SIST EN 196-8:2010
(Main)Methods of testing cement - Part 8: Heat of hydration - Solution method
Methods of testing cement - Part 8: Heat of hydration - Solution method
This European Standard describes a method of determining the heat of hydration of cements by means of solution calorimetry, also known as the solution method. The heat of hydration is expressed in joules per gram of cement.
This standard is applicable to cements and hydraulic binders whatever their chemical composition.
NOTE 1 Another procedure, called the semi-adiabatic method, is described in EN 196-9. Either procedure can be used independently.
NOTE 2 It has been demonstrated that the best correlation between the two methods is obtained at 7 days for the solution method (EN 196-8) compared with 41 h for the semi-adiabatic method (EN 196-9).
Prüfverfahren für Zement - Teil 8: Hydratationswärme - Lösungsverfahren
Diese Europäische Norm beschreibt ein Verfahren zur Messung der Hydratationswärme von Zementen mit Hilfe eines Lösungskalorimeters, das so genannte Lösungsverfahren. Die Hydratationswärme wird in Joule je Gramm Zement angegeben.
Diese Europäische Norm gilt für Zemente und hydraulische Bindemittel, ungeachtet ihrer chemischen Zusammen¬setzung.
ANMERKUNG 1 Ein anderes Verfahren, das so genannte teiladiabatische Verfahren, ist in EN 196-9 beschrieben. Beide Verfahren können unabhängig voneinander angewendet werden.
ANMERKUNG 2 Es wurde nachgewiesen, dass sich die beste Korrelation zwischen den beiden Verfahren nach 7 Tagen bei Hydratation nach dem Lösungsverfahren (EN 196-8) und nach 41 h bei Hydratation nach dem teiladiabatischen Verfahren (EN 196-9) ergibt.
Méthodes d'essais des ciments - Partie 8: Chaleur d'hydratation - Méthode par dissolution
La présente norme européenne décrit une méthode de mesure de la chaleur d’hydratation des ciments par
calorimétrie de dissolution, appelée méthode par dissolution. La chaleur d’hydratation est exprimée en joules
par gramme de ciment.
La présente norme s’applique aux ciments et aux liants hydrauliques quelle que soit leur composition
chimique.
NOTE 1 Une autre méthode, dite méthode semi-adiabatique, est décrite dans la norme EN 196-9. Les deux
méthodes peuvent être utilisées indépendamment.
NOTE 2 Il a été démontré que la meilleure corrélation entre les deux méthodes est obtenue en comparant les valeurs
à 7 jours par la méthode par dissolution (EN 196-8) et à 41 heures par la méthode semi-adiabatique (EN 196-9).
Metode preskušanja cementa - 8. del: Toplota hidratacije - Metoda raztapljanja
Ta evropski standard opisuje metodo za določanje toplote hidratacije cementov s pomočjo kalorimetrije raztapljanja, ki je znana tudi kot metoda raztapljana. Toplota hidratacije je izražena v joulih na gram cementa. Ta standard velja za cemente in hidravlična veziva, ne glede na njihovo kemično sestavo.
General Information
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Metode preskušanja cementa - 8. del: Toplota hidratacije - Metoda raztapljanjaPrüfverfahren für Zement - Teil 8: Hydratationswärme - LösungsverfahrenMethods of testing cement - Part 8: Heat of hydration - Solution method91.100.10Cement. Mavec. Apno. MaltaCement. Gypsum. Lime. MortarICS:Ta slovenski standard je istoveten z:EN 196-8:2010SIST EN 196-8:2010en,fr,de01-junij-2010SIST EN 196-8:2010SLOVENSKI
STANDARDSIST EN 196-8:20041DGRPHãþD
SIST EN 196-8:2010
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 196-8
March 2010 ICS 91.100.10 Supersedes EN 196-8:2003English Version
Methods of testing cement - Part 8: Heat of hydration - Solution method
Prüfverfahren für Zement - Teil 8: Hydratationswärme - Lösungsverfahren 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 196-8:2010: ESIST EN 196-8:2010
EN 196-8:2010 (E) 2 Contents Page Foreword . 31Scope . 42Normative references . 43Principle . 44Materials . 44.1Acid mixture . 44.2Zinc oxide (ZnO) . 54.3Anhydrous cement . 54.4Hydrated cement . 55Apparatus . 56Calorimeter calibration . 76.1Principle . 76.2Procedure . 76.3Calculation of calibration characteristics . 86.3.1Corrected temperature increase, ∆∆∆∆Tc . 86.3.2Thermal leakage coefficient, K . 86.3.3Thermal capacity, C . 87Determination of heat of solution . 97.1Heat of solution of anhydrous cement . 97.1.1Procedure . 97.1.2Calculation . 107.1.3Expression of results . 107.2Heat of solution of hydrated cement . 117.2.1Procedure . 117.2.2Correction for bound water . 117.2.3Calculation . 117.2.4Expression of results . 128Heat of hydration . 138.1Calculation of results . 138.2Reporting of results . 138.3Precision . 138.3.1Repeatability . 138.3.2Reproducibility . 13Bibliography . 14
