1、BS EN 196-9:2010ICS 91.100.10NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDMethods of testingcementPart 9: Heat of hydration Semi-adiabatic methodThis British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 31 May2010.
2、BSI 2010ISBN 978 0 580 68244 5Amendments/corrigenda issued since publicationDate CommentsBS EN 196-9:2010National forewordThis British Standard is the UK implementation of EN 196-9:2010. Itsupersedes BS EN 196-9:2003 which is withdrawn.The UK participation in its preparation was entrusted to Technic
3、alCommittee B/516/12, Sampling and testing.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance with a Brit
4、ish Standard cannot confer immunityfrom legal obligations.BS EN 196-9:2010EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 196-9 March 2010 ICS 91.100.10 Supersedes EN 196-9:2003English Version Methods of testing cement - Part 9: Heat of hydration - Semi-adiabatic method Prfverfahren fr Zement -
5、 Teil 9: Hydratationswrme - Teiladiabatisches Verfahren This European Standard was approved by CEN on 21 February 2010. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without
6、 any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language ma
7、de by translation under the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Fin
8、land, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES
9、KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 196-9:2010: EBS EN 196-9:2010EN 196-9:2010 (E) 2 Contents Page Foreword 31 Scope 42 Normative references 4
10、3 Principle 44 Apparatus . 45 Determination of the heat of hydration . 75.1 Laboratory 75.2 Procedure . 85.2.1 Mortar composition . 85.2.2 Mixing 85.2.3 Positioning of the test sample 85.3 Measurement of heating . 86 Calculation of the heat of hydration 96.1 Principles of calculations . 96.2 Calcula
11、tion of the heat accumulated in the calorimeter 96.3 Calculation of heat lost into ambient atmosphere . 106.4 Calculation of heat of hydration . 117 Expression of results 117.1 Reporting of results . 117.2 Precision . 117.2.1 Repeatability . 117.2.2 Reproducibility . 11Annex A (normative) Calibratio
12、n of the calorimeter 12A.1 Principle 12A.2 Apparatus and power supply . 12A.3 Calibration procedure . 13A.3.1 Determination of the coefficient of total heat loss, . 13A.3.2 Determination of the thermal capacity 15Annex B (informative) Worked example of determination of heat of hydration . 17B.1 Gene
13、ral test conditions . 17B.2 Basic calculations 17B.3 Determination of test results 17Bibliography 20BS EN 196-9:2010EN 196-9:2010 (E) 3 Foreword This document (EN 196-9:2010) has been prepared by Technical Committee CEN/TC 51, “Cement and building limes“, the secretariat of which is held by NBN. Thi
14、s European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by September 2010, and conflicting national standards shall be withdrawn at the latest by September 2010. Attention is drawn to the possibility that some
15、of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association, and s
16、upports essential requirements of EU Directive(s). This document supersedes EN 196-9:2003. EN 196, Methods of testing cement, consists of the following parts: Part 1: Determination of strength Part 2: Chemical analysis of cement Part 3: Determination of setting times and soundness Part 5: Pozzolanic
17、ity test for pozzolanic cement Part 6: Determination of fineness Part 7: Methods of taking and preparing samples of cement Part 8: Heat of hydration Solution method Part 9: Heat of hydration Semi-adiabatic method Part 10: Determination of the water-soluble chromium (VI) content of cement CEN/TR 196-
18、4, Methods of testing cement Part 4: Quantitative determination of constituents According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republi
19、c, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN 196-9:2010EN 196-9:2010 (E) 4 1 Scope This Europ
20、ean Standard describes a method of measuring the heat of hydration of cements by means of semi-adiabatic calorimetry, also known as the Langavant method. The aim of the test is the continuous measurement of the heat of hydration of cement during the first few days. The heat of hydration is expressed
21、 in joules per gram of cement. This standard is applicable to all cements and hydraulic binders, whatever their chemical composition, with the exception of quick-setting cements. NOTE 1 An alternative procedure, called the solution method, is described in EN 196-8. Either procedure can be used indep
22、endently. NOTE 2 It has been demonstrated that the best correlation between the two methods is obtained at 41 h for the semi-adiabatic method (EN 196-9) compared with seven days for the heat of solution method (EN 196-8). 2 Normative references The following referenced documents are indispensable fo
23、r 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 196-1, Methods of testing cement Part 1: Determination of strength EN 573-3:2009, Aluminium and alumi
24、nium alloys Chemical composition and form of wrought products Part 3: Chemical composition and form of products 3 Principle The semi-adiabatic method consists of introducing a sample of freshly made mortar into a calorimeter in order to determine the quantity of heat emitted in accordance with the d
25、evelopment of the temperature. At a given point in time the heat of hydration of the cement contained in the sample is equal to the sum of the heat accumulated in the calorimeter and the heat lost into the ambient atmosphere throughout the period of the test. The temperature rise of the mortar is co
26、mpared with the temperature of an inert sample in a reference calorimeter. The temperature rise depends mainly on the characteristics of the cement and is normally between 10 K and 50 K. 4 Apparatus 4.1 Calorimeter, consisting of an insulated flask sealed with an insulated stopper and encased in a r
27、igid casing which acts as its support (see Figure 1). Both the calorimeter used for the test and that for the reference (see 4.2) shall have the following construction and characteristics: a) Insulated flask (e.g. Dewar flask), made of silver plated borosilicate glass; cylindrical in shape with a he
28、mispherical bottom. The internal dimensions shall be approximately 95 mm in diameter and 280 mm in depth; and external diameter of approximately 120 mm. A rubber disc of approximately 85 mm diameter and 20 mm thickness shall be placed at the bottom of the flask to act as support for the sample conta
