodNOTE The damping ratio is determined from the amplitude of oscillation of the pendulum and plotted against the temperature. The peak of the curve thus obtained is taken as the glass transition tempe

25、rature.3.4periodabsolute value of the time between two oscillations in the same direction of the free damped oscillation3.5logarithmic damping ratiologarithm of the ratio between consecutive amplitudes of a free damped oscillation4 PrincipleImmediately after a coating material is applied to a test p

26、anel, it is dried or cured as specified. The dried or cured test panel is fixed in the apparatus and a rigid-body pendulum with a cylindrical edge (see Figure 1) is lowered on to the film. The heating rate and the amplitude of the first pendulum oscillation are set. The pendulum is released and allo

27、wed to oscillate. As the temperature is raised, the amplitude of oscillation of the pendulum becomes progressively smaller. When the temperature becomes greater than Tg, the amplitude of oscillation becomes gradually larger again. The damping ratio is determined from measurements of the amplitude of

28、 oscillation of the pendulum and plotted against the temperature. The peak of the curve thus obtained is recorded as the glass transition temperature. When the network structure of the dried or cured coatings film on the substrate is heated, it begins to change. When network structure changes, visco

29、sity changes occur. The oscillation of the pendulum is damped by the change in viscosity. After all chemical bonds have been formed, the viscosity decreases due to a rise of the temperature. Therefore a peak is produced. The maximum height of this peak can be read off as Tgp.5 Pendulum-damping appar

30、atus5.1 General. Figure 1 shows an example of a pendulum-damping apparatus. In addition to the pendulum itself, the apparatus includes an electromagnet with which the required oscillation can be generated, a temperature-controlled test block, and a displacement sensor that detects each swing of the

31、pendulum. The amplitude and period of the swings of the pendulum, the time that elapses from the beginning of the first oscillation and the temperature of the sample are monitored by computer. The logarithmic damping ratio and the temperature of the test panel are recorded.2 ISO 2012 All rights rese

32、rvedBS ISO 12013-2:2012ISO 12013-2:2012(E)Key1 displacement sensor 5 dried or cured film on the test panel2 electromagnet 6 test panel3 temperature-controlled test block 7 cylindrical edge4 rigid-body pendulum with cylindrical edgeFigure 1 Pendulum-damping apparatus5.2 Temperature-controlled test bl

33、ock, shown in Figure 2. The dried or cured test panel is mounted on a mounting table (A), the temperature of which is regulated by means of an electric heating current passing through the block from B. ISO 2012 All rights reserved 3BS ISO 12013-2:2012ISO 12013-2:2012(E)Dimensions in millimetresKeyA

34、mounting table for test panel B connection for electric-power supplyFigure 2 Temperature-controlled test block5.3 Rigid-body pendulum, of which Figure 3 shows the dimensions. The pendulum is designed so that its oscillation is generated by an electromagnet. The period and amplitude of oscillation ar

35、e recorded automatically by a computer.4 ISO 2012 All rights reservedBS ISO 12013-2:2012ISO 12013-2:2012(E)Dimensions in millimetresKey1 cylindrical edge 2 displacement sensor 3 electromagnetFigure 3 Rigid-body pendulum, steel, mass 45 g5.4 Cylindrical edge, attached to the rigid-body pendulum and p

36、laced in contact with the dried or cured film of coating material on the test panel at the beginning of the test. The shape and dimensions of the cylindrical edge are shown in Figure 4.Dimensions in millimetresFigure 4 Cylindrical edge, brass, mass 4 g ISO 2012 All rights reserved 5BS ISO 12013-2:20

37、12ISO 12013-2:2012(E)6 SamplingTake a representative sample of the product to be tested (or of each product in the case of a multicoat system), as specified in ISO 15528.Examine and prepare each sample for testing, as specified in ISO 1513.7 Test panels7.1 SubstrateSelect the substrate from those sp

38、ecified in ISO 1514, ensuring that the panels are planar and rigid. Metal, glass or plastic panels are recommended, with dimensions of 25 mm 50 mm (0,3 mm to 1,0 mm).7.2 Preparation and coatingPrepare each test panel in accordance with ISO 1514, coat it with the product under test and dry or cure th

39、e coating as specified by the manufacturer. The test coating shall be smooth and free from surface irregularities.Key1 position of temperature sensor 3 dried or cured coating material2 position of cylindrical edge 4 test panel (substrate)Figure 5 Test arrangement of temperature sensor, dried or cure

40、d coating material and cylindrical edge7.3 Thickness of coatingAfter completion of the test, determine the dry-film thickness, in micrometres, of the coating, on a part of the test panel not affected by the test, by one of the procedures specified in ISO 2808.8 ProcedureCarry out the determination i

41、n duplicate.The starting temperature and the temperature increase are dependent not only on the type of coating material and the substrate used, but also on the test conditions. The test conditions should preferably be agreed between the interested parties. If the conditions have not been agreed, a)

42、 to d) are recommended.a) Carry out the determination at a temperature of (23 2) C and a relative humidity of (50 5) %.b) Set the temperature at which the measurements are to begin to approximately 30 C and the heating rate to 10 C/min.6 ISO 2012 All rights reservedBS ISO 12013-2:2012ISO 12013-2:201

43、2(E)c) Set the temperature at which the measurements are to finish to more than 30 C above the expected glass transition temperature.d) Measure the logarithmic damping ratio every 12 s. The oscillation of the rigid-body pendulum is performed at each reading interval. The time to draw a rigid-body pe

44、ndulum to a magnet is 1 s to 2 s.Place the test panel carrying the dried or cured coating material on the test block (5.2). Mount the temperature sensor on to the dried or cured coating (see Figure 5) and record the temperature.Place the cylindrical edge, mounted on the pendulum, in contact with the

45、 dried or cured coating on the test panel (see Figure 5). Start the apparatus.During the test, the temperature of the test panel and the logarithmic damping ratio is recorded. The logarithmic damping ratio is calculated from the oscillation amplitudes of a pendulum and plotted against the temperatur

46、e.9 Expression of resultsThe glass transition temperature determined by pendulum method, Tgp, of dried or cured paint on substrate is estimated as the logarithmic damping ratio, , for the temperature. An example of such a plot is given in Figure 6. Record the peak of the plot as the glass transition

47、 temperature. Calculate the mean of the values obtained in the two individual determinations and round this mean value to the nearest whole number.Keyt period of oscillation, in seconds O logarithmic damping ratio logarithmic damping ratio period of oscillationT temperature, in degrees celsiusFigure

48、 6 Example of a plot for determining the glass transition temperature Tgpof a dried or cured film of coating material on a substrate10 Precision10.1 GeneralPrecision data for this method have been obtained with a melaminepolyester resin. ISO 2012 All rights reserved 7BS ISO 12013-2:2012ISO 12013-2:2

49、012(E)10.2 Repeatability limitThe repeatability limit r is the value below which the absolute difference between two single test results, each the mean of duplicates, can be expected to lie with a 95 % probability when this method is used under repeatability conditions (i.e. test results obtained on identical material by one operator in one laboratory within a short interval of time using the standardized test method). For the particular melaminepolyester resin tested, r has be