Methods of testing cement - Part 11: Heat of hydration - Isothermal Conduction Calorimetry method

This document specifies the apparatus and procedure for determining the heat of hydration of cements and other hydraulic binders at different test ages by isothermal conduction calorimetry.
This test procedure is intended for measuring the heat of hydration of cement up to 7 days in order to obtain correspondence between Isothermal Conduction Calorimetry (ICC) and EN 196 8 and EN 196 9. Nevertheless this test duration may be critical for some apparatus, even if they can work properly at shorter test ages.
Contrary to EN 196 8 this method gives the heat of hydration continuously over the time. Additionally, the heat flow versus time is given.

Prüfverfahren für Zement - Teil 11: Bestimmung der Hydratationswärme von Zement durch isotherme Wärmeflusskalorimetrie

Dieses Dokument legt die Prüfeinrichtung und das Verfahren zur Bestimmung der Hydratationswärme von Zement und anderer hydraulischer Binder zu unterschiedlichen Prüfaltern mittels isothermischer Wärme¬flusskalorimetrie fest.
Um einen Zusammenhang zwischen der isothermen Wärmeflusskalorimetrie und EN 196 8 und EN 196 9 zu erhalten, sieht dieses Verfahren die Messung der Hydratationswärme von Zement über einen Zeitraum von bis zu 7 Tagen vor. Dennoch kann diese Prüfdauer für einige Geräte kritisch sein, auch wenn diese bei kürzeren Prüfdauern ordnungsgemäß funktionieren.
Im Gegensatz zu EN 196 8 legt dieses Verfahren die Hydratationswärme im Zeitverlauf dar. Zusätzlich wird der Wärmefluss im Verhältnis zur Zeit angegeben.

Méthodes d’essais des ciments - Partie 11: Chaleur d’hydratation - Méthode par calorimétrie à conduction isotherme

La présente Norme européenne spécifie l’appareillage et le mode opératoire permettant de déterminer la chaleur d’hydratation des ciments et autres liants hydrauliques à différents âges d’essai par calorimétrie à conduction isotherme.
Ce mode opératoire sert à mesurer la chaleur d’hydratation du ciment pendant une durée allant jusqu’à 7 jours afin d’obtenir une correspondance entre la calorimétrie à conduction isotherme  et les normes EN 196-8 et EN 196-9. Néanmoins, cette durée d’essai peut être critique pour certains appareils, même s’ils peuvent fonctionner correctement à des âges d’essai plus courts.
Contrairement à l’EN 196-8 (méthode par dissolution), cette méthode donne la chaleur d’hydratation de façon continue dans le temps. Elle donne également le flux thermique en fonction du temps.

Metode preskušanja cementa - 11. del: Toplota hidratacije - Izotermna kondukcijska kalorimetrija (ICC)

Ta evropski standard določa napravo in postopek za določanje toplote hidratacije cementov ter drugih hidravličnih veziv pri različnih preskusnih starostih z izotermno kondukcijsko kalorimetrijo.
Ta preskusni postopek je namenjen merjenju toplote hidratacije cementa do 7 dni, da se pridobijo podatki, ki so skladni s standardom EN 196 8. Kljub temu je lahko trajanje preskusa kritično za nekatere naprave, tudi če lahko pravilno delujejo pri krajših preskusnih starostih.
V nasprotju s standardom EN 196 8 (metoda z raztopino) ta metoda kontinuirano podaja toploto hidratacije. Poleg tega je podan tudi toplotni tok v primerjavi s časom.

General Information

Status
Published
Publication Date
18-Dec-2018
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
19-Dec-2018
Completion Date
19-Dec-2018

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Metode preskušanja cementa - 11. del: Toplota hidratacije - Izotermna kondukcijska kalorimetrija (ICC)Prüfverfahren für Zement - Teil 11: Bestimmung der Hydratationswärme von Zement durch isotherme WärmeflusskalorimetrieMéthodes d’essais des ciments - Partie 11: Chaleur d’hydratation - Méthode par calorimétrie à conduction isothermeMethods of testing cement - Part 11: Heat of hydration - Isothermal Conduction Calorimetry method91.100.10Cement. Mavec. Apno. MaltaCement. Gypsum. Lime. MortarICS:Ta slovenski standard je istoveten z:EN 196-11:2018SIST EN 196-11:2019en,fr,de01-februar-2019SIST EN 196-11:2019SLOVENSKI

