1、 Reference number ISO 29582-1:2009(E) ISO 2009INTERNATIONAL STANDARD ISO 29582-1 First edition 2009-07-15 Methods of testing cement Determination of the heat of hydration Part 1: Solution method Mthodes dessai des ciments Dtermination de la chaleur dhydratation Partie 1: Mthode par dissolution ISO 2
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5、n below. COPYRIGHT PROTECTED DOCUMENT ISO 2009 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the
6、address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2009 All rights reservedISO 29582-1:2009(E) ISO 2009 All righ
7、ts reserved iii Contents Page Foreword iv 1 Scope . 1 2 Normative references . 1 3 Principle. 1 4 Reagents and materials . 2 5 Apparatus 2 6 Calorimeter calibration. 4 7 Determination of heat of solution . 6 8 Heat of hydration 10 9 Test report . 10 Bibliography . 12 ISO 29582-1:2009(E) iv ISO 2009
8、All rights reservedForeword ISO (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 interested in a su
9、bject 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 Electrotechnical Commission (
10、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 technical commi
11、ttees 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. ISO shall not b
12、e held responsible for identifying any or all such patent rights. ISO 29582-1 was prepared by Technical Committee ISO/TC 74, Cement and lime. ISO 29582 consists of the following parts, under the general title Methods of testing cement Determination of the heat of hydration: Part 1: Solution method P
13、art 2: Semi-adiabatic method INTERNATIONAL STANDARD ISO 29582-1:2009(E) ISO 2009 All rights reserved 1 Methods of testing cement Determination of the heat of hydration Part 1: Solution method 1 Scope This part of ISO 29582 describes a method of determining the heat of hydration of cements by means o
14、f solution calorimetry, also known as the solution method. The heat of hydration is expressed in joules per gram of cement. This part of ISO 29582 is applicable to cements and hydraulic binders, whatever their chemical composition. NOTE 1 Another procedure, called the semi-adiabatic method, is descr
15、ibed in ISO 29582-2. Either procedure can be used independently. NOTE 2 It has been demonstrated that the best correlation between the two methods is obtained at 7 d for the solution method in this part of ISO 29582 compared with 41 h for the semi-adiabatic method in ISO 29582-2. 2 Normative referen
16、ces The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 197-1, Cement Part 1: Composition, specifi
17、cations and conformity criteria for common cements 3 Principle The method consists of measuring the heats of solution, in an acid mixture, of anhydrous cement and cement hydrated under standardized conditions for a predetermined period of time, e.g. 7 days. These standardized hydration conditions ar
18、e as follows: water/cement ratio of 0,40; use of neat cement paste; storage at a constant temperature of (20,0 0,2) C during the whole hydration process. The heat of hydration for each period, H i , is obtained from the difference between the heat of solution of anhydrous cement, Q a , and that of h
19、ydrated cement, Q i . ISO 29582-1:2009(E) 2 ISO 2009 All rights reserved4 Reagents and materials 4.1 Acid mixture, analytical-reagent quality, obtained by adding 2,760 g of 40 % hydrofluoric acid (HF) per 100,0 g of (2,00 0,01) mol/l nitric acid (HNO 3 ), or 2,600 ml of hydrofluoric acid for every 1
20、00,0 ml of nitric acid. WARNING Hydrofluoric acid can cause painful skin burns which heal only with difficulty and precautions in handling this very corrosive substance should be strictly observed. 4.2 Acid mixture, proposed alternative, containing ammonium fluoride (NH 4 F) instead of hydrofluoric
21、acid, prepared as follows. Place about 400 g of (2,00 0,01) mol/l nitric acid and 7,2 g of ammonium fluoride in the flask. Then, add (2,00 0,01) mol/l nitric acid to make a total mass of 425,0 g 0,1 g. Any other procedure in the preparation of acid mixture can be adopted, provided that the same mass
22、 ratio of nitric acid to ammonium fluoride is conserved. The quantity (mass or volume) of acid used, which is common to all tests, shall be measured to 0,2 %. In the case of a dispute , only the reference acid mixture containing hydrofluoric acid is used. 4.3 Zinc oxide (ZnO), analytical quality, us
