60216-8 © IEC:2010 –3– 112/165/NP INTERNATIONAL ELECTROTECHNICAL COMMISSION ____________ ELECTRICAL INSULATING MATERIALS – THERMAL ENDURANCE PROPERTIES – Part 8: Instructions for calculating thermal endurance characteristics using simplified procedures FOREWORD 1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization 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 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 participate in this preparatory work. 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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 any 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 national or regional publication shall be clearly indicated in the latter. 5) IEC itself does not provide any attestation of conformity. Independent certification bodies provide conformity assessment services and, in some areas, access to IEC marks of conformity. IEC is not responsible for any services carried out by independent certification bodies. 6) All users should ensure that they have the latest edition 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 direct 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 indispensable 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. This International Standard has been developed by a Joint Working Group of IEC TC 112 and ISO TC 61 SC6. The text of this standard is based on the following documents: FDIS Report on voting XX/XX/FDIS XX/XX/RVD Full information on the voting for the approval of this standard 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. 60216-8 © IEC:2010 –4– 112/165/NP The committee has decided that the contents of this publication will remain unchanged until the stability date 1 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 amended. ————————— 1 The National Committees are requested to note that for this publication the stability date is 2018 60216-8 © IEC:2010 –5– 112/165/NP 1 Introduction 2 3 4 5 The term thermal endurance is used here to refer to tests made in air, excluding any other influence or stress applied to the test specimens. Thermal endurance properties evaluated in different environments and/or with different stresses applied to the test specimens require different test procedures. 6 7 8 In this International Standard, the study of the thermal ageing of materials is based solely on the change in certain properties resulting from a period of exposure to elevated temperature. The properties studied are always measured after the temperature has returned to ambient. 9 10 11 Properties of materials change at various rates on thermal ageing. To enable comparisons to be made of the thermal ageing of different materials, the criteria for judgment depend on the type of property to be studied and its acceptable limiting value. 12 13 14 In the application of this standard it is assumed that a practically linear relationship exists between the logarithm of the time required to cause the predetermined property change and the reciprocal of the corresponding absolute temperature (Arrhenius Law). 15 16 For the materials tested, no transition, in particular a first-order transition, should occur in the temperature range under study. 17 18 60216-8 © IEC:2010 –6– 112/165/NP CONTENTS 19 20 1 Scope ...............................................................................................................................7 21 2 Normative references .......................................................................................................7 22 3 Terms, definitions, symbols and abbreviated terms...........................................................8 4 3.1 Definitions ...............................................................................................................8 3.3 Symbols and abbreviated terms...............................................................................9 Testing procedure .......................................................................................................... 10 23 24 25 4.1 4.2 4.3 26 27 28 29 30 31 5 32 33 34 35 36 37 38 39 40 41 42 43 Outline description of procedures .......................................................................... 13 Simplified calculation procedures .......................................................................... 14 5.2.1 Times to end-point, thermal endurance graph ............................................ 14 5.2.2 Calculation of the regression line............................................................... 14 5.2.3 Calculation of deviation from linearity ........................................................ 15 5.2.4 Temperature index and halving interval ..................................................... 15 5.2.5 Validity of simplified calculations ............................................................... 16 5.3 Use of correlation coefficient ................................................................................. 16 5.4 Determination of RTI ............................................................................................. 16 5.5 Evaluation of results .............................................................................................. 17 5.6 Test report ............................................................................................................ 20 Bibliography.......................................................................................................................... 21 44 Annex A (informative) Example: simplified statistical analysis ............................................... 22 45 46 47 48 49 50 51 52 53 54 General ................................................................................................................. 10 Test specimens ..................................................................................................... 10 Preparation and number of test specimens ............................................................ 