STANDARD
SIST EN 196-11:2019
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 196-11
December
t r s z ICS
{ sä s r rä s r English Version
Methods of testing cement æ Part

s sã Heat of hydration æ Isothermal Conduction Calorimetry method Méthodes d 5essais des ciments æ Partie

s sã Chaleur d 5hydratation æ Méthode par calorimétrie à conduction isotherme
Prüfverfahren für Zement æ Teil

s sã Bestimmung der Hydratationswärme von Zement durch isotherme Wärmeflusskalorimetrie This European Standard was approved by CEN on

t v September
t r s zä

egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä

translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä

CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä

EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre:
Rue de la Science 23,
B-1040 Brussels

t r s z CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN

s { xæ s sã t r s z ESIST EN 196-11:2019

EN 196-11:2018 (E) 2 Contents Page European foreword ...................................................................................................................................................... 3 1 Scope .................................................................................................................................................................... 4 2 Normative references .................................................................................................................................... 4 3 Terms and definitions ................................................................................................................................... 4 4 Apparatus .......................................................................................................................................................... 6 4.1 General................................................................................................................................................................ 6 4.2 Principle ............................................................................................................................................................. 6 4.3 Thermostat ........................................................................................................................................................ 7 4.4 Calorimeter technical parameters............................................................................................................ 7 5 Calibration ......................................................................................................................................................... 8 5.1 General................................................................................................................................................................ 8 5.2 Steady-state calibration................................................................................................................................ 9 5.2.1 General................................................................................................................................................................ 9 5.2.2 Calibration coefficient

.............................................................................................................................. 10 5.2.3 Time constant

............................................................................................................................................. 10 5.3 Pulse calibration ........................................................................................................................................... 11 5.3.1 General.............................................................................................................................................................. 11 5.3.2 Time constant

............................................................................................................................................. 12 5.4 Determination of the calorimeter parameters .................................................................................. 12 5.5 Improvement of common calibration procedure ............................................................................. 12 6 Sample ............................................................................................................................................................... 13 6.1 General.............................................................................................................................................................. 13 6.2 Test sample ..................................................................................................................................................... 13 6.3 Reference sample .......................................................................................................................................... 13 7 Testing procedure ........................................................................................................................................ 14 7.1 General.............................................................................................................................................................. 14 7.2 Method A - “External mixing”.................................................................................................................... 14 7.3 Method B - “Internal mixing” .................................................................................................................... 14 7.4 Measurement .................................................................................................................................................. 15 7.5 Expression of results ................................................................................................................................... 15 7.6 Test result ........................................................................................................................................................ 16 7.7 Test report ....................................................................................................................................................... 16 8 Precision .......................................................................................................................................................... 17 8.1 Repeatability .................................................................................................................................................. 17 8.2 Reproducibility .............................................................................................................................................. 17

SIST EN 196-11:2019

EN 196-11:2018 (E) 3 European foreword This document (EN 196-11:2018) 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 June 2019, and conflicting national standards shall be withdrawn at the latest by September 2020. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. EN 196 consists of the following parts, under the general title Methods of testing cement: — Part 1: Determination of strength; — Part 2: Chemical analysis of cement; — Part 3: Determination of setting times and soundness; — Part 4: Quantitative determination of constituents (CEN/TR 196-4); — 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. According to the CEN-CENELEC Internal Regulations, the national standards organisations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 196-11:2019

EN 196-11:2018 (E) 4

1 Scope This document specifies the apparatus and procedure for determining the heat of hydration of cements and other hydraulic binders at different test ages by isothermal conduction calorimetry. This test procedure is intended for measuring the heat of hydration of cement up to 7 days in order to obtain correspondence between Isothermal Conduction Calorimetry (ICC) and EN 196-8 and EN 196-9. Nevertheless this test duration may be critical for some apparatus, even if they can work properly at shorter test ages. Contrary to EN 196-8 this method gives the heat of hydration continuously over the time. Additionally, the heat flow versus time is given. 2 Normative references There are no normative references in this document. 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. ISO and IEC maintain terminological databases for use in standardization at the following addresses:

IEC Electropedia: available at http://www.electropedia.org/

ISO Online browsing platform: available at http://www.iso.org/obp 3.1 isothermal conduction calorimeter apparatus able to measure the heat flow generated by a sample kept at constant temperature Note 1 to entry: The constant temperature condition is achieved by maintaining the sample in thermal contact with a heat sink. 3.2 output of calorimeter electric signal from the calorimeter expressed in V 3.3 thermal power heat rate produced by the sample during the test Note 1 to entry: It is commonly expressed, with reference to the unit mass of cement, in W/g or J/(s×g). 3.4 heat time integral of the thermal power and expressed in J/g 3.5 calibration coefficient

ratio between the thermal power produced in the calorimeter and the output of the calorimeter Note 1 to entry: Expressed in W/V. SIST EN 196-11:2019