23、ed to determine the thermal capacity of the calorimeter and prepare as follows. Weigh 40 g to 50 g. Ignite at (950 25) C for 1 h. Cool in a desiccator. Grind to pass a 125 m sieve. Store in a desiccator. 4.4 Anhydrous cement, from which metallic iron has been removed with a magnet, stored in a seale
24、d container to avoid absorption of water or carbon dioxide. Bring the test sample to ambient temperature and carefully homogenize it before use. 4.5 Hydrated cement, test sample prepared as follows. Vigorously mix, either manually or mechanically, (100,0 0,1) g of anhydrous cement with (40,0 0,1) g
25、of distilled or deionized water for 3 min at ambient temperature. Place the resulting paste in plastic or glass cylindrical vials (three for each hydration period being tested) so that each vial contains 15 g to 20 g of material. Seal the vials by means of a stopper and, if necessary, with paraffin
26、wax or similar material and store them horizontally in a thermostatic bath maintained at a temperature of (20,0 0,2) C. 5 Apparatus 5.1 Calorimeter, comprised of the following (see Figure 1). NOTE The method does not deal with the standardization of the calorimetric apparatus, or the measuring instr
27、uments. Insulated flasks with a volume of about 650 ml have proved to be suitable. 5.1.1 Dissolution vessel, consisting of an insulated flask (e.g. Dewar flask), placed either in a heat insulated container set inside a box constructed of insulating material (e.g. wood, plastics), or immersed in a th
28、ermostatic water bath regulated to 0,2 C; and an insulated stopper (made of cork or plastic) through which holes are provided for the thermometer, the stirrer and the funnel used for introducing the sample. The insulation of the calorimeter shall ensure that the thermal leakage coefficient, K, (dete
29、rmined in accordance with 6.3) is less than 0,06 K per 15 min for each kelvin above ambient temperature. The internal surface of the flask, that part of the thermometer immersed in the acid mixture and the lower part of the stopper, shall be acid-mixture-resistant. ISO 29582-1:2009(E) ISO 2009 All r
30、ights reserved 3Key 1 stirrer motor 7 support 2 thermometer 8 flask support 3 ambient thermometer 9 box 4 flask 10 stirrer 5 insulating material 11 stopper 6 container 12 funnel Figure 1 Typical heat-of-solution calorimeter apparatus 5.1.2 Thermometer, either a Beckmann thermometer with a 5 C to 6 C
31、 scale and subdivisions every 0,01 C, or other measurement apparatus of an equal or higher accuracy, such as a thermistor or platinum resistance thermometer, positioned such that the end of the thermometer is at least 4 cm below the level of the liquid surface. Express temperature readings with a re
32、solution of 0,002 C. Adjust the zero of the Beckmann thermometer so that the upper limit of the scale is approximately the ambient, or water bath, temperature. Calibrate the thermometer in a thermostatic bath against a 0,01 C graduated and calibrated thermometer. ISO 29582-1:2009(E) 4 ISO 2009 All r
33、ights reserved5.1.3 Funnel, of acid-mixture-resistant plastics, through which the sample is introduced into the flask and which extends below the lower part of the stopper by 5 mm to 6 mm and is sealed during the test. 5.1.4 Stirrer, of acid-mixture-resistant plastics, positioned such that the blade
34、s are as close as possible to the bottom of the flask and rotated by a motor at a speed of (450 50) min1 . The motor shall have a low power rating (e.g. a motor of a few watts) so as to prevent any excessive heat emission from affecting measurements. 5.2 Thermostatic bath, e.g. water bath, for stori
35、ng the hydrated samples at a temperature of (20,0 0,2) C. 5.3 Mortar or electric grinder, for crushing the hydrated samples. 5.4 Plastic or glass vials, of capacity approximately 20 ml, for storing the hydrated paste. 5.5 Sieve, of mesh size 125 m. 5.6 Sieve, of mesh size 600 m. 5.7 Chronometer, gra