11 4.3.1 Preparation................................................................................................ 11 4.4 Exposure temperatures and times ......................................................................... 11 Simplified numerical and graphical evaluation procedures .............................................. 13 5.1 5.2 A.1 A.2 A.3 A.4 A.5 Simplified statistical analysis of TI data ................................................................. 22 A.1.1 Temperature index and halving interval ..................................................... 22 2 Comparation between linearity evaluation through s y and r .................................. 22 Effect of number of temperatures .......................................................................... 22 Conclusions .......................................................................................................... 22 Examples Test Reports ......................................................................................... 23 A.5.1 Example 1 ................................................................................................. 23 A.5.2 Example 2 ................................................................................................. 23 A.5.3 Example 3 ................................................................................................. 24 A.5.4 Dependence of cut-off value for correlation coefficient............................... 25 55 56 57 Figure 1 - Determination of the time to reach the end-point at each temperature Property variation (according to IEC 60216-1) ........................................................................... 18 58 59 Figure 2 - Thermal endurance graph - Temperature index - Halving interval (according to IEC 60216-1) ......................................................................................................................... 19 60 61 Figure 3 - Thermal endurance graph - Relative temperature index - Halving interval (according to IEC 60216-1)..................................................................................................... 20 62 63 64 Table 1 – Suggested exposure temperatures and times ........................................................ 13 60216-8 © IEC:201X –7– 112/165/NP ELECTRICAL INSULATING MATERIALS – THERMAL ENDURANCE PROPERTIES – 65 66 67 68 69 70 Part 8: Instructions for calculating thermal endurance characteristics using simplified procedures 71 1 Scope 72 73 This part of IEC 60216 specifies the general ageing conditions and simplified procedures to be used for deriving thermal endurance characteristics. 74 75 The procedures specify the principles for evaluating the thermal endurance properties of materials exposed to elevated temperature for long periods. 76 77 78 In the application of this standard, it is assumed that a practically linear relationship exists between the logarithm of the time required to cause the predetermined property change and the reciprocal of the corresponding absolute temperature (Arrhenius relationship). 79 80 For the valid application of the standard, no transition, in particular no first-order transition should occur in the temperature range under study. 81 82 Throughout the rest of this standard the term "insulating materials" is always taken to mean "insulating materials and simple combinations of such materials". 83 2 Normative references 84 85 86 87 88 89 90 The following normative documents contain provisions which, through reference in this text, constitute provisions of this part of IEC 60216. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this part of IEC 60216 are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of IEC and ISO maintain registers of currently valid International Standards. 91 IEC 60085: Electrical insulation - Thermal evaluation and designation 92 93 IEC 60216-1: Electrical insulating materials –Properties of thermal endurance – Part 1: Ageing procedures and evaluation of test results 94 95 IEC 60216-2: Guide for the determination of thermal endurance properties of electrical insulating materials – Part 2: Choice of test criteria 96 97 IEC 60216-3: Guide for the determination of thermal endurance properties of electrical insulating materials – Part 3: Instructions for calculating thermal endurance characteristics 98 99 IEC 60216-4-1: Guide for the determination of thermal endurance properties of electrical insulating materials – Part 4: Ageing ovens – Section 1: Single-chamber ovens 100 101 i) IEC 60216 - 5: Determination of Relative Thermal Endurance Index (RTE) of an Insulating Material 102 ISO 291:1997, Plastics – Standard atmospheres for conditioning and testing 60216-8 © IEC:201X –8– 112/165/NP 103 104 ISO 11346:1997, Rubber, vulcanized or thermoplastic – Estimation of life-time and maximum temperature of use from an Arrhenius plot 105 3 Terms, definitions, symbols and abbreviated terms 106 107 For the purposes of this document, the following terms, definitions, symbols and abbreviations apply. 108 3.1 Definitions 109 110 111 112 113 114 3.1.1 temperature index TI numerical value of the temperature in degrees Celsius derived from the thermal endurance relationship at a time of 20 000 h (or other specified time) [IEC 60050-212-12-11, modified] 115 116 117 118 119 120 3.1.2 halving interval HIC numerical value of the temperature interval in kelvins which expresses the halving of the time to end-point taken at the temperature equal to TI [IEC 60050-212-12-13, modified] 121 122 123 124 125 3.1.3 thermal endurance graph graph in which the logarithm of the time to reach a specified end-point in a thermal endurance test is plotted against the reciprocal thermodynamic test temperature [IEC 60050-212-12-10] 126 127 128 129 130 131 132 3.1.4 thermal endurance graph paper graph paper having a logarithmic time scale as the ordinate, graduated in powers of ten (from 10 h to 100 000 h is often a convenient range). Values of the abscissa are proportional to the reciprocal of the thermodynamic (absolute) temperature. The abscissa is usually graduated in a non-linear (Celsius) temperature scale oriented with temperature increasing from left to right. 