1S 1528 ( Part 16): 1991 aredta aTTe sera arafaat F aT aa st ate afew water tafaat AUT 16 wea ATT TATA Taha H aegare wea site ate Goma Feral BT 1 250° Bo Ae AT ATH AT HAT Indian Standard METHODS OF SAMPLING AND PHYSICAL TESTS FOR REFRACTORY MATERIALS PART 16 DETERMINATION OF THERMAL CONDUCTIVITY UP TO 1250°C OF DENSE AND INSULATING REFRACTORY PRODUCTS ACCORDING TO THE HOT WIRE PARALLEL METHOD UDC 66°76 : 536°21 © BIS 1991 BUREAU OF INDIAN STANDARDS MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG ‘NEW DELHI 110002 March 1991 Price Group 5Refractories Sectional Committee, MTD 15 FOREWORD This Indian Standard ( Part 16) was adopted by the Bureau of Indian Standards, after the draft finalized by the Reftactories Sectional Committee had been approved by the Metallurgical Engincer- ing Division Council. ‘Methods of sampling and physical tests for refractory materials were originally covered in IS 485 : 1953, ‘Methods for sampling and testing of refractory materials ( temarive )’. This Indian Standard on methods of sampling and physical testing of refractory materials was first published in 1962. As a result of experience gained during these years, certain modifications have been made in the Methods ‘of sampling, Methods of physical tests and the Methods for the determination of warpage in refractory materials. ‘The Sectional Committee while issuing this revision felt it desirable to issue the standard in separate parts. Other parts of this standard, published so far, cover the following: Part 1 Determination of pyrometric cone equivalent (PCE) or softening point ( second revision ) Part 2 Determination of refractoriness under load ( first revision ) Part 3 Determination of spalling resistance ( second revision ) Part 4 Determination of cold crushing strength ( first revision ) Part $ Determination of modulus of rupture (Jirst revision ) Part 6 Determination of permanent change after reheating (first revision ) Part 7 Methods of sampling and criteria of conformity ( first revision ) Part 8 Determination of apparent porosity {first revision ) Part 9 Determination of true specific gravity and true density ( second revision ) Part 10 Determination of size of refractory bricks (first revision ) Part 11 Determination of warpage (first revision ) Part 12. Determination of bulk density (first revision ) Fart 13. Determisation of resistance to the disintegration effect of carbon monoxide (frst revision Part 14 Determination of sieve analysis (first revision ) Part 15 Method for determination of bulk density, apparent porosity and true porosity of dense shaped refractory products. In the formulation of this standard assistance has been taken from: a) ISO DIS 8894-2 Refractory materials — Determination of thermal conductivi Parallel hot wire method. International Organization for Standardization. b) Method developed by Central Glass and Ceramic Research Institute. Part 2IS 1528 ( Part 16) : 1991 Indian Standard METHODS OF SAMPLING AND PHYSICAL TESTS FOR REFRACTORY MATERIALS PART 16 DETERMINATION OF THERMAL CONDUCTIVITY UP TO 1 250°C OF DENSE AND INSULATING REFRACTORY PRODUCTS ACCORDING TO THE HOT WIRE PARALLEL METHOD 1 SCOPE, 1.1 This standard prescribes the method of deter- mination of the thermal conductivity of non- clectrical conducting refractory materials up to 1 250°C by hot wire parallel method. 1.2 The test method js suitable for homogeneous insulating and dense test pieces ( test pieces can bo obtained as bricks or parts of bricks or can be prepared. from moaolithic materials ). The test method is also suitable for unshaped refractory materials such as powders and granular materials and chemically bonded unfired bricks. 1.3 The test_method is applicable to refractory material with a thermal conductivity up to 25 Wan? K=}, 2 REFERENCES: 2.1 The Indian Standards given below are neces- sary adjuncts to this standar IS No. 1528 (Pact 7): 1974 Title Methods of sampling and physical tests for retractory materials : Part 7 Methods of sampling "and criteria for conformity ( first revision ) Direct recording electrical ‘measuring instruments 3 TERMINOLOGY 3.0 For the ‘purpose of this standard, following definition shall apply. 