SIST EN 196-8:2010
EN 196-8:2010 (E) 3 Foreword This document (EN 196-8:2010) 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 196-8:2003. 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 196-8:2010
EN 196-8:2010 (E) 4 1 Scope This European Standard describes a method of determining the heat of hydration of cements by means of solution calorimetry, also known as the solution method. The heat of hydration is expressed in joules per gram of cement. This standard is applicable to cements and hydraulic binders whatever their chemical composition. NOTE 1 Another procedure, called the semi-adiabatic method, is described in EN 196-9. Either procedure can be used independently. NOTE 2 It has been demonstrated that the best correlation between the two methods is obtained at seven days for the solution method (EN 196-8) compared with 41 h for the semi-adiabatic method (EN 196-9). 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 197-1:2000, Cement — Part 1: Composition, specifications and conformity criteria for common cements 3 Principle The method consists in measuring the heats of solution, in an acid mixture, of anhydrous cement and cement hydrated under standardized conditions for a predetermined period of time, e.g. seven days. These standardized hydration conditions are as follows: water/cement ratio 0,40; use of neat cement paste; storage at constant temperature of (20,0 ± 0,2) °C during the whole hydration process. The heat of hydration for each period, Hi, is obtained from the difference between the heat of solution of anhydrous cement, Qa, and that of hydrated cement, Qi. 4 Materials 4.1 Acid mixture Analytical reagent quality acid mixture, obtained by adding 2,760 g of 40 % hydrofluoric acid (HF) for every 100,0 g of (2,00 ± 0,01) mol/l nitric acid (HNO3), or 2,600 ml of hydrofluoric acid for every 100,0 ml of nitric acid. WARNING — Hydrofluoric acid can cause painful skin burns which heal only with difficulty and precautions in handling this very corrosive substance should be strictly observed. The quantity (mass or volume) of acid to be used, which is common to all tests, shall be measured to ± 0,2 %. SIST EN 196-8:2010
EN 196-8:2010 (E) 5 4.2 Zinc oxide (ZnO) Use zinc oxide of analytical quality to determine the thermal capacity of the calorimeter. Weigh 40 g to 50 g. Ignite at (950 ± 25) °C for 1 h. Cool in a desiccator. Grind to pass a 125 µm sieve. Store in a desiccator. 4.3 Anhydrous cement Store anhydrous cement, from which metallic iron has been removed with a magnet, in a sealed container to avoid absorption of water or carbon dioxide. Bring the test sample to ambient temperature and carefully homogenize it before use. 4.4 Hydrated cement Prepare the hydrated cement test sample by vigorously mixing, either manually or mechanically, (100,0 ± 0,1) g of anhydrous cement with (40,0 ± 0,1) g of distilled or deionised water for 3 min at ambient temperature. Place the resulting paste in plastics or glass cylindrical vials (three for each hydration period to be tested) so that each vial contains 15 g to 20 g of material. Seal the vials by means of a stopper and, if necessary, with paraffin wax or similar material and store them horizontally in a thermostatic bath maintained at a temperature of (20,0 ± 0,2) °C. 5 Apparatus 5.1 Calorimeter. NOTE The method does not deal with the standardization of the calorimetric apparatus, or the measuring instruments. Insulated flasks with a volume of about 650 ml have proved to be suitable. A suitable calorimeter (see Figure 1) comprises the following: a) Dissolution vessel, consisting of: an insulated flask (e.g. Dewar flask), placed either in a heat insulated container set inside a box constructed of insulating material (e.g. wood, plastics), or immersed in a thermostatic water bath regulated to ± 0,2 °C; and an insulated stopper (made of cork or plastics) through which holes are provided for the thermometer, the stirrer and the funnel used for introducing the sample. The insulation of the calorimeter shall ensure that the thermal leakage coefficient, K (determined in accordance with 6.3), is less than 0,06 K per 15 min for each Kelvin above ambient temperature. The internal surface of the flask, that part of the thermometer immersed in the acid mixture and the lower part of the stopper, shall be acid mixture resistant. b) Thermometer, either a Beckmann thermometer