133 134 135 3.1.5 degrees of freedom number of data values minus the number of parameter values 136 137 138 139 3.1.6 correlation coefficient number expressing the completeness of the relation between members of two data sets, equal to the covariance divided by the square root of the product of the variances of the sets 140 NOTE 141 142 143 3.1.7 end-point a point at which a definable event in a study takes place 144 145 146 3.1.8 time to end-point (failure time) time measure until a failure occurs. The value of its square is between 0 (no correlation) and 1 (complete correlation). 60216-8 © IEC:201X –9– 112/165/NP 147 148 149 150 3.1.9 square root of mean square deviation of points from regression line Sy mean deviation of data points from the regression line 151 152 153 154 155 3.1.10 square of the correlation coefficient 2 r represents the fraction of the variation in one variable that may be explained by the other variable. 156 157 158 159 3.1.11 destructive test diagnostic property test, where the test specimen is irreversibly changed by the property measurement, in a way which precludes a repeated measurement on the same specimen 160 161 162 163 164 3.1.12 non-destructive test diagnostic property test, where the properties of the test specimen are not permanently changed by the measurement, so that a further measurement on the same specimen may be made after appropriate treatment 165 166 167 168 169 3.2 proof test diagnostic property test, where each test specimen is, at the end of each ageing cycle, subjected to a specified stress, further ageing cycles being conducted until the specimen fails on testing 170 171 172 173 3.2.1 temperature group (of specimens) number of specimens being exposed together to the same temperature ageing in the same oven 174 175 NOTE Where there is no risk of ambiguity, either temperature groups or test groups may be referred to simply as groups. 176 177 178 179 3.2.2 test group (of specimens) number of specimens removed together from a temperature group (as above) for destructive testing 180 3.3 Symbols and abbreviated terms a,b Regression coefficients a,b,c,d Numbers of specimens for destructive tests n Number of y-values N Total number of test specimens r Correlation coefficient F Fisher distributed stochastic variable sy Square root of mean square deviation of points from regression line x Reciprocal thermodynamic temperature (1/Θ) y Logarithm of time to end-point ϑ Temperature, °C Θ Temperature, thermodynamic (Kelvins) Θ0 Value in Kelvins of 0 °C (273,15 K) 60216-8 © IEC:201X – 10 – τ Time (to end-point) χ2 χ 2 -distributed stochastic variable µ2 Central second moment of group of values TI Temperature Index TC Lower 95 % confidence limit of TI HIC Halving interval at temperature equal to TI RTI Relative temperature index 112/165/NP 181 4 Testing procedure 182 4.1 General 183 184 Simplified procedures, which do not test the data dispersion but only deviations from linear behaviour, are described. 185 186 187 It is possible, with some limitations, to evaluate the thermal endurance data graphically. In this case, statistical assessment of data dispersion is not possible, but it is considered important to evaluate any deviation of the data from the linear relationship. 188 189 190 Since the temperature is very often the dominant ageing factor affecting an electrical insulating material (EIM) certain basic thermal classes are useful and have been recognized as such internationally (see IEC 60085). 191 4.2 Test specimens 192 193 194 The accuracy of endurance test results depends largely on the number of specimens aged at each temperature. Generally, the following instructions, which influence the testing procedure, apply. 195 196 197 Where the test criterion for non-destructive or proof tests is based upon the initial value of the property, this should be determined from a group of specimens of at least twice the number of specimens in each temperature group. 198 199 The dimensions and method of preparation of the test specimens shall be in accordance with the specifications given for the relevant test method. 200 201 For a criterion requiring a destructive test, the minimum total number (N) of test specimens needed depends on 202 N=a×b×c+d 203 (1) where 204 205 a is the number of specimens in a test group undergoing identical treatment at one temperature and discarded after determination of the property (usually five); 206 b is the number of treatments, i.e. exposure lengths, at one temperature; 207 c is the number of exposure temperature levels; 208 209 210 211 212 d is the number of specimens in the group used to establish the initial value of the property. Normal practice is to select d = 2a when the diagnostic criterion is a percentage change of the property from its initial level. When the criterion is an absolute property level, d is usually given the value of zero, unless reporting of the initial value is required. 213 214 a) For a criterion requiring non-destructive testing, in most cases a group of five test specimens for each exposure temperature is adequate. 60216-8 © IEC:201X – 11 – 112/165/NP 215 216 b) For proof-test criteria, a group of at least 11 and possibly 21 specimens will be required for each exposure temperature. 