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
Public Enquiry End Date
19-Nov-2009
Publication Date
04-May-2010
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
23-Apr-2010
Due Date
28-Jun-2010
Completion Date
05-May-2010

Relations

Effective Date
01-Jun-2010

Overview

EN 196-9:2010 - Methods of testing cement - Part 9: Heat of hydration - Semi-adiabatic method describes a standardized laboratory procedure to measure the heat of hydration of cements and hydraulic binders using semi-adiabatic calorimetry (the Langavant method). The test provides a continuous record of heat released during the first days after mixing and expresses results in joules per gram (J/g) of cement. The standard applies to all cements and hydraulic binders except quick-setting cements.

Key Topics and Requirements

  • Principle: Heat emitted by a freshly mixed mortar sample is monitored in a semi-adiabatic calorimeter; the heat of hydration equals heat accumulated in the calorimeter plus heat lost to the ambient atmosphere.
  • Apparatus: Details for a semi-adiabatic calorimeter (Dewar-style insulated flask), reference calorimeter, insulated stopper, platinum resistance thermometers, temperature recording equipment, and a disposable mortar box (~800 cm³).
  • Calibration: Calorimeter calibration and performance limits are specified (coefficient of total heat loss ≤ 100 J·h⁻¹·K⁻¹ for a 20 K rise). Calibration procedures are given in Annex A.
  • Mortar composition and mixing: Test mortar batch mass and proportions are specified (total mass 1 575 ± 1 g comprising 360 g cement, 1 080 g standard sand, 180 g distilled or deionised water) and mixing timing is defined to limit thermal loss.
  • Laboratory conditions: Ambient and test-room temperature control requirements (e.g., mixing room (20 ± 2) °C; test room 20.0 ± 1.0 °C) and instrument placement guidance (reference calorimeter for up to six test calorimeters).
  • Measurement and calculation: Continuous temperature recording, calculation of heat accumulated, correction for heat losses, and expression of results in J/g. Precision, repeatability, and reproducibility information are included.
  • Limits and notes: Test sample temperature should not exceed 75 °C. EN 196-9 provides correlation guidance with the solution method (EN 196-8), noting best correlation at 41 h for semi-adiabatic vs 7 days for solution.

Applications and Users

EN 196-9:2010 is used for:

  • Quality control in cement production (monitoring early hydration heat for process control).
  • R&D and product development of cements and blended hydraulic binders (evaluating reaction kinetics).
  • Specification and compliance testing for builders, concrete producers, and standards laboratories.
  • Academic and materials research into hydration behavior and thermal effects in concrete. Typical users: cement manufacturers, independent testing laboratories, construction materials engineers, research institutions, and conformity assessment bodies.

Related Standards

  • EN 196-1 - Methods of testing cement - Determination of strength (reference for mortar preparation).
  • EN 196-8 - Heat of hydration - Solution method (alternative procedure; comparison and correlation with EN 196-9).
  • Relevant calibration and instrumentation standards referenced within EN 196-9:2010.

Keywords: EN 196-9:2010, heat of hydration, semi-adiabatic calorimetry, Langavant method, cement testing, calorimeter calibration, hydraulic binders.

Frequently Asked Questions

SIST EN 196-9:2010 is a standard published by the Slovenian Institute for Standardization (SIST). Its full title is "Methods of testing cement - Part 9: Heat of hydration - Semi-adiabatic method". This standard covers: 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).

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).

SIST EN 196-9:2010 is classified under the following ICS (International Classification for Standards) categories: 91.100.10 - Cement. Gypsum. Lime. Mortar. The ICS classification helps identify the subject area and facilitates finding related standards.

SIST EN 196-9:2010 has the following relationships with other standards: It is inter standard links to SIST EN 196-9:2004. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.

SIST EN 196-9:2010 is associated with the following European legislation: EU Directives/Regulations: 305/2011, 89/106/EEC; Standardization Mandates: M/114. When a standard is cited in the Official Journal of the European Union, products manufactured in conformity with it benefit from a presumption of conformity with the essential requirements of the corresponding EU directive or regulation.

SIST EN 196-9:2010 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.

Standards Content (Sample)


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

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

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
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.
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

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
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