1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 12013-1:2012Paints and varnishes Determination of curing characteristics using a free damped oscillation methodPart 1: Start temperature of the curing reactionBS ISO 12013
2、-1:2012 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 12013-1:2012. 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 r
3、equest to its 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 66517 2 ICS 87.040 Compliance with a Brit
4、ish Standard cannot 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 12013-1:2012 ISO 2012Paints and varnishes Determ
5、ination of curing characteristics using a free damped oscillation method Part 1: Start temperature of the curing reactionPeintures et vernis Dtermination des caractristiques de polymrisation par une mthode utilisant un pendule amorti Partie 1: Temprature de dbut de raction de polymrisationINTERNATIO
6、NAL STANDARDISO12013-1First edition2012-10-15Reference numberISO 12013-1:2012(E)BS ISO 12013-1:2012ISO 12013-1:2012(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
7、form or by any means, electronic or mechanical, 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 4
8、7E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 12013-1:2012ISO 12013-1:2012(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 pa
9、nels 67.1 Substrate . 67.2 Preparation and coating 67.3 Thickness of coating 78 Procedure 79 Expression of results . 810 Precision 810.1 General . 810.2 Repeatability limit 810.3 Reproducibility limit . 811 Test report . 8Annex A (informative) Selection of pendulum and knife edge . 9Bibliography .10
10、BS ISO 12013-1:2012ISO 12013-1:2012(E)ForewordISO (the International 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
11、interested in a subject for which a technical committee has been 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 Electrotech
12、nical Commission (IEC) on all matters of electrotechnical standardization.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
13、 technical committees are circulated to the member bodies for 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.
14、ISO shall not be held responsible for identifying any or all such patent rights.ISO 12013-1 was prepared by Technical Committee ISO/TC 35, Paints and varnishes, Subcommittee SC 9, General test methods for paints and varnishes.ISO 12013 consists of the following parts, under the general title Paints
15、and varnishes Determination of curing characteristics using a free damped oscillation method: Part 1: Start temperature of the curing reaction Part 2: Glass transition temperatureiv ISO 2012 All rights reservedBS ISO 12013-1:2012ISO 12013-1:2012(E)IntroductionA freshly applied coating dries and/or c
16、ures depending on its physical and chemical characteristics. There are “wet characteristics” of various substrates and the evaporation of the solvent in the drying/or curing process. The structure of the coating changes according to the drying or curing process of the coating. The start temperature
17、of reaction is very important. It is essential to consider the evaporation of the solvent in the measurement of the start temperature of reaction.a) While a solvent evaporates, the curing of the coating begins. The evaporation of the solvent depends on:1) the evaporation behaviour of the solvents;2)
18、 the behaviour of the solvents in the coating film during each drying stage. This is affected by the boiling point.b) The evaporation characteristic of the solvents depends on the solubility and the thermal conductivity of the substrate. ISO 2012 All rights reserved vBS ISO 12013-1:2012BS ISO 12013-
19、1:2012Paints and varnishes Determination of curing characteristics using a free damped oscillation method Part 1: Start temperature of the curing reaction1 ScopeThis part of ISO 12013 specifies a free damped oscillation method for determining the start temperature of the curing reaction of coatings.
20、2 Normative referencesThe 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 document (including any amendments) applies.ISO 1513, Paints and varnish
21、es Examination and preparation of test samplesISO 1514, Paints and varnishes Standard 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
22、Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 4618 and the following apply.3.1periodabsolute value of the time between two oscillations in the same direction of the free damping oscillation3.2logarithmic damping ratioLlogarithm of the ratio between co
23、nsecutive amplitudes of a free damped oscillation3.3crosslinking temperatureTcltemperature at which the logarithmic damping ratio starts to increase rapidly and the period of oscillation starts to decrease rapidlyNOTE Figure 1 shows a study diagram from which the crosslinking temperature can be dedu
24、ced (labelled 1).3.4start temperature of reactiontemperature at which the logarithmic damping ratio begins to increaseNOTE The start temperature of reaction is shown in Figure 1(labelled 2).INTERNATIONAL STANDARD ISO 12013-1:2012(E) ISO 2012 All rights reserved 1BS ISO 12013-1:2012ISO 12013-1:2012(E
25、)Keyt period of oscillation 1 crosslinking temperature and network formationL logarithmic damping ratio 2 start temperature of reactionT temperature O period of oscillation logarithmic damping ratioFigure 1 Temperature dependence of the logarithmic damping ratio4 PrincipleA coating is applied to a t
26、est panel. The coated panel is fixed in the apparatus and a rigid-body pendulum with a knife edge is lowered on to the coating. The heating rate and the amplitude of the first pendulum oscillation are set. The pendulum is released and allowed to oscillate. As the coating starts to dry or cure, the l
27、ogarithmic damping ratio increases and the amplitude of oscillation of the pendulum becomes progressively smaller. The damping ratio is determined from measurements of the amplitude of the oscillation of the pendulum and plotted against the temperature. The point at which the logarithmic damping rat