217 218 c) For a criterion requiring a destructive test, the minimum total number (N) of test specimens needed is derived as follows: 219 220 221 222 223 224 NOTE 1 When there is a large number of specimens to be tested, it may be possible in certain cases to deviate from the relevant test specifications and to reduce this number. However, it must be recognized that the precision of the test result depends to a large extent on the number of specimens tested. In contrast, when the individual results are too scattered, an increase in the number of specimens may be necessary in order to obtain satisfactory precision. It is advisable to make an approximate assessment, by means of preliminary tests, of the number and duration of the ageing tests required. 225 4.3 Preparation and number of test specimens 226 4.3.1 227 228 The specimens used for the ageing test should constitute a random sample from the population investigated and are to be treated uniformly. 229 230 The material specifications or the test standards will contain all necessary instructions for the preparation of specimens. 231 232 233 234 235 The thickness of specimens is in some cases specified in the list of property measurements for the determination of thermal endurance (see IEC 60216-2); otherwise the thickness shall be reported. Some physical properties are sensitive even to minor variations of specimen thickness. In such cases, the thickness after each ageing period may need to be determined and reported if required in the relevant specification. 236 237 238 239 The thickness is also important because the rate of ageing may vary with thickness. Ageing data of materials with different thicknesses are not always comparable. Consequently, a material may be assigned more than one thermal endurance characteristic derived from the measurement of properties at different thicknesses. 240 241 242 243 The tolerances of specimen dimensions should be the same as those normally used for general testing; where specimen dimensions need smaller tolerances than those normally used, these special tolerances should be given. Screening measurements ensure that specimens are of uniform quality and typical of the material to be tested. 244 245 246 247 Since processing conditions may significantly affect the ageing characteristics of some materials, it shall be ensured that, for example, sampling, cutting sheet from the supply roll, cutting of anisotropic material in a given direction, moulding, curing, pre-conditioning, are performed in the same manner for all specimens. 248 4.4 Exposure temperatures and times 249 250 251 For TI determinations, test specimens should be exposed to not less than three, preferably at least four, temperatures covering a sufficient range to demonstrate a linear relationship between time to end-point and reciprocal thermodynamic (absolute) temperature. 252 253 254 To reduce the uncertainties in calculating the appropriate thermal endurance characteristic, the overall temperature range of thermal exposure needs to be carefully selected, observing the following requirements: 255 256 257 a) the lowest exposure temperature shall be one which will result in a mean or median time to end-point more than 1/4 the extrapolation time (which is generally 20000 hours) when determining TI. 258 259 NOTE 1 The mean time corresponding to TI is generally 20000 hours, thus the lowest exposure temperature shall correspond to a mean time >= 5000 hours; 260 b) the extrapolation necessary to establish TI shall not be more than 25 K; Preparation 60216-8 © IEC:201X – 12 – 112/165/NP 261 262 c) the highest exposure temperature shall be one which will result in a mean or median time to end-point of more than 100 h. 263 264 265 NOTE 2 For some materials, it may not be possible to achieve a time to end-point of less than 500 h while retaining satisfactory linearity. However, it is important that a smaller range of mean times to end-point will lead to a larger confidence interval of the result for the same data dispersion. 266 Table 1 gives guidance in making initial selections. 267 268 A number of recommendations and suggestions, temperatures, will be found in IEC 60216-1 Annex B. 269 270 271 When required, before the heat-ageing procedure is started, an initial test shall be made at room temperature with the required number of specimens conditioned and tested in accordance with the chosen test method. 272 273 274 Selection of adequate exposure temperatures requires previously determined information on the material under test. If such information is not available, exploratory tests may help in selecting exposure temperatures which are suitable for evaluating the thermal endurance characteristics. 275 276 For heat ageing, ovens shall be used that meet the requirements specified in IEC 60216-4, in particular with respect to the temperature tolerances and ventilation rates of air exchange. 277 278 279 280 281 282 283 It is good practice to keep an adequate number of test specimens separately as a reserve of the original material batch from which such specimens may subsequently be prepared. In this way, any required ageing of additional specimens in case of unforeseen complications will introduce a minimum risk of producing systematic differences between groups of specimens. Such complications may arise, for example, if the thermal endurance relationship turns out to be non-linear, or if specimens are lost due to thermal runaway of an oven. Moreover they can be used: useful in establishing times 284 - for cases in which the accuracy requires heat ageing at an additional temperature; 285 - as reference specimens. and 286 They shall be stored in an appropriately controlled atmosphere (see ISO 291). 287 288 289 Before the heat-ageing procedure is started, an initial test shall be made at room temperature with the required number of specimens conditioned and tested in accordance with the chosen test method. 290 291 Thermosetting materials shall be conditioned for 48 h at the lowest exposure temperature of the range selected. 292 293 NOTE 3 If necessary, thermoplastic materials should be annealed for 48 h at the lowest exposure temperature of the range selected. 294 295 Place the required number of specimens in each of the ovens maintained at the selected temperatures. 