31 Thermal Conductivity ( Coefficient of Thermal Conductivity ) — It is the property of the refrac- tory material and is defined as the rate of heat flow through unit area of the material at unit temperature gradient and is expressed by: Thema condusviy = 24 wm 6236 : 1971 where = quantity of heat flow in time ‘t” 4 = area of the material measured normal to the direction of heat flow, and dy Gem Rate of change of temperature with distance in the disection of heat flow. 3.4.1 The thermal conductivity of a refractory material should be expressed in watts per metre per kelvin (17 )m.K ). 4 PRINCIPLE 4.1 The hot wire parallel method isa dynamic ‘measuring procedure based on the measurement of the temperature increase at a certain location at some distance from a linear heat source embedded in between two test pieces. 4.2 The heat source is a wire at a certain distance from which a thermocouple is fitted; the thermo- couple fads runing paral to the heating wire see Fig. 1), 43 The increase of temperature of the measure- ‘ment thermocouple as a function of time, measured from the moment the power is switched on, is a measure of the thermal conductivity of the test pieces. 44 Unidirectional testing is not possible; the coefficient of thermal conductivity being the mean value of two directions. This makes measurements of an isotropic materials inaccurate where a varia- tion in different directions is expected. 5 GENERAL 5.1 Figure 2 illustrates the testing arrangement. 5.2 Measuring Arrangement — Method I S.2.1 Method I—The measuring arrangement consists of hot wire ( or heater ) and a differential thermocouple, The latter is formed from a ‘measurement couple and a reference couple connected in opposition. The leads of the ‘measurement thermocouple should run parallel to the hot wire at a distance of 15 + 1mm. The diameter of this thermocouple should be the same as that of the hot wire which should not exceed 0°35 mm (see Fig. 1 and Fig. 2).18 1528 ( Part 16 REFERENCE THERMOCOUPLE, OPTIONAL INSULATING {LAYER (6mm) MEASUREMENT MEASURING: CIRCUIT, THERMOCOUPLE aI. L_ vowtace TAPS HEATING CIRCUIT Fig. 1 DIAGRAM oF THE LOCATION OF HEATING CIRCUIT AND. MEASURING: (DirreRENtiat THoxmocource Cixcurt ), Metaop I REFERENCE evening cover SCE ae [—]REcistration DEVICE MEASURERMENT t trembcoun 151mm U Got ene 4 py AMPEREMETER -YOLTMETER ‘ac of de POWER SOURCE Fic, 2. DiaGRaM oF THE MEASURING ARRANGEMENT5.2.1.1 The output of the reference thermocouple should be kept stable by placing it between the top outer face of the upper test piece and a cover of the same material as the test pieces. An insulat- ing layer between cover, including reference thermocouple, and the upper test piece is option- ally allowed in case of at least one. x-value in the ‘temperature range higher than 15 W/m.X. 5.3 Measuring Arrangement — Method IT $.3.1 The measuring. arrangement consists of a hot wire ( or heater ) and a differential resistance (see Fig. 3). The latter is formed from a measurement platinum resistance and reference. ‘The leads of the measurement platinum resistance are placed parallel to the hot wire at a distance of 15 + 1 mm. The diameter of the sensor should be of 0'085 mm (approx ) for uniform contact REFERENCE SAMPLE COVER BRICK COVER BRICK TO BRIDGE y circurT 151528 ( Part 16): 1991 with the sample. The diameter of the hot wire should not exceed 0°35 mm. The reference wire (platinum should be kept stable by placing it between two bricks of the same material as. the test pieces ). §.3.2, The sample is placed in the furnace as shown, in Fig. 4, One test piece (brick size) one covered brick, and a half brick cut in length-wise on which the reference platinum wire is placed and it is covered by the rest half. A certain air gap is left in between the test piece and the refe- rence sensor. 5.4 Measuring Circuit: ‘The hot wire is. about 200 mm long and is sym- metrically embedded in between the test pieces (se Fig. 5). 70 VARIABLE. RESISTANCE 1 REFERENCE HAL BRICK SAMPLE ‘BRICK (Lengthwise Holt) Figy 3. DIAGRAM OF THE LOCATION OF HEATING CiRCUTT.AND MEASURING CIRCUIT (Beatin Resistance ), Metuop IIS 1528 ( Part 16): 1991 Fic. 4 Test ARRANGEMENT INSIDE THE FURNACE, MetHop IL 5.4.1 The hot wire is expediently made of a Pt Rh alloy (10 %Rh ) corresponding to the positive leg, of the Pt Ri-Pt thermocouple. Also other stan- dardized thermocouples may be used. When such thermocouples are used, provisions of 8 shall be adapted. 