EN 196-11:2018 (E) 5 3.6 baseline output BO output of the calorimeter when there is an inert sample in the testing and reference cell, both with the same thermal capacity Note 1 to entry: Expressed in V. 3.7 baseline drift BD representation of the slope of the linear regression of the baseline output versus time measured over a specified period Note 1 to entry: It is expressed in W/g per time period, with reference to the unit mass of cement1. The baseline drift measured in V per time period and unit mass of cement, is converted in unit W per time period and unit mass of cement by the calibration coefficient. 3.8 baseline noise BN representation of the standard deviation of the regression of the Baseline output versus time measured over a specified period Note 1 to entry: It is expressed in W/g, with reference to the unit mass of cement. 3.9 testing cell testing ampoule measuring cell specifically dedicated to the sample under test Note 1 to entry: It is the sample that generates heat. 3.10 reference cell reference ampoule measuring cell specifically dedicated to an inert sample Note 1 to entry: It is a sample that doesn’t generate heat and it is used to reduce the BD and BN. 3.11 ampoule container into which the sample is placed for a measurement 3.12 ampoule holder holder into which the ampoule is placed for a measurement Note 1 to entry: The ampoule holder conducts the heat from the sample in the ampoule to the heat flow sensor.

1 The mass of cement to be used is the mass of the sample that will be used for the measurement. SIST EN 196-11:2019

EN 196-11:2018 (E) 6
3.13 time constant

order of magnitude of the time needed to reach the new thermal equilibrium Note 1 to entry: It is a measure of the thermal inertia of the test cell and it is expressed in s. 3.14 detection limit DL minimum value of thermal power that an apparatus is able to detect Note 1 to entry: This value is an estimation of the quality of the measurement that is dependent on the whole measuring chain and not only on the design of the instrument. 4 Apparatus 4.1 General This part gives general requirements related to the relevant properties and design of a calorimeter. Although the design of individual calorimeters from different manufacturers may vary, it should meet the specifications as described below. 4.2 Principle An isothermal heat conduction calorimeter is called “isothermal” as the temperature changes in it (if the instrument and the method are well designed) are so low so that the results are – from a practical point of view – the same as if the measurement had been made at perfectly isothermal conditions. The term is convenient to use here as most other cement calorimeters are (semi-) adiabatic, but it does not imply that the measurements are made under perfectly isothermal conditions. An isothermal heat conduction calorimeter has to consist of a constant-temperature heat sink to which at least two heat-flow sensors and sample holders (calorimetric cells) are attached in a manner resulting in good thermal conductivity. One cell contains the sample of interest and the other one, the reference cell, contains a blank sample that doesn’t evolve heat. If the calorimeter contains more than two cells, at least one has to act as reference cell. Often the conduction calorimeters with more than two cells have own reference cells for each of the sample cells. The cells, including the holder, shall have the same heat capacity on the reference side and on the sample side. This may be realized by adopting the same design and materials on both sides. If an inert sample with similar heat capacity as the sample is charged into the reference ampoule, noise and drift will be substantially decreased (balancing). The heat released by the hydrating cement sample, flows across the sensor into the heat sink. The voltage output from a measurement is the difference between the voltages from the test cell and the reference cell. The heat-flow sensor senses the small temperature gradient that develops across the device. However, the heat is removed from the hydrating sample fast enough that, for practical purposes, the sample remains at a constant temperature (isothermal). SIST EN 196-11:2019

EN 196-11:2018 (E) 7

Key 1 thermostat 2 heat flow sensors 3 heat sink 4 sample 5 reference Figure 1 — Schematic drawing of a heat conduction calorimeter 4.3 Thermostat Although the driving force of heat flow is a temperature gradient, the overall temperature in the calorimeter (heat sink) during test should be essentially constant (isothermal). For this purpose the calorimeter should be equipped with a thermostat. The temperature instability of the thermostat should not exceed 0,2°C. The working temperature of the apparatus should be at (20 ± 0,2) °C. 4.4 Calorimeter technical parameters The technical parameter of the calorimeters that have to be specified to perform the heat of hydration determinations and to ensure an acceptable robustness of the results are the following: — Detection limit (DL); — Baseline noise (BN); — Baseline drift (BD). The calorimeter has to meet the following specifications: — DL: < 2,8 W/g; — BN: < 10,5 W/g; — BD: < 5,5 W/g per week. NOTE The above specifications have been defined on the basis of the technical specifications of the apparatus currently used for calorimetric measurements on hydraulic binders. For the time being there are no experimental data correlating these specifications with

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