296 297 If there is a risk of cross-contamination between test specimens originating from different materials, use separate ovens for each material. 298 299 300 301 At the end of each heat-ageing period, the required number of test specimens is removed from the oven and conditioned, if necessary, under the appropriately controlled atmosphere (see ISO 291). The test, in accordance with the selected test criterion, shall be carried out at room temperature. 60216-8 © IEC:201X – 13 – 112/165/NP 302 303 NOTE 4 After the first week, during which the number of determinations of the characteristic under investigation can vary depending on the material under test, the test durations are generally selected in accordance with annex C. 304 305 Continue this procedure until the numerical value of the characteristic under investigation reaches the relevant threshold value. 306 Table 1 – Suggested exposure temperatures and times for TI corresponding to 20000 h Estimated value of TI in range °C 95-104 Exposure temperature °C Boxes: duration of exposure cycle in days 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 280 290 300 310 320 330 340 360 28 105-114 115-124 125-134 135-144 145-154 155-164 165-174 175-184 14 28 7 14 28 3 7 14 28 1 3 7 14 28 1 3 7 14 28 1 3 7 14 28 1 3 7 14 28 3 7 14 28 185-194 195-204 205-214 215-224 225-234 235-244 245-254 1 1 3 7 14 28 1 3 7 14 28 1 3 7 14 28 1 3 7 14 28 1 3 7 14 28 1 3 7 14 28 3 7 14 28 1 1 3 7 14 1 3 7 1 3 307 308 309 NOTE 2 This table is intended primarily for cyclic proof testing and non-destructive tests, but may also be used as a guide for selection of suitable time intervals for destructive tests. In this case, cycle times of 56 days, or even more, may be required. 310 311 312 NOTE 3 When extending the test programme by submitting additional specimens to ageing at temperatures below the lower of the originally planned ageing temperatures, a temperature interval of 10 K and cycle duration of 42 days for TI determination should be considered. 313 5 Simplified numerical and graphical evaluation procedures 314 5.1 315 316 317 At a chosen temperature, the variations in the numerical value of a chosen characteristic (for example, a mechanical, optical or electrical property: see IEC 60216-2) are determined as a function of time. 318 319 The procedure is continued until the specified end-point value of that characteristic has been reached, resulting in the time to end-point at that particular temperature. 320 321 322 323 Further specimens are exposed at a minimum of two other temperatures and the variations in the relevant characteristic determined. It is recommended that test specimens be heated-aged at three or four temperatures, and the time to end-point for each of the temperatures determined. Outline description of procedures 1 60216-8 © IEC:201X – 14 – 112/165/NP 324 325 326 When the data at all temperatures are complete, a thermal endurance graph is drawn, and a relatively simple statistical calculation made, to assess whether the linearity of the graph justifies the calculation of thermal endurance characteristics. 327 328 329 330 331 The test chosen shall relate to a characteristic which is likely to be of significance in practice and, wherever possible, use shall be made of test methods specified in international standards (see, for example, IEC 60216-2). If the dimensions and/or form of the test specimens are altered by the heat treatment, then only test methods which are independent of these effects may be used. 332 For the selection of the end-point, two factors shall be considered: 333 334 a) the period of time for which a temperature index shall be estimated. For general purposes, a period of 20 000 h is recommended; for special purposes, other times may be specified; 335 336 b) the acceptable change in value of the chosen characteristic. This value depends on the conditions of use foreseen. 337 5.2 Simplified calculation procedures 338 5.2.1 339 340 341 342 343 For destructive tests for each exposure temperature and for the group removed from the oven after each heat-ageing period, the mean value of the chosen property is plotted as a function of the logarithm of the time of ageing (see figure 1). The point at which this graph intersects the horizontal line representing the end-point criterion is taken as the time to end-point of the temperature group. 344 345 346 347 For non-destructive tests, the value of property measured on each specimen after each ageing period is plotted and the point at which this graph intersects the horizontal line representing the end-point criterion is taken as the time to end-point of the specimen. The time to end-point of the temperature group is the mean of the specimen times. 348 349 350 351 When applying a proof test, each ageing time shall be calculated as the mean of the times at the beginning and end of the ageing period. The ageing time of the temperature group shall be taken as the time of the ageing period in which the median failure on proof test takes place. 352 353 354 The mean times to end point are plotted versus the reciprocal values of the exposure temperatures. The intersection of this curve with the chosen time limit (in general 20 000 h) gives the temperature index sought. 355 5.2.2 356 357 358 The ageing function assumed for the purposes of this standard is the equation relating the absolute (Kelvin) temperature Θ to the time needed for a fixed change in the value of property, τ : 359 τ = Ae B/Θ Times to end-point, thermal endurance graph Calculation of the regression line 360 where 361 A and B are constants dependent on material and diagnostic test; 362 Θ is the absolute temperature, equal to ϑ + Θ 0 ; 363 ϑ is the temperature in degrees Celsius (°C); 364 Θ 0 = 273,15 K. 365 This may be expressed as a linear equation: (2) 60216-8 © IEC:201X – 15 – y = a + bx 366 367 (3) where 368 y = ln τ 369 x = 1/ Θ 370 a = ln A 371 b = B. 372 373 112/165/NP Given a group of paired x, y values, the values of a and b giving the best fit linear relationship are determined from the x, y values: b= 374 (∑ xy − ∑ x∑ y / k ) ⎡ x − ( x) / k ⎤ ∑ ⎢⎣∑ ⎥⎦ 2 a= 375 2 (∑ y − b∑ x ) k (4) (5) 376 where k is the number of x , y values. 