5.4.2 The hot wire shall preferably be heated by ac current supplied by a stabilized power source so that while starting to switch over the power source from an equivalent resistance of the same order of magnitude to the hot wire, switch-on effects may be prevented, as far as possible. 5.43 The current through the hot wire shall be measured with an instrument of class 0°2 or better to IS 6236: 1971. ‘The power input to the hot Wire must be kept constant. [f'no constant ac voltage is available. de voltage may be used. 5.4.4 The clecttic power developed in the hot wire must be measured to within - 0'5 percent for each measurement, It is measured through voltage taps fitted on both ends of the hot wire. 5.4.5 The taps and leads INSIDE the test array should be of the same material and diameter. OUTSIDE the test pieces, the lead-ins ( particularly the current leads ) should be of larger diameter to avoid excessive power loss. 5.46 The change in the temperature of the hot wire (Method I) thermocouple ( Method IL) is registered by a recording instrument. The recor ding instrument shall be of the muiti-range type having scales of 0-20 pV up to. 0-250 nV. The accuracy shall be better than 1 percent of the full scale deflection, While selecting the instrument care shall be taken to see that the proper working range is available. 5.4.7 The output of the thermocouple platinum wire shall be constant fo within 1 percent of the full scale deflection of the recording instrument over a period of 10 minutes before the start of the ‘measurement. 5.5 Furnace — For measuring at temperatures above ambient temperature, the test assembly complete with the measuring arrangement is intro~ duced into a furnace. 45.5.1 For the testing of test pieces up to standard brick size, an electrically heated furnace with the following internal dimensions is recommended: Height — 300 mm Width — 200 mm Depth — 220 - 250 mm $5.2 The test assembly is laid on two supports of 125mm x 10mm x 20mm in such a way that an all round uniform heating of the measuring test pieces is possible. The supports must be placed underneath in such a way that the test piece rests on the 125 mm x 10 mm surface, The refractory parts which support the test pieces may only have direct contact with the other furnace building ‘material in the cold region of the furnace so that electrical contacts with the heating elements are prevented,5.5.3 The furnace temperature is controlled by a thermocouple, the junction of which is mounted in the immediate vicinity of the heating element. 5.5.4 If samples have to be tested in an atmosphere other than air, the furnace shall be equipped adequately. 6 SAMPLING G.1 The samples to be measured shalll be selected in accordance with IS 1528 ( Part 7) : 1974. 7 SHAPE AND PREPARATION OF TEST PIECES 7.4 Dense and Insulating Shaped Products The test assembly is composed of two or three test pieces, depending on the dimensions of the samples, 7.L.1 It is convenient to use test picces of standard brick dimensions of 230mm x 114mm x 76 mm, However, the minimum dimensions of the test piece shail be 200 mm x 100 mm x 50 mm. 71.2 Two or three test pieces of the-same size shall be laid with their large faces on top of one another, to form a test assembly. The mating faces shall be ground flat, the flatness being con- trolled by means of a ruler. Visible deviations shall not be permitted. Test pieces which have to be ground or cut wet shall be dried before they are placed in the furnace. 7.4.3 The hot wire and thermocouple platinum wire shall be embedded between the faces of the test pieces so that a good contact is ensured. In the case of dense and hard test pieces, grooves are expediently cut into the mating faces to accom- modate the hot wire and the thermocouple. The width and depth of the grooves shall correspond to the diameter of the wire. The wires. shall be cemented into the grooves in order to ensure a good heat transfer in such away that the heat transfer to both test pieces is equal ( see Fig. 5). ‘Naw LILLE Sy Mece 7 Pi PLL OM tebe OAV 4 IS 1528 ( Part 16) : 1991 Finely ground material of the test piece mixed and stirred