Methods of testing cement - Part 9: Heat of hydration - Semi-adiabatic method

This European 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 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 independently.
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).

Prüfverfahren für Zement - Teil 9: Hydratationswärme - Teiladiabatisches Verfahren

Diese Europäische Norm beschreibt ein Verfahren zur Messung der Hydratationswärme von Zementen mit Hilfe der teiladiabatischen Kalorimetrie, das so genannte Langavant-Verfahren. Ziel dieser Prüfung ist die kontinuierliche Messung der Hydratationswärme von Zement während der ersten Tage. Die Hydratations¬wärme wird in Joule je Gramm Zement angegeben.
Diese Europäische Norm ist anwendbar für alle hydraulischen Bindemittel, ungeachtet ihrer chemischen Zusammensetzung, mit Ausnahme von schnell erstarrenden Zementen.
ANMERKUNG 1   Ein anderes Verfahren, das so genannte Lösungsverfahren, ist in EN 196-8 beschrieben. Beide Verfahren können unabhängig voneinander angewendet werden.
ANMERKUNG 2   Es wurde nachgewiesen, dass sich die beste Korrelation zwischen den beiden Verfahren nach 41 h für das teiladiabatische Verfahren (EN 196-9) und nach 7 Tagen für das Lösungsverfahren (EN 196-8) ergibt.

Méthodes d'essais des ciments - Partie 9: Chaleur d'hydratation - Méthode semi-adiabatique

La présente norme européenne décrit une méthode de mesure de la chaleur d'hydratation
des ciments par calorimétrie semi-adiabatique, dite méthode de Langavant. L'essai a pour but
de mesurer en continu la chaleur d'hydratation du ciment au cours des tout premiers jours. La
chaleur d’hydratation est exprimée en joules par gramme de ciment.
La présente norme s'applique à tous les ciments et liants hydrauliques, quelle que soit leur
composition chimique, à l'exception des ciments à prise rapide.
NOTE 1 Une autre méthode dite méthode de dissolution est décrite dans l’EN 196-8. Les deux
méthodes peuvent être utilisées indépendamment.
NOTE 2 Il a été démontré que la meilleure corrélation entre les deux méthodes est obtenue à 41 h
par la méthode semi-adiabatique (EN 196-9), et à 7 jours par la méthode de dissolution (EN 196-8).

Metode preskušanja cementa - 9. del: Toplota hidratacije - Semiadiabatska metoda

Ta evropski standard opisuje metodo za merjenje toplote hidratacije cementov s pomočjo semiadiabatske metode, ki je znana tudi kot Langavantova metoda. Namen preskusa je neprekinjeno merjenje toplote hidratacije cementa prvih nekaj dni. Toplota hidratacije je izražena v joulih na gram cementa. Ta standard velja za vse cemente in hidravlična veziva, ne glede na njihovo kemično sestavo, z izjemo hitrovezočih cementov.

General Information

Status
Published
Publication Date
23-Mar-2010
Current Stage
9060 - Closure of 2 Year Review Enquiry - Review Enquiry
Due Date
04-Jun-2022
Completion Date
04-Jun-2022

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Metode preskušanja cementa - 9. del: Toplota hidratacije - Semiadiabatska metodaPrüfverfahren für Zement - Teil 9: Hydratationswärme - Teiladiabatisches VerfahrenMethods of testing cement - Part 9: Heat of hydration - Semi-adiabatic method91.100.10Cement. Mavec. Apno. MaltaCement. Gypsum. Lime. MortarICS:Ta slovenski standard je istoveten z:EN 196-9:2010SIST EN 196-9:2010en,de01-junij-2010SIST EN 196-9:2010SLOVENSKI

STANDARDSIST EN 196-9:20041DGRPHãþD
SIST EN 196-9:2010
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE 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

Prüfverfahren für Zement - Teil 9: Hydratationswärme - 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 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 made 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, Finland, 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
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR 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: ESIST EN 196-9:2010