377 378 379 NOTE 1 Since most "scientific" calculators with "statistics" functions have regression analysis facilities, the calculations implied by equations (2) to (4) above are executed by the calculator. It is important in this case that x is entered as the independent variable and y as the dependent. 380 381 NOTE 2 It is usually possible with such calculators to enter the time and temperature values and convert them to x and y before the summation is executed. 382 383 NOTE 3 used. 384 5.2.3 385 386 Calculate the coefficient of determination (square of correlation coefficient). Again, this can be done in the regression facility of the calculator. Logarithms to another base (for example, 10) may be used but will affect the value to be Calculation of deviation from linearity r 387 2 ( xy − ∑ x ∑ y / k ) 2 ∑ = 2 ⎡ x 2 − ( x )2 / k ⎤ ⎡ y 2 − ( ∑ ∑ y ) / k ⎤⎥⎦ ⎥⎦ ⎢⎣∑ ⎢⎣∑ (6) 388 389 390 If the value of r>0,985 then the values of TI and HIC may be determined. If this condition is not satisfied, then the deviations from the fundamental assumption are too great to allow the calculation. 391 392 Note This is not a Fisher linearity test, but an expression of the mean deviation of data from the regression line, as a fraction of the range of data values 393 5.2.4 394 Temperature index and halving interval ϑ= b (ln τ − a ) − Θ0 (7) 395 396 Using equation (7), calculate the temperatures corresponding to values of τ (time in hours) of 20 000, 10 000 and 2 000, designated ϑ 20 000 , ϑ 10 000 , and ϑ 2 000 respectively. 397 398 Using the data pairs ( ϑ 20 000 , 20 000) and ( ϑ 2 000 , 2 000) draw the regression line on thermal endurance paper to obtain the thermal endurance graph. 60216-8 © IEC:201X 399 – 16 – 112/165/NP Calculate the values of TI and HIC: 400 TI = ϑ 20 000 , HIC = ϑ 10 000 – ϑ 2 000 401 402 NOTE If a value τ , different from 20 000 is used for the calculation of TI, replace 10 000 and 2 000 in the above by τ /2 and τ /10. 403 5.2.5 404 405 406 407 408 409 The calculation procedure given above is only valid when the numbers of data contributing to the mean time to end-point for all temperature groups are approximately equal (if the value of s y is less than 0,30 and/or r>0). In addition, the procedure does not test the scatter of the test data for acceptability. For these reasons, the result cannot be given the status of full statistical acceptance, and the procedure should only be used when there is already satisfactory experience of the behaviour of the material in thermal endurance testing. 410 411 In all cases of doubt, the fuller analysis described in IEC 60216-3 should be carried out, especially if there is doubt about the acceptability of scatter of test data. 412 5.3 413 414 415 The reliability of the extrapolation of -the graph depends on obtaining an acceptable Arrhenius plot, which may not be possible with materials showing behaviour related to a transition phenomenon in the chosen temperature range. 416 417 418 For this purpose the correlation coefficient r is calculated in accordance with 5.2.3. If this calculation results in a value smaller than 0,985 (for three test temperatures; see also IEC 60216) an additional test at a different test temperature may improve the linearity of data. 419 420 421 422 423 Note It should be taken care of misinterpretation of the value of the correlation coefficient. A coefficient greater than 0,95 gives not automatically satisfactory calculations. The correlation coefficient cannot be used in this way. If the correlation coefficient is greater than 0,95, this indicates that the regression is responsible for a significant part of the variation of the result. It does not indicate that the deviations from regression linearity are small enough for the regression estimated to be valid. 424 5.4 425 426 For determination of RTI, the chosen reference material, its thermal endurance and the method of determination are of central importance. 427 428 429 430 431 The reference material shall be of the same type as the tested material, and have a history of satisfactory service. It shall have a known temperature index for the property and a threshold value which are the same, or at least reasonably similar to, those to be employed in the RTI test. The TI and HIC of the reference material should also be approximately the same as the values expected for the tested material. 432 433 434 435 Since processing conditions may significantly affect the ageing characteristics of some materials, the sampling, cutting of sheet from the supply roll, cutting of anisotropic material in the same direction, moulding, curing, preconditioning, etc. shall be performed in the same manner for both materials, and the specimens shall be tested in the same thickness. 436 437 438 439 The relative temperature index (RTI) is a thermal endurance characteristic which is derived from the two thermal endurance relationships or curves resulting from the comparative testing of the test material and the reference material. The RTI is specifically related to the time corresponding to the TI originally determined for the reference material. 