with 2 percent ( m/m ) of dextrine is used as cement. The grain size shall not exceed 63 um. 7.1.4 The test assembly with the embedded wires shall be dried before the test. 7.2 Chemically Bonded Bricks and Monolithic Materials ‘Testing of chemically bonded unfired bricks, and monolithic materials of all types ( e.g. concrete, castables, mortars, plastics, ete, ) in coujunetion with the ‘specifications laid down for the prepara~ tion and pretreatment of test pieces may also be carried out according to the method laid down in this standard. Clauses § and 6.1 are valid for the number, the dimensions and the processing of the test pieces. 72.1 Because the materials enumerated in 6.2 still contain a considerable amount of water” after setting, which escapes when the test assembly is heated’ up, the thermal conductivity changes continuously under these conditions. Therefore a pretreatment of the test pieces shall be agreed bet- ‘ween the purchaser and the manufacturer. 7.3 Powder and Granular Materials ‘The testing of powders and granular maierials is carried out in a 2-part ceramic container, each part having minimum internal dimensions of 200 mm x 100 mm x 50 mm ( see Fig. 6). The container material itself shall have good thermal conductivity (e. g. magnesite ). The lower part of the container is a rectangular box with a bottom. It is filled to the brim with the powder or the granular material to be tested. On top of this, the hot wire and the thermocouple are spread ‘out, resting on the edge of the box. ‘Then the upper part—a box with the same internal dimensions, without a bottom — is placed on it and filled to the brim. Finally the container 7, Pow! ECE, CLD Fic, 5 Eaneppine or Hor Wine aNp TazrMocourLe15.1528 ( Parta6 ) : 1998 COVERING SLAg a SSS) [I Fic, 6 Conraters wits Hor,Wire ano. Tnexmocourte Lao on BOTIOMED, CONTAINER is covered with a slab of the same ceramic mate- rial, The slab must be large enough to rest. on the edge of the box and must not load the material to betested. ‘The powder or the granular mat the usally ld ip loosely UE ogre apectod way of vibrating or pressing of the powder or the grain with a defined load is allowable. The density of the assembly. shall be determined and stated, ‘ensuring that it is the same in the upper and lower halves of the test assembly. 8 PROCEDURE, 8.1 Before the start of the thermal conductivity test, a state of thermal equilibrium shall have been achieved in the furnace and consequently in the’ test assembly. Temperature differences in the test piece-assembly more than 5 K will eause incorrect measurements. 8.2, The: temperature difference:can- be measured: directly. by using the circuit. shown in Fig... The furnace temperature: shall be regulated:.in such a way that the fluctuations in temperature of the measuring circuit do:ot exceed 0°05 K (see Fig. 2). ‘The: constant :initial: temperature “conditions: are essential for precise measurements. Table 1 shows, the choice of the power input to the hot wire in relation to the recording range and the period of relevant -measurement. for several. thermal, con- ductivity levels. ‘The preseribed accuracy ofthe time measurements is also given in Table 1. 8.3 After. checking .these conditions the current can be switched over 0 the heating circuit. This moment corresponds‘-with zero time of. measure+ ments, ‘The following data shall be recorded: a) Furnace temperature, b). Differential thermocouplevemf-as.a function of timeyand ©) Power input into the hot wire 9 EXPRESSION OF RESULTS 9.4: The crelation,. between thermal. conduetivit ‘and.the measured-data is given by'the equation: esr) hermal conductivity in Werm=7K=3, heating currentin A Us Voltage in'V T= length “of -the:-hot»-wire: between: the: voltage:taps P and, in'm. @ ‘Table 1 Recommendationof Power. Anput.and Recording. Range. of Instruments. (Clause 8.2) “Thermal imum rr of Recommended Power Level (Wan!) Conductivity Duration of test Measurement of ¢ eee ee eis () 020g O=80 a 01004 0-200 (Wim Key Mar 7 scale. scale scale stale © o1 2500 40 S + a on 1260 20 = 15 30 © 10 900 20 1s 40 5 150 20 450 10 30 15 150 = 40 350 10 o 130 300 = s 190 oF 120 300 = = 16 100 02 240 = = = 25 65 02 315 = = NOTE — This is based on a deflection in agreement with 08 % (full scale )AV() = temperature difference between the measurement and:reference thermo- couples at time t. period of time in seconds after switch- ing on the heating circuit, separation of hot wire and measure- ‘ment thermocouple in m, and thermal diffusivity in m*, s— a= = exponential integral {pu x Av (21) 2A Atchison t-te expression —FUCT) ig calculated from Table 2. 