EN 196-9:2010 (E) 2 Contents Page Foreword .............................................................................................................................................................. 31Scope ...................................................................................................................................................... 42Normative references ............................................................................................................................ 43Principle .................................................................................................................................................. 44Apparatus ............................................................................................................................................... 45Determination of the heat of hydration ............................................................................................... 75.1Laboratory .............................................................................................................................................. 75.2Procedure ............................................................................................................................................... 85.2.1Mortar composition ............................................................................................................................... 85.2.2Mixing ...................................................................................................................................................... 85.2.3Positioning of the test sample .............................................................................................................. 85.3Measurement of heating ....................................................................................................................... 86Calculation of the heat of hydration .................................................................................................... 96.1Principles of calculations ..................................................................................................................... 96.2Calculation of the heat accumulated in the calorimeter .................................................................... 96.3Calculation of heat lost into ambient atmosphere ........................................................................... 106.4Calculation of heat of hydration ......................................................................................................... 117Expression of results .......................................................................................................................... 117.1Reporting of results ............................................................................................................................. 117.2Precision ............................................................................................................................................... 117.2.1Repeatability ......................................................................................................................................... 117.2.2Reproducibility ..................................................................................................................................... 11Annex A (normative)

Calibration of the calorimeter ...................................................................................... 12A.1Principle ................................................................................................................................................ 12A.2Apparatus and power supply ............................................................................................................. 12A.3Calibration procedure ......................................................................................................................... 13A.3.1Determination of the coefficient of total heat loss, . ....................................................................... 13A.3.2Determination of the thermal capacity .............................................................................................. 15Annex B (informative)

Worked example of determination of heat of hydration ......................................... 17B.1General test conditions ....................................................................................................................... 17B.2Basic calculations................................................................................................................................ 17B.3Determination of test results .............................................................................................................. 17Bibliography ...................................................................................................................................................... 20

SIST EN 196-9:2010

EN 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. This 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 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 supports 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: Pozzolanicity 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 196-4, 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 Republic, 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. SIST EN 196-9:2010

EN 196-9:2010 (E) 4 1 Scope This European 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 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 independently. 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 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 196-1, Methods of testing cement — Part 1: Determination of strength EN 573-3:2009, Aluminium and aluminium 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 development 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 compared 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 rigid 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 hemispherical 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 container 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 a support 40 mm to 50 mm thick made of a material having low thermal SIST EN 196-9:2010

EN 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 low 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 into 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/m3 approximately) 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, shall 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 central part ensuring the tight fitting of the stopper. d) Performance characteristics. The coefficient of total heat loss of the calorimeter shall not exceed 100 J⋅h-1⋅K-1 for a temperature rise of 20 K. This value, together with the thermal capacity, shall be determined in accordance with the calibration 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 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 an aluminium cylinder of the same thermal capacity as the mortar box and mortar sample may be used.

SIST EN 196-9:2010
EN 196-9:2010 (E) 6 56410789132
Key
platinum resistance thermometer 5
thermometer pocket 9
rigid casing 2
gasket 6
dewar flask 10
oil 3
insulating stopper 7
mortar sample
mortar box 8
rubber disc
Figure 1 — Typical calorimeter SIST EN 196-9:2010

EN 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 sectional area not greater than 0,25 mm2 in 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 K⋅mW-1 (thermal resistance equivalent to that of a copper conductor with a sectional area of 0,25 mm2 and 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 temperature 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 the coefficient of heat loss of the calorimeter is less than 100 J⋅h-1⋅K-1 for 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, having 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 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 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 recording 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 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 approximately 120 mm. The velocity of the ventilation air around the calorimeters shall be less than 0,5 m⋅s-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 in the centre. SIST EN 196-9:2010

EN 196-9:2010 (E) 8 5.2 Procedure 5.2.1 Mortar composition The composition of the mortar shall be in accordance with EN 196-1 and the test sample shall have a total mass of (1 575 ± 1) g. Each batch of mortar to be mixed shall consist of (360,0 ± 0,5) g cement; (1 080 ± 1) g sand from a sample of CEN standard sand complying with the requirements in EN 196-1; and (180,0 ± 0,5) g distilled or deionised water. NOTE Since it is not possible to recover all the material added to the mixer bowl the mortar batch to be mixed should be slightly more than 1 575 g, the proportions by mass of the various constituents being maintained. 5.2.2 Mixing The cement, the water, the sand, the mortar box, the mixer bowl and the other instruments coming into contact with the mortar shall be stored in the test room. With the mixer in the operating position, pour the sand and then the cement into the mixer bowl; homogenise the mixture of sand and cement for 30 s at low speed; pour in the water, record the time, and mix immediately at low speed for 60 s; set the mixer to high speed and mix for a further 60 s. NOTE In order to avoid thermal losses, it is recommended to carry out the mixing in a relatively short time. It is for this reason that the mixing time prescribed in EN 196-1 has been shortened. 5.2.3 Positioning of the test sample Immediately after mixing weigh (1 575 ± 1) g of mortar into the box (see 4.4) which has previously been weighed, with its lid, to an accuracy of ± 0,5 g. Place the lid in position making sure that i

...