440 441 442 The RTI consists of two numbers; one representing the temperature derived and the other the associated HIC. The derivation may be numerical or graphical (more details are given in IEC 60216-5). Validity of simplified calculations Use of correlation coefficient Determination of RTI 60216-8 © IEC:201X – 17 – 112/165/NP 443 444 445 446 The test chosen shall relate to a characteristic which is likely to be of significance in practice and, wherever possible, use shall be made of test methods specified in International Standards. If the dimensions and/or form of the test specimens are altered by the heat treatment, then only test methods which are independent of these effects may be used. 447 For the selection of the end-point, two factors shall be agreed upon: 448 449 a) the period of time for which a time-temperature limit shall be estimated; for general purposes, a period of 20 000 h is recommended; 450 NOTE 3 Other times (shorter or longer than 20 000 h) may be chosen if necessary. 451 452 b) the acceptable threshold value of the chosen characteristic; this threshold value depends on the conditions of use foreseen. 453 5.5 Evaluation of results 454 455 456 457 For both destructive and non-destructive tests, for each exposure temperature and for each heat ageing period, the value of the chosen property is plotted as a function of the logarithm of the time (see figure 1). The point at which this graph intersects the horizontal line representing the end-point criterion is taken as the time to failure. 458 When applying a proof test, the times to failure shall be calculated as the mean values. 459 460 461 The calculation of the thermal endurance curve is based on these times to failures and the respective exposure temperatures. If mean values are used, the logarithmic mean represents the time to failure. 462 Calculate a first-order regression line. 463 464 465 466 467 Plot the times to failure versus exposure temperatures on graph paper having a logarithmic time scale as the ordinate and an abscissa based on the reciprocal of the absolute temperature but showing the correlated values in degrees Celsius. The first order regression line is drawn through the points plotted on the graph, which thus represents the thermal endurance of the material under test. An example is given in figure 2. 468 469 Calculate the temperature index (TI) corresponding to the time limit chosen (generally 20 000 h) and the halving interval (HIC); calculate the correlation coefficient 60216-8 © IEC:201X – 18 – 112/165/NP Property value in relative units % 100 End-point criterion 50 Exposure temperatures 190 °C 171 °C 149 °C 130 °C 0 0 20 50 100 200 500 1 000 2 000 5 000 10 000 Ageing time h IEC 1197/01 470 471 472 Figure 1 - Determination of the time to reach the end-point at each temperature - Property variation (according to IEC 60216-1) 473 474 475 476 NOTE When the temperature scale is chosen in such a way that equal intervals correspond to equal intervals of reciprocal Kelvins, then the various points obtained will be found to lie on a straight line if a linear dependence exists. When the temperature range used is comparatively small, a curve can be prepared using an abscissa scale proportional to the temperature; in this case the curve can be fit to a straight line only with great circumspection. 477 TI r original TI of the reference material; 478 to time corresponding to TIC; 479 480 A point on the test material's thermal endurance relationship or graph from the comparative test, having coordinates 9A,to; 481 482 B point on the reference material's thermal endurance relationship or graph, having coordinates 9B,to; 483 484 HICr HIC for the reference material at point TIC of its original thermal endurance relationship or graph; 485 HIC(A) HIC for the test material at point A; HIC(B) HIC for the reference material at point B. 60216-8 © IEC:201X – 19 – 112/165/NP 100 000 Time h 10 000 1 000 100 TI 10 HIC 120 160 140 180 Temperature °C 2,6 2,5 2,4 2,3 Reciprocal thermodynamic temperature K –3 2,2 × 10 –1 Temperature estimate, 20 000 h Temperature estimate, 10 000 h IEC 1200/01 486 487 488 Figure 2 - Thermal endurance graph - Temperature index - Halving interval (according to IEC 60216-1) 489 490 The points A and B may be determined either graphically or numerically, and the RTI then determined using equation (8): 491 RTI =TI t+9A-9B . (8) 492 493 494 When reporting the RTI, the usual information regarding the property, end-point and test specimen data should be supplemented with corresponding information regarding the reference material. 495 496 When required, the test material may be assigned to an insulation thermal class according IEC 60085. 60216-8 © IEC:201X – 20 – 112/165/NP 100 000 B A Reference material, TI = TIr RTI = Ti r + 1A – 1B 10 000 Time h Test material 1 000 Reference material 100 1A 1B 10 120 160 140 180 Temperature °C 2,6 2,5 2,4 Reciprocal thermodynamic temperature K 2,3 –3 2,2 × 10 –1 IEC 1201/01 497 498 499 Figure 3 - Thermal endurance graph - Relative temperature index - Halving interval (according to IEC 60216-1) 500 5.6 Test report 501 Make the test report, reporting in the format TI s = xxx , HIC s = yy , y 502 503 The test report shall include 504 505 all information necessary for complete identification of the material tested; description of the tested material including dimensions and any conditioning of the specimens; 506 507 the property investigated, the chosen end-point, and, if this is a percentage value, the initial value of the property; 508 509 the test method used for determination of the property (for example, by reference to an IEC publication); 510 511 512 any relevant information on the test procedure, for example, ageing environment; details of the ageing conditions, if these are other than the exposure of unstressed specimens to hot air 60216-8 © IEC:201X – 21 – 112/165/NP 513 514 shape, dimensions and method of preparation of the test specimens, with reference to the relevant standard; 515 conditioning; 516 type of oven, with details of rate and direction of airflow; 517 times and temperatures of exposure in ovens; 518 the individual test temperatures, with the appropriate data: 519 520 o for non-destructive tests, the individual times to end-point, with the graphs of variation of property with ageing time 521 522 o for proof tests, the