with a 5 °C to 6 °C scale and subdivisions every 0,01 °C or other measurement apparatus of an equal or higher accuracy such as a thermistor or platinum resistance thermometer, positioned such that the end of the thermometer is at least 4 cm below the level of the liquid surface. Express temperature readings with a resolution of ± 0,002 °C. Adjust the zero of the Beckmann thermometer so that the upper limit of the scale is approximately the ambient, or water bath, temperature. Calibrate the thermometer in a thermostatic bath against a 0,01 °C graduated and calibrated thermometer. c) Funnel, of acid mixture resistant plastics, through which the sample is introduced into the flask and which extends below the lower part of the stopper by 5 mm to 6 mm and is sealed during the test. d) Stirrer, of acid mixture resistant plastics, positioned such that the blades are as close as possible to the bottom of the flask and rotated by a motor at a speed of (450 ± 50) min-1. The motor shall be low power rated (e.g. a motor of a few watts) so as to prevent any excessive heat e
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Metode preskušanja cementa - 8. del: Toplota hidratacije - Metoda raztapljanjaPrüfverfahren für Zement - Teil 8: Hydratationswärme - LösungsverfahrenMethods of testing cement - Part 8: Heat of hydration - Solution method91.100.10Cement. Mavec. Apno. MaltaCement. Gypsum. Lime. MortarICS:Ta slovenski standard je istoveten z:FprEN 196-8kSIST FprEN 196-8:2009en,fr,de01-oktober-2009kSIST FprEN 196-8:2009SLOVENSKI
STANDARD
kSIST FprEN 196-8:2009
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
FINAL DRAFT
FprEN 196-8
August 2009 ICS 91.100.10 Will supersede EN 196-8:2003English Version
Methods of testing cement - Part 8: Heat of hydration - Solution method
Prüfverfahren für Zement - Teil 8: Hydratationswärme - Lösungsverfahren 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 196-8:2009: EkSIST FprEN 196-8:2009
FprEN 196-8:2009 (E) 2 Contents page Foreword . 41Scope. 52Normative references . 53Principle . 54Materials . 54.1Acid mixture . 54.2Zinc oxide (ZnO) . 64.3Anhydrous cement . 64.4Hydrated cement . 65Apparatus . 65.1Calorimeter . 66Calorimeter calibration . 86.1Principle . 86.2Procedure . 86.3Calculation of calibration characteristics. 96.3.1Corrected temperature increase, ∆∆∆∆Tc. . 96.3.2Thermal leakage coefficient, K . 96.3.3Thermal capacity, C . 97Determination of heat of solution . 107.1Heat of solution of anhydrous cement . 107.1.1Procedure . 107.1.2Calculation . 117.1.3Expression of results. 127.2Heat of solution of hydrated cement . 127.2.1Procedure . 127.2.2Correction for bound water . 127.2.3Calculation . 137.2.4Expression of results. 148Heat of hydration . 148.1Calculation of results . 148.2Reporting of results . 148.3Precision . 148.3.1Repeatability . 14kSIST FprEN 196-8:2009
FprEN 196-8:2009 (E) 3 8.3.2Reproducibility . 14Bibliography . 15
kSIST FprEN 196-8:2009
FprEN 196-8:2009 (E) 4 Foreword This document (FprEN 196-8:2009) 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 196-8:2003. 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 196-8:2009
FprEN 196-8:2009 (E) 5 1 Scope This European Standard describes a method of determining the heat of hydration of cements by means of solution calorimetry, also known as the solution method. The heat of hydration is expressed in joules per gram of cement. This standard is applicable to cements and hydraulic binders whatever their chemical composition. NOTE 1 Another procedure, called the semi-adiabatic method, is described in EN 196-9. Either procedure can be used independently. NOTE 2 It has been demonstrated that the best correlation between the two methods is obtained at 7 days for the solution method (EN 196-8) compared with 41 h for the semi-adiabatic method (EN 196-9). 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 197-1, Cement — Part 1: Composition, specifications and conformity criteria for common cements 3 Principle The method consists in measuring the heats of solution, in an acid mixture, of anhydrous cement and cement hydrated under standardized conditions for a predetermined period of time, e.g. 7 days. These standardized hydration conditions are as follows: water/cement ratio 0,40; use of neat cement paste; storage at constant temperature of (20,0 ± 0,2) °C during the whole hydration process. The heat of hydration for each period, Hi, is obtained from the difference between the heat of solution of anhydrous cement, Qa, and that of hydrated cement, Qi. 4 Materials 4.1 Acid mixture Analytical reagent quality acid mixture, obtained by adding 2,760 g of 40 % hydrofluoric acid (HF) for every 100,0 g of (2,00 ± 0,01) mol/l nitric acid (HNO3), or 2,600 ml of hydrofluoric acid for every 100,0 ml of nitric acid. WARNING Hydrofluoric acid can cause painful skin burns which heal only with difficulty and precautions in handling this very corrosive substance should be strictly observed. The quantity (mass or volume) of acid to be used, which is common to all tests, shall be measured to ± 0,2 %. kSIST FprEN 196-8:2009