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Metode preskušanja cementa - 9. del: Toplota hidratacije - Semiadiabatska metodaPrüfverfahren für Zement - Teil 9: Hydratationswärme - Teiladiabatisches VerfahrenMethods of testing cement - Part 9: Heat of hydration - Semi-adiabatic method91.100.10Cement. Mavec. Apno. MaltaCement. Gypsum. Lime. MortarICS:Ta slovenski standard je istoveten z:FprEN 196-9kSIST FprEN 196-9:2009en,fr,de01-oktober-2009kSIST FprEN 196-9:2009SLOVENSKI

STANDARD
kSIST FprEN 196-9:2009
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
FINAL DRAFT
FprEN 196-9
August 2009 ICS 91.100.10 Will supersede EN 196-9:2003English Version
Methods of testing cement - Part 9: Heat of hydration - Semi-adiabatic method

Prüfverfahren für Zement - Teil 9: Hydratationswärme - Teiladiabatisches Verfahren This draft European Standard is submitted to CEN members for unique acceptance procedure. It has been drawn up by the Technical Committee CEN/TC 51.

If this draft becomes a European Standard, 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 any alteration.

This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other language made 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, Cyprus, Czech Republic, 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 United Kingdom.

Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without notice and shall not be referred to as a European Standard.

EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,

B-1000 Brussels © 2009 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. FprEN 196-9:2009: EkSIST FprEN 196-9:2009

FprEN 196-9:2009 (E) 2 Contents page Foreword ................................................................................................................................................. 31Scope.......................................................................................................................................... 42Normative references ............................................................................................................... 43Principle ..................................................................................................................................... 44Apparatus .................................................................................................................................. 45Determination of the heat of hydration ................................................................................... 75.1Laboratory ................................................................................................................................. 75.2Procedure .................................................................................................................................. 85.2.1Mortar composition ................................................................................................................... 85.2.2Mixing ......................................................................................................................................... 85.2.3Positioning of the test sample ................................................................................................. 85.3Measurement of heating ........................................................................................................... 86Calculation of the heat of hydration ........................................................................................ 96.1Principles of calculations ......................................................................................................... 96.2Calculation of the heat accumulated in the calorimeter ....................................................... 96.3Calculation of heat lost into ambient atmosphere .............................................................. 106.4Calculation of heat of hydration ............................................................................................ 117Expression of results.............................................................................................................. 117.1Reporting of results ................................................................................................................ 117.2Precision .................................................................................................................................. 117.2.1Repeatability ............................................................................................................................ 117.2.2Reproducibility ........................................................................................................................ 11Annex A (normative)

Calibration of the calorimeter ......................................................................... 12A.1Principle ................................................................................................................................... 12A.2Apparatus and power supply ................................................................................................. 12A.3Calibration procedure ............................................................................................................. 13A.3.1Determination of the coefficient of total heat loss, . .......................................................... 13A.3.2Determination of the thermal capacity .................................................................................. 16Annex B (informative)

Worked example of determination of heat of hydration ............................. 18B.1General test conditions .......................................................................................................... 18B.2Basic calculations ................................................................................................................... 18B.3Determination of test results ................................................................................................. 18Bibliography ......................................................................................................................................... 21

kSIST FprEN 196-9:2009

FprEN 196-9:2009 (E) 3 Foreword This document (FprEN 196-9:2009) has been prepared by Technical Committee CEN/TC 51, "Cement and building limes", the secretariat of which is held by NBN. This document is currently submitted to the Unique Acceptance Procedure. This document will supersede EN 196-9:2003. This European Standard on the methods of testing cement comprises the following Parts: EN 196-1 Methods of testing cement — Part 1: Determination of strength EN 196-2 Methods of testing cement — Part 2: Chemical analysis of cement EN 196-3 Methods of testing cement — Part 3: Determination of setting times and soundness EN 196-5 Methods of testing cement — Part 5: Pozzolanicity test for pozzolanic cement EN 196-6 Methods of testing cement — Part 6: Determination of fineness EN 196-7 Methods of testing cement — Part 7: Methods of taking and preparing samples of cement EN 196-8 Methods of testing cement — Part 8: Heat of hydration — Solution method EN 196-9 Methods of testing cement — Part 9: Heat of hydration — Semi-adiabatic method EN 196-10 Methods of testing cement — Part 10: Determination of the water-soluble chromium (VI) content of cement CEN/TR 196-4 Methods of testing cement — Part 4: Quantitative determination of constituents kSIST FprEN 196-9:2009