numbers and durations of the ageing cycles, with the numbers of specimens reaching end-point during the cycles 523 524 o for destructive tests, the ageing times and individual property values, with the graphs of variation of property with ageing time; 525 the thermal endurance graph; 526 reference to this International Standard; 527 Bibliography 528 529 IEC 60050(212): International Electrotechnical Vocabulary (IEV) – Chapter 212: Insulating solids, liquids and gases 530 531 IEC 60212: Standard conditions for use prior to and during the testing of solid electrical insulating materials 532 533 IEC 60493-1, Guide for the statistical analysis of ageing test data – Part 1: Methods based on mean values of normally distributed test results 534 535 ISO 2578:1993, Plastics – Determination of time-temperature limits after prolonged exposure to heat 536 60216-8 © IEC:201X – 22 – 112/165/NP Annex A (informative) Example: simplified statistical analysis 537 538 539 A.1 Simplified statistical analysis of TI data 540 Extract from “Simplified calculation procedures” in IEC 60216-1: ⎡ ⎢ µ2 y = ⎣ () ∑ y 2 − ( ∑ y ) 2 / k ⎤⎥⎦ 541 “ 542 Calculate the mean deviation of data points from the regression line: sy = 543 (10) k () ⎛⎜ 1 − r 2 ⎞⎟ µ y ⎝ ⎠ 2 k −2 ( ) (11) 544 A.1.1 Temperature index and halving interval 545 546 547 If the value of s y obtained from equation (11) is less than 0,16 (or 0,0695 if using logarithms to base 10) then the values of TI and HIC may be determined. If this condition is not satisfied, then the deviations from the fundamental assumption are too great to allow the calculation.” 548 A.2 549 550 551 552 Each of the following 3 pages details the calculation on a set of data for TI. The times and two of the three temperatures in each case are the same. The third temperature is given three different (related) values, leading to variation of the correlation coefficient, and consequently of the value of s y . 553 The descriptive table of this analysis is: Comparation between linearity evaluation through s y and r 2 Linearity property of group Correlation coefficient Value of s y Satisfactory linearity 0,999118177223061 0,0825382511051849 Compensatable non-linearity 0,991834310219611 0,250708128634552 Excessive non-linearity 0,981145251025673 0,37993902904637 554 555 556 557 In each page report in A.5, paragraph a) gives the 60216-3 report on the full analysis of the data file. Paragraph b) gives the report calculated as in 60216-1 (simplified). Paragraph c) lists the values in the original data file, with the mean values for the log times, and paragraph d) shows the graphic output from 60216-3 analysis, including data points for individual times. 558 A.3 559 560 The tables in clause A.5.4 show the dependence of cut-off value for correlation coefficient on the number of temperatures and the relative independence of the cut-off value for s y . 561 A.4 562 563 – A value of 0.95 is much too low to be used realistically (0.995 would be more appropriate for 3-temperature data). 564 – The value of 0.16 proposed for the cut-off point in B.1.1 above is realistic. Effect of number of temperatures Conclusions 60216-8 © IEC:201X – 23 – 565 A.5 566 A.5.1 567 a) IEC 60216-3 report on full analysis 568 TI (HIC): 169,7 (10,0) 569 F = 0,56606 (1/12: F95 = 4,747) p = 0,4663 570 Examples Test Reports Example 1 Linear 572 Correlation coefficient Sy = 0,0825382511051849 0.999118177223061 c) Data file for 60216-3 analysis Table A.1 Data set for example 1 574 Temperature 575 TC = 166,3 b) IEC 60216-1 (simplified) calculations 571 573 Original Time Values Log mean time 185 7410 6610 6170 5500 8910 8,82836233194414 200 3200 2620 2460 2540 3500 7,95003798439189 220 1100 740 720 620 910 6,68642618690896 d) 60216-3 analysis graph 576 577 Figure A.1 Analysis Graph for Example 1 578 A.5.2 579 a) IEC 60216-3 report on full analysis 580 TI (HIC) : 163,4 (11.4) 581 F = 5,2227 (1/12: F95 = 4,747) p = 0,0413 582 112/165/NP Example 2 TC = 158,7 b) IEC 60216-1 (simplified) calculations 60216-8 © IEC:201X – 24 – 112/165/NP 583 Minor non-linearity, compensated Sy = 0,250708128634552 584 Correlation coefficient 585 0.991834310219611 c) Data file for 60216-3 analysis# Table A.2 Data set for example 2 586 Temperature 587 Original Time Values Log Mean Time 180 7410 6610 6170 5500 8910 8,82836233194414 200 3200 2620 2460 2540 3500 7,95003798439189 220 1100 740 720 620 910 6,68642618690896 d) 60216-3 analysis graph 588 589 Figure A.2 Analysis Graph for Example 2 590 591 A.5.3 Example 3 592 a) IEC 60216-3 report on full analysis 593 TI (HIC) cannot be reported: 594 TI = 155,8, HIC = 12.8, 595 F = 11,995 (1/12: F95 = 4,747) p = 4,6884e-3 596 b) IEC 60216-1 (simplified) calculations 597 Excessive non-linearity 598 Correlation coefficient 599 TC = 148,.2 c) Data file for 60216-3 analysis Sy = 0,37993902904637 0,981145251025673 60216-8 © IEC:201X – 25 – Table A.3 Data set for example 3 600 Temperature 601 Original Time Values 605 606 7410 6610 6170 5500 8910 8,82836233194414 200 3200 2620 2460 2540 3500 7,95003798439189 220 1100 740 720 620 910 6,68642618690896 d) 60216-3 analysis graph Figure A.2 Analysis Graph for Example 2 A.5.4 Dependence of cut-off value for correlation coefficient Table A.4 Dependence of cut-off value for correlation coefficient on the number of temperatures θ1 175 180 185 θ2 200 200 200 θ3 220 220 220 r0 0,981145251025673 0,991834310219752 0,999118177223061 sy 0,37993902904637 0,250708128634552 0,0825382511051849 Rejected in 60216-3 Accepted after adjustment Acceptable linearity Table A.5 Relative independence of the cut-off value for s y . 607 608 609 610 Log Mean Time 175 602 603 604 112/165/NP θ1 175 180 185 θ2 200 200 200 θ3 220 220 220 θ4 240 240 240 r0 0,990128557470239 0,993223870062064 0,992078909781926 sy 0,236370223011478 0,195988591044968 0,211839838691374 Rejected in 60216-3 Accepted after adjustment Accepted after adjustment