FprEN 196-8:2009 (E) 6 4.2 Zinc oxide (ZnO) Use zinc oxide of analytical quality to determine the thermal capacity of the calorimeter. Weigh 40 g to 50 g. Ignite at (950 ± 25) °C for one hour. Cool in a desiccator. Grind to pass a 125 µm sieve. Store in a desiccator. 4.3 Anhydrous cement Store anhydrous cement, from which metallic iron has been removed with a magnet, in a sealed container to avoid absorption of water or carbon dioxide. Bring the test sample to ambient temperature and carefully homogenize it before use. 4.4 Hydrated cement Prepare the hydrated cement test sample by vigorously mixing, either manually or mechanically, (100,0 ± 0,1) g of anhydrous cement with (40,0 ± 0,1) g of distilled or deionised water for 3 min at ambient temperature. Place the resulting paste in plastics or glass cylindrical vials (three for each hydration period to be tested) so that each vial contains 15 g to 20 g of material. Seal the vials by means of a stopper and, if necessary, with paraffin wax or similar material and store them horizontally in a thermostatic bath maintained at a temperature of (20,0 ± 0,2) °C. 5 Apparatus 5.1 Calorimeter NOTE The method does not deal with the standardization of the calorimetric apparatus, or the measuring instruments. Insulated flasks with a volume of about 650 ml have proved to be suitable. A suitable calorimeter (see Figure 1) comprises the following: a) Dissolution vessel, consisting of: an insulated flask (eg. Dewar flask), placed either in a heat insulated container set inside a box constructed of insulating material (e.g. wood, plastics), or immersed in a thermostatic water bath regulated to ± 0,2 °C; and an insulated stopper (made of cork or plastics) through which holes are provided for the thermometer, the stirrer and the funnel used for introducing the sample. The insulation of the calorimeter shall ensure that the thermal leakage coefficient, K, (determined in accordance with 6.3) is less than 0,06 kelvins per 15 min for each kelvin above ambient temperature. The internal surface of the flask, that part of the thermometer immersed in the acid mixture and the lower part of the stopper, shall be acid mixture resistant. b) Thermometer, either a Beckmann thermometer with a 5 °C to 6 °C scale and subdivisions every 0,01 °C or other measurement apparatus of an equal or higher accuracy such as a thermistor or platinum resistance thermometer, positioned such that the end of the thermometer is at least 4 cm below the level of the liquid surface. Express temperature readings with a resolution of ± 0,002 °C. Adjust the zero of the Beckmann thermometer so that the upper limit of the scale is approximately the ambient, or water bath, temperature. Calibrate the thermometer in a thermostatic bath against a 0,01 °C graduated and calibrated thermometer. c) Funnel, of acid mixture resistant plastics, through which the sample is introduced into the flask and which extends below the lower part of the stopper by 5 mm to 6 mm and is sealed during the test. d) Stirrer, of acid mixture resistant plastics, positioned such that the blades are as close as possible to the bottom of the flask and rotated by a motor at a speed of (450 ± 50) min -1. The motor shall kSIST FprEN 196-8:2009
FprEN 196-8:2009 (E) 7 be low power rated (e.g. a motor of a few watts) so as to prevent any excessive heat emission from affecting measurements. 125749610832111
Key
1
flask 5
thermometer 9
insulating material 2
container 6
stirrer 10
flask support 3
box 7
funnel 11
ambient thermometer 4
stopper 8
support 12
stirrer motor Figure 1 — Typical heat of solution calorimeter apparatus kSIST FprEN 196-8:2009
FprEN 196-8:2009 (E) 8 5.2 Thermostatic bath, e.g. water bath, for storing the hydrated samples at a temperature of (20,0 ± 0,2) °C. 5.3 Mortar or electric grinder, for crushing the hydrated samples. 5.4 Plastics or glass vials, of c
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