FprEN 196-9:2009 (E) 4

1 Scope This European 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 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 independently. 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 7 days for the heat of solution method (EN 196-8). 2 Normative references 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 196-1, Methods of testing cement — Part 1: Determination of strength EN 573-3, Aluminium and aluminium 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 development 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 compared 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 rigid 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) an insulated flask (e.g. Dewar flask), made of silver plated borosilicate glass; cylindrical in shape with a hemispherical 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 container and evenly distribute the load on the glass wall. kSIST FprEN 196-9:2009

FprEN 196-9:2009 (E) 5 b) a 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 a support 40 mm to 50 mm thick made of a material having low thermal 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 low 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) an insulating stopper, made of three parts.  The lower part, which is inserted into 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/m3 approximately) 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.  The central part, which serves to ensure the tightness of the calorimeter whilst contributing to the reduction of losses, shall consist of a foam rubber disc 120 mm in diameter.  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 central part ensuring the tight fitting of the stopper. d) performance characteristics. The coefficient of total heat loss of the calorimeter shall not exceed 100 J⋅h-1⋅K-1 for a temperature rise of 20 K. This value, together with the thermal capacity, shall be determined in accordance with the calibration procedure given in Annex A (see A.3.1). Recalibration is necessary:  at least every 4 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 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 an aluminium cylinder of the same thermal capacity as the mortar box and mortar sample may be used.

kSIST FprEN 196-9:2009
FprEN 196-9:2009 (E) 6 56410789132
Key
platinum resistance thermometer 5
thermometer pocket 9
rigid casing 2
gasket 6
dewar flask 10
oil 3
insulating stopper 7
mortar sample
mortar box 8
rubber disc
Figure 1 — Typical calorimeter kSIST FprEN 196-9:2009

FprEN 196-9:2009 (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 sectional area not greater than 0,25 mm2 in 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 K⋅mW-1 (thermal resistance equivalent to that of a copper conductor with a sectional area of 0,25 mm2 and 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 temperature 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 (4 wires 0,5 mm in diameter), but shall be such that the coefficient of heat loss of the calorimeter is less than 100 J⋅h-1⋅K-1 for 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, having 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 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 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 recording 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 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 approximately 120 mm. The velocity of the ventilation air around the calorimeters shall be less than 0,5 m⋅s-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 in the centre. kSIST FprEN 196-9:2009

FprEN 196-9:2009 (E) 8 5.2 Procedure 5.2.1 Mortar composition The composition of the mortar shall be in accordance with EN 196-1 and the test sample shall have a total mass of (1 575 ± 1) g. Each batch of mortar to be mixed shall consist of (360,0 ± 0,5) g cement; (1 080 ± 1) g sand from a sample of CEN standard sand complying with the requirements in EN 196-1; and (180,0 ± 0,5) g distilled or deionised water. NOTE Since it is not possible to recover all the material added to the mixer bowl the mortar batch to be mixed should be slightly more than 1 575 g, the proportions by mass of the various constituents being maintained. 5.2.2 Mixing The cement, the water, the sand, the mortar box, the mixer bowl and the other instruments coming into contact with the mortar shall be stored in the test room. With the mixer in the operating position, pour the sand and then the cement into the mixer bowl; homogenise the mixture of sand and cement for 30 s at low speed; pour in the water, record the time, and mix immediately at low speed for 60 s; set the mixer to high speed and mix for a further 60 s. NOTE In order to avoid thermal losses, it is recommended to carry out the mixing in a relatively short time. It is for this reason that the mixing time prescribed in standard EN 196-1 has been shortened. 5.2.3 Positioning of the test sample Immediately after mixing weigh (1 575 ± 1) g of mortar into the box (see 4.4) which has previously been weighed, with its lid, to an accuracy of ± 0,5 g. Place the lid in position making sure that it seals tightly. Fill the thermometer pocket with (2,5 ± 0,5) cm3 of oil (e.g. thin mineral oil) in order to improve the thermal contact between the test sample and the thermometer. Weigh the filled mortar box, to an accuracy of ± 0,5 g in order to be able to check at the end of the test for any lea

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