29、iner and evenly distribute the load on the glass wall. b) Very rigid casing, having a sufficiently wide base to ensure good stability of the whole unit (e.g. made of duralumin, 3 mm thick). The flask shall be separated from the lateral walls of the casing by approximately 5 mm air space and rest on
30、a support 40 mm to 50 mm thick made of a material having low thermal BS EN 196-9:2010EN 196-9:2010 (E) 5 conductivity (e.g. expanded polystyrene). The upper edge of the flask shall be protected by a rubber gasket above, and in contact with, which shall be a ring, not less than 5 mm thick, made of lo
31、w thermal conductivity material, fixed to the calorimeter casing. The ring shall serve to locate the flask in position and provide a bearing surface for the stopper so as to ensure the tightness of the locking device. c) Insulating stopper, made of three parts: 1) the lower part, which is inserted i
32、nto the flask and which serves to provide a maximum prevention of heat loss into the external atmosphere. It shall be cylindrical in shape, of diameter equal to the internal diameter of the flask, and in thickness approximately 50 mm. It shall be made of expanded polystyrene (class 20 kg/m3approxima
33、tely) or of another material of similar thermal characteristics. Its base can be protected by a layer of plastic (e.g. polymethyl methacrylate), approximately 2 mm thick; 2) the central part, which serves to ensure the tightness of the calorimeter whilst contributing to the reduction of losses, shal
34、l consist of a foam rubber disc 120 mm in diameter; 3) the upper part, which is intended to ensure the correct and consistent positioning of the stopper unit against the Dewar flask, shall consist of a rigid casing incorporating a snap locking device in such a way as to compress the foam rubber cent
35、ral part ensuring the tight fitting of the stopper. d) Performance characteristics. The coefficient of total heat loss of the calorimeter shall not exceed 100 Jh-1K-1for a temperature rise of 20 K. This value, together with the thermal capacity, shall be determined in accordance with the calibration
36、 procedure given in Annex A (see A.3.1). Recalibration is necessary: at least every four years or after 200 tests; whenever deterioration occurs in the calorimeter or an insulating component. In order not to impair the insulation of the calorimeter, the temperature of the mortar under test shall not
37、 exceed 75 C. 4.2 Reference calorimeter, having the same construction and characteristics as the test calorimeter (see 4.1). It shall contain a mortar box in which is a sample of mortar mixed at least 12 months previously (and is considered to be inert). NOTE Where an inert sample is not available a
38、n aluminium cylinder of the same thermal capacity as the mortar box and mortar sample may be used. BS EN 196-9:2010EN 196-9:2010 (E) 6 56410789132Key 1 platinum resistance thermometer 5 thermometer pocket 9 rigid casing 2 gasket 6 dewar flask 10 oil 3 insulating stopper 7 mortar sample 4 mortar box
39、8 rubber disc Figure 1 Typical calorimeter BS EN 196-9:2010EN 196-9:2010 (E) 7 4.3 Platinum resistance thermometers, for the reference calorimeter and each test calorimeter, having a minimum range 19 C to 75 C. If the conductors of the electrical resistor are made of copper they shall have a section
40、al area not greater than 0,25 mm2in the part which passes through the stopper. If they are made of another metal the total thermal resistance per centimetre of conductor shall be greater than 0,10 KmW-1(thermal resistance equivalent to that of a copper conductor with a sectional area of 0,25 mm2and
41、1 cm in length). The thermal output of the thermometer shall not exceed 3 mW. Direct current supply, which constitutes a power input, shall be avoided if the thermal output exceeds 0,2 mW. It is advisable to ensure the accuracy of the overall temperature measuring and recording equipment. The temper
42、ature of the test sample shall be measured to an accuracy of 0,3 C. Where the calorimeter is calibrated in situ with the conductors used for the tests of heat of hydration, the total sectional area of the conductors will be a maximum of 0,80 mm2(four wires 0,5 mm in diameter), but shall be such that
43、 the coefficient of heat loss of the calorimeter is less than 100 Jh-1K-1for a temperature rise of 20 K (see A.3.1.1). The protective sheath of these conductors shall be made of a material having a low thermal conductivity. 4.4 Mortar box, consisting of a cylindrical container fitted with a cover, h
44、aving a volume of approximately 800 cm3, designed to contain the sample of mortar under test. The mortar box, discarded after each test, shall be impermeable to water vapour. This shall be checked in use by weighing the mortar box after each test (see 5.2.3). It shall be made of electrically counter
45、 welded tin plate of nominal thickness 0,3 mm; have a diameter of approximately 80 mm and a height of approximately 165 mm. Its height shall be designed to provide an air space of approximately 10 mm between the top of the mortar box and the stopper. The lid of the mortar box shall be fitted with a
46、central thermometer pocket in the form of a cylindrical pipe, closed at its base. The internal diameter of the pocket shall be slightly greater than that of the thermometer. Its length shall be approximately 100 mm to 120 mm and enable it to extend to the centre of the test sample. 4.5 Temperature r
47、ecording apparatus, capable of recording the measurements taken by each thermometer. 4.6 Mortar mixing apparatus, conforming to EN 196-1. 5 Determination of the heat of hydration 5.1 Laboratory The laboratory where the mortar is mixed shall be maintained at a temperature of (20 2) C. The room where
48、the test is carried out shall be maintained at a temperature of (20,0 1,0) C. The measured temperature of the reference calorimeter shall be considered to be the ambient temperature and shall be maintained during the test within 0,5 C. The distance between each of the calorimeters shall be approxima
49、tely 120 mm. The velocity of the ventilation air around the calorimeters shall be less than 0,5 ms-1. When several tests are being carried out simultaneously, at least one reference calorimeter shall be provided for every six test calorimeters; where several test calorimeters are used with one reference calorimeter, a hexagonal arrangement shall be used with the reference calorimeter i