28、io begins to increase rapidly is recorded as the start temperature of reaction.5 Pendulum-damping apparatus5.1 General. Figure 2 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 ge
29、nerated, a temperature-controlled test block, and a displacement sensor that detects each swing of the pendulum. The swings of the pendulum, the time that elapses from the beginning of the first oscillation and the temperature of the coating are monitored electronically.5.2 Temperature-controlled te
30、st block, shown in Figure 3. The coated 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.2 ISO 2012 All rights reservedBS ISO 12013-1:2012ISO 12013-1:2012(E)Key1 displacement sensor 5 coating
31、2 electromagnet 6 test panel3 temperature-controlled test block 7 knife edge4 rigid-body pendulumFigure 2 Pendulum-damping apparatus ISO 2012 All rights reserved 3BS ISO 12013-1:2012ISO 12013-1:2012(E)Dimensions in millimetresKeyA mounting table for test panel B connection for electric-power supplyF
32、igure 3 Temperature-controlled test block5.3 Rigid-body pendulum, of which Figure 4 shows the dimensions of two different types. These pendulums are designed so that their oscillation is generated by an electromagnet. The period and amplitude of oscillation are recorded automatically by a computer.N
33、OTE Guidance on the selection of the pendulum is given in Annex A.5.4 Knife edge, attached to the pendulum and placed in contact with the coated test panel at the beginning of the test. The shape and dimensions of the knife edge are shown in Figure 5.NOTE Guidance on the selection of the knife edge
34、is given in Annex A.4 ISO 2012 All rights reservedBS ISO 12013-1:2012ISO 12013-1:2012(E)Dimensions in millimetresa) Type 1, steel, mass 51 g b) Type 2, steel, mass 45 gKey1 knife edge 2 displacement sensor 3 electromagnetFigure 4 Rigid-body pendulum ISO 2012 All rights reserved 5BS ISO 12013-1:2012I
35、SO 12013-1:2012(E)Dimensions in millimetresKeyA knife edge A, material steel, mass 6 g, see Annex AB knife edge B, material steel, mass 6 g, see Annex AFigure 5 Dimension of knife edge6 SamplingTake a representative sample of the product to be tested (or of each product in the case of a multicoat sy
36、stem), 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 specified in ISO 1514, ensuring that the panels are planar and rigid. Metal, glass or plastic panels are recommended, with dimensions of 25
37、mm 50 mm (0,3 mm to 1,0 mm).7.2 Preparation and coatingPrepare each test panel in accordance with ISO 1514 and then coat it with the product under test by using the draw-down method. The direction of application shall be as indicated by the arrow in Figure 6. The test coating shall be smooth and fre
38、e from surface irregularities.6 ISO 2012 All rights reservedBS ISO 12013-1:2012ISO 12013-1:2012(E)Key1 position of temperature sensor 4 direction of application of coating2 position of knife edge 5 test panel (substrate)3 coatingFigure 6 Test arrangement of temperature sensor, coating, and knife-edg
39、e7.3 Thickness of coatingAfter completion of the test, determine the thickness, in micrometres, of the dry 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 in duplicate.The starting temperature and th
40、e temperature increase are dependent not only on the type of coating 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) to d) are recommended.a) Carry out the determinatio
41、n 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 preferably 30 C and the heating rate to 10 C/min.c) Set the temperature at which the measurements are to finish to more than 20 C above the expected start temperature o
42、f the reaction.d) Measure the logarithmic damping ratio L every 12 s. The oscillation of the rigid-body pendulum is performed at each reading interval. The time to draw a rigid-body pendulum to a magnet is 1 s to 2 s.Immediately after the product under test has been applied to the test panel, place
43、the coated test panel on the test block (5.2). Mount the temperature sensor on the upper surface of the test panel (see Figure 6) and record the temperature.Place the knife edge, mounted on the pendulum, in contact with the coating on the test panel (see Figure 6). Start the apparatus.During the tes
44、t, the temperature of the test panel and the period of oscillation of the pendulum are recorded. The logarithmic damping ratio L is calculated from the amplitude of oscillation of the pendulum and plotted against the temperature. ISO 2012 All rights reserved 7BS ISO 12013-1:2012ISO 12013-1:2012(E)9
45、Expression of resultsThe starting temperature of reaction is taken to be the temperature, in degrees Celsius, at which the logarithmic damping ratio start to increase rapidly (see Figure 1). Calculate the mean of the values obtained in the two individual determinations and round this mean value to t
46、he nearest whole number.10 Precision10.1 GeneralPrecision data for this method have been obtained with a melaminepolyester resin.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 exp
47、ected 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 h
48、as been found to be 4 C.10.3 Reproducibility limitThe reproducibility 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 test method is used under reproducibility conditions (
49、i.e. test results obtained on identical material by operators in different laboratories using the standardized test method). For the particular melaminepolyester resin tested, R has been found to be 20 C.11 Test reportThe test report shall contain at least the following information:a) all details necessary for complete identification of the product tested (manufacturer, trade name, batch number, etc.);b) a reference to this part of ISO 12013 (ISO 12013-1:2012);c) details of the coated