9.2 Example to Mlustrate Determination. of the ‘Thermal Conductivity In the following example for the determination of the thermal conductivity, the evalution of the ‘measurement is illustrated (see also Table 3 ). a) The values measured and calculated: have been compiled into Table 3. b) Incol 2 the differential thermocouple emf in microvolts is given at times 1, In col 3 this emf is converted to kelvin K ), - Ay (26) 6) In col 4 is the expression Cy calculated by division of the temperature difference at the moment 2t and at the time t. This expression should be-calculated from data of col 3. Examples: Ay (21) Av (60) _ 1229 K yg Ay) Av G0) Ay (2t)_ Av (96) __ 16063 Av Gt) Av(48) F056 K IS 1528 ( Part 16): 1991 Ep) values fssociated with the individual-A* (21) 4) The -Bi values are taken ‘Ae (2) from Table 2 of this standard and entered feo 5 ©) By substituting the expression—Bi(~ 4), Ay(+), power input and length of the hot wirein 9.1, is caleulated and entered incol 6. The time from which A becomes almost constant depends on the material. These values of 4 saa bo sonsiderod ascurate y(t v . ‘Avti, between 15 and 2°4, f) The actual value of A of a single test can be calculated us the mean value of the accurate values of col 6, for values of 8) The mean value of two tests at one tempe- rature will be reported. ‘The individual values of both tests should not deviate by ‘more than 5 percent from their mean value, 10 TEST REPORT 10.1 The test report shallinclude the following: 4) the testing establishment; b), the date of test; ©) designation of the test material (manu- facturer, customer, tye, batch number, sie ete, 5 @) dimensions of the measured test piece ©) number of the measured test pieces, on which series of measurements have been carried out; ) the individual values of thermal conductivity in Wam +, K™ with the corresponding test ‘temperature in °C; 2) furnace atmosphere; and fh) a reference to this method (Part 16 of 1S : 1528)IS 1528 ( Part 16): 1991 | o-os7s | 00370 3°2480 | 3°0917 2.4227 | 2"0473 1°5295 | 174852 11646 | 171358 o-9197 | 0°8997 07439 | 0°7313, 0°6173 | 0°6063 05193 | 0°5108 o4a2e 073818 073324 072919 or2s82 02298 0'2058 071853 071676 071523 on1389 on1272 On1168 071076 | 0°1068 10-0995 0-0922 00856 00797 0-074 070695 0652 or0612 070542 or0si1 orods2 or04s6 070432 oro4i0 00389 070352 070336 070320 00306 070292 00279 070268 0.0256 o'0246 29485 | 2°8166 1°9764 | 1'9094 1°4852 | 174028, r4o81 | 1084 0°8803 | o°8616 o-7171 | 0-7034 ‘0'5956 | 0°3852 o-0600 00565 0532 0502 oroa7s oro449 070426 oro404 00384 ‘0365 070347 070331 00316 070302 or0288 070276 070264 070253 070243 0°4865 | 0°4788 | 0°4712 (ot Av(2t) Table 2 ni ( az) #8 a Fmetion of S129. aan | >i satalsl «la ra | $3BG2 | HTERT | H3DIS | FOIE] FEOIO | TGON | HOT 276949 | 2°5820 | 24772 18461 | 1°7862 | 1.7295 113642 | 173274] 1°2920 10557 | 1-0310| 10071 0'8434| 0 8259 | 0'8082 0'6900 | 0°6770 | 0°6644 0°5750 | 0°5652 | 0°5555 408s 073510 03072 02709 072406 02150 071931 ons or1ss2 NOTE — Table 2 has been made up of statements found in the literature, see The expressions [Lec gp J sesntes inthe iterate a -» (~4) 7) av Gn Av) ‘and —Ei (x), respectively,1S 1528 ( Part 16): 1991 Table 3 Example of an Evaluation of the Measurements for the Determination of the ‘Thermal Conductivity in Accordance with the Hot Wire Parallel Method ( Clause 9.2) Time AV(1) PSTE) =e =n) ~~ «) (wv) OK) avG) 4 ar CW 1) ‘ 05s 005s 499 oor s 29 2 247 Om 246 02034 14s 18 4450434 196 0478 158 4 608 0593 +8 06321 157 30 71 O78 109 07828 154 155 36 372 08st rot 09177 154 8 1082 1056, sz 11294 133 o 1601209 146 13274 188 n 14051371 96 tea? 1607 120 1840 1-795 vl Nore — Ut = 1432 Wn| Standard Mark The use of the Standard Mark is governed by the provisions of the Bureau of indian Standards Act, 1986 and the Rules and Regulations made thereunder. 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