36、duated in seconds, for timing the temperature readings. 5.8 Two platinum crucibles, of capacity approximately 20 ml, for ignition of samples. 5.9 Electric furnace, naturally ventilated, capable of operating at (950 25) C, for ignition of samples. 5.10 Analytical balance, capable of weighing to an ac
37、curacy of 0,000 1 g. 5.11 Balance, of capacity 2 kg, capable of weighing to an accuracy of 0,2 g. 6 Calorimeter calibration 6.1 Principle Calibration of the calorimeter is carried out in order to determine its thermal capacity and thermal leakage coefficient. These characteristics are determined by
38、dissolving the ignited zinc oxide (4.2) in the acid mixture (4.1) and measuring the temperature of the calorimeter at fixed intervals of time. The temperature of the acid mixture shall be so set that after the dissolution reaction, the calorimeter temperature is at least 0,5 C below the ambient temp
39、erature. Where a water bath is used, the temperature of the bath is considered to be the ambient temperature for the calorimeter. 6.2 Procedure Measure a quantity of acid mixture (4.1) by mass or volume to 0,2 % such that the liquid level is approximately 2 cm below the calorimeter stopper. Place th
40、e acid mixture in the flask. Immediately before the determination of the thermal capacity, ignite the zinc oxide at (950 25) C for a maximum of 5 min and cool in a desiccator to room temperature. The mass of zinc oxide, m ZnO , being used, weighed to 0,000 1 g, is that required to satisfy Equation (
41、1): acid ZnO 60 1 m m = (1) where m acidis the mass of the acid mixture (4.1). ISO 29582-1:2009(E) ISO 2009 All rights reserved 5 Carry out the procedure as follows. a) Preliminary period: Stir the acid mixture for 40 min to 50 min. b) Pre-period: When the rate of temperature increase is constant, s
42、tart the timing using the chronometer (5.7) and record the initial temperature. c) Sample introduction: After 15 min, record the temperature, T 0 , and immediately add the zinc oxide sample to the acid mixture, taking not more than 1 min. d) Dissolution period: Stir the mixture for 30 min, after whi
43、ch the dissolution is considered as being complete, and then record the temperature, 30 . T Record the ambient temperature, T a . If the difference between T aand 30 T is less than 0,5 C, then repeat the test. e) Post-period: Record the final temperature, 45 T , after an additional 15 min. In order
44、to reduce reading errors, determine temperatures 15 , T 30 T and 45 T as the average of five different readings recorded at intervals of 1 min over the period 2 min before to 2 min after the prescribed time, T i(i.e. T i2 , Ti1 , T i , Ti+1 , Ti+2 ). Determine the value of T 0by extrapolation of the
45、 function of temperature against time in the period T 4to T 1 . If the extrapolated value differs from the T 0reading by more than 0,002 C, then replace T 0by the extrapolated value. If more than a trace of zinc oxide is found adhering to the tip of the funnel or to the stopper when the calorimeter
46、is opened, repeat the calibration. NOTE The temperature readings, therefore, effectively start 17 min before the zinc oxide sample is introduced and the last reading takes place 47 min after its introduction. The total duration of the calibration is 64 min. 6.3 Calculation of calibration characteris
47、tics 6.3.1 Corrected temperature increase, T cCalculate the corrected temperature increase, T c , expressed in kelvin, from Equation (2): c3 004 53 0 () 2 () TTTTT = (2) where 30 T and 45 T are the average values of five measurements made at intervals of 1 min. 6.3.2 Thermal leakage coefficient, K C
48、alculate the thermal leakage coefficient, K, in kelvin per 15 min per kelvin temperature difference, (K/15 minK 1 ), from Equation (3): 01 54 53 0 30 0 () () () TT TT K TT = (3) ISO 29582-1:2009(E) 6 ISO 2009 All rights reserved6.3.3 Thermal capacity, c Calculate the thermal capacity, c, expressed i
49、n joules per kelvin, from Equation (4): ZnO fa f c 1 077,43 0,364 (30 ) 0,50 ( ) m cT T T T =+ + (4) where m ZnOis the mass of zinc oxide, expressed in grams; T fis the temperature at the end of the dissolution period, i.e. 30 Beck , TT + where T Beckcorresponds to the zero on the Beckmann thermometer, with all temperatures expressed in degrees Celsius; T ais the temperature (i.e. ambient temperature) of zinc oxide when introdu
