CEN/TC 51/WG 15 - Revision of methods of testing cement

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.

This European Standard describes three methods of determining the fineness of cement.
The sieving method serves only to demonstrate the presence of coarse cement particles. This method is primarily suited to checking and controlling the production process.
The air-jet sieving method measures the retention on sieving and is suitable for particles which substantially pass a 2,0 mm test sieve. It may be used to determine the particle size distribution of agglomerates of very fine particles. This method may be used with test sieves in a range of aperture sizes, e.g. 63 μm and 90 μm.
The air permeability method (Blaine) measures the specific surface area (mass related surface area) by comparison with a reference material sample. The determination of the specific surface area serves primarily to check the consistency of the grinding process of one and the same plant. This method only enables a limited assessment of the properties of the cement in use.
NOTE   The air permeability method may not give significant results for cements containing ultrafine materials.
The methods are applicable to all the cements defined in EN 197.

This document describes the analytical procedures used to determine the content of C3A in the clinker starting from a chemical analysis on cement. The method can be applied to CEM type I and IV for the determination of the requirement of C3A, as defined on EN 197 1.
This document describes two methods, traditional wet and XRF analysis (EN 196 2), which can be considered to be equivalent, in the scope of this CEN/TR 17365, for the determination of Al2O3, Fe2O3 and SO3.
The same methods are described in EN 196 2, but for the scope of this document, the X-ray fluorescence (XRF) is the preferred method to be used for the determination of Al2O3, Fe2O3 and SO3.

This European Standard specifies methods for the determination of the total organic carbon content (TOC) in limestone.
The standard describes the reference method and alternative methods which can be considered to be equivalent.
In the case of a dispute, only the reference method is used.
Any other methods may be used provided they are calibrated, either against the reference method or against internationally accepted reference materials, in order to demonstrate their equivalence.

This part of EN 196 specifies the method for the determination of the water-soluble chromium (VI) content of cement.
A reference method is described consisting of two stages, an extraction procedure and an analysis of the filtered extract. Guidance on other extraction procedures, suitable for screening tests, for factory production control or other purposes, is given but in case of dispute or failure to comply with a regulatory limit only the reference method is used. The reference method has alternatives whereby the filtered extract may be subjected to an oxidation step or not. The criteria by which the appropriate procedure is selected are set down. Other instrumental procedures may be used for the analysis of the filtered extract provided they are calibrated against the analysis of the filtered extract using the reference procedure. In the case of a dispute, only the reference method is used.
Annex A sets out a normative procedure to be followed in case this test method is used as the basis for evaluation of conformity of a cement with the regulatory limit in Regulation (EC) 1907/2006 .
This part of EN 196 describes a method that applies to cements. It may have wider applicability but this would need to be verified by testing on a product-by-product basis. Guidance in the possible application of this European Standard to the determination of the water-soluble chromium (VI) content of cement-containing preparations is given in Annex B.
Annexes C and D provide information on other test procedures based on paste extraction and thus depart from the performance of cement in its normal conditions of use. They may be carried out with or without the oxidation process. Users should be aware that results using these methods might be significantly different to those obtained by the reference method. In the case of dispute or failure to comply with the regulatory limit only the reference method is used.
Annex E provides guidance on a method for determination of the excess reducing agent content of cement as used in the factory internal control system of some countries. Manufacturers using such an internal control method should ensure themselves of the relevance of results in comparison with testing by the reference method.

This European Standard specifies the methods for determining standard consistence, setting times and soundness of cements.
The method applies to common cements and to other cements and materials, the standards for which call up this method. It may not apply to other cement types that have, for example, a very short initial setting time. The method is used for assessing whether the setting time and soundness of a cement is in conformity with its specification.
This part of EN 196 describes the reference methods and allows the use of alternative procedures and equipment, as indicated in notes, provided that they have been calibrated against the reference methods. In the event of a dispute, only the reference equipment and procedures are used.

This part of EN 196 describes the method for the determination of the compressive and, optionally, the flexural strength of cement mortar. The method applies to common cements and to other cements and materials, the standards for which call up this method. It may not apply to other cement types that have, for example, a very short initial setting time.
The method is used for assessing whether the compressive strength of cement is in conformity with its specification and for validation testing of a CEN Standard sand, EN 196 1, or alternative compaction equipment.
This part of EN 196 describes the reference equipment and procedure and allows alternative compaction equipment and procedures to be used provided that they have been validated in accordance with the appropriate provisions in this document. In the event of a dispute, only the reference equipment and procedure are used.

This European Standard specifies the methods for the chemical analysis of cement.
This document describes the reference methods and, in certain cases, an alternative method which can be considered to be equivalent. In the case of a dispute, only the reference methods are used.
An alternative performance-based method using X-ray fluorescence (XRF) is described for SiO2, Al2O3, Fe2O3, CaO, MgO, SO3, K2O, Na2O, TiO2, P2O5, Mn2O3, SrO, Cl and Br. When correctly calibrated according to the specified procedures and reference materials, it provides a method equivalent to the reference methods but has not been validated for use yet as a reference procedure for conformity and dispute purposes. It can be applied to other relevant elements when adequate calibrations have been established. This method is based on beads of fused sample and analytical validation using certified reference materials, together with performance criteria. A method based on pressed pellets of un-fused sample can be considered as equivalent, providing that the analytical performance satisfies the same criteria.
Any other methods may be used provided they are calibrated, either against the reference methods or against internationally accepted reference materials, in order to demonstrate their equivalence.
This document describes methods which apply principally to cements, but which can also be applied to their constituent materials. They can also be applied to other materials, the standards for which call up these methods. Standard specifications state which methods are to be used.

This European Standard specifies the method of measuring the pozzolanicity of pozzolanic cements conforming to [1] EN 197-1. This standard does not apply to Portland pozzolana cements or to pozzolanas.
This method constitutes the reference procedure.

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 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).

This European Standard describes the equipment to be used, the methods to be followed and the provisions for taking samples of cement, representative of given lots for testing, to assess the quality of products prior to, during or after delivery.
The provisions of this standard are only applicable when samples of cement are:
a)   required for evaluating the conformity of a cement at any time with a standard; or
b)   requested for checking a delivery or a lot with a standard, the provisions of a contract or the specification in an order.
The standard is applicable to the taking of samples of all types of cements defined by European Standards for cements whether they are:
c)   contained in silos;
d)   contained in bags, canisters, drums or any other packages;
e)   transported in bulk in road vehicles, railway wagons, ships, etc.
NOTE   The requirements of this standard can also, by agreement between the parties, be followed for acceptance inspections for all non-standardized hydraulic binders.

This European Technical Report describes procedures for determining the contents of most of the constituents of the cements that fall within the scope of EN 197-1.
In principle, the method described in Clause 6 applies to all cements, whatever the number and nature of their constituents, but in practice is limited to the cements identified in Table 1.
The method in clause 6 should be considered to be the method of choice and is based on a sequential selective dissolution of the cement’s constituents, generally of an unknown number, where they are not available separately for analysis at the same time as the cement.
The method of choice enables the quantitative determination (by mass) of: Portland cement clinker, blastfurnace slag, siliceous fly ash, natural pozzolans, limestone, silica fume and set regulators in cements of the types identified in Table 1. Table 1 is derived from Table 1 of EN 197-1.
NOTE 1   Where cements contain calcareous fly ash, burnt shale and/or constituents that partly contain mineral phases, similar to those of clinker, further investigation into the characteristics of those constituents will be necessary before the method can be applied.
The method of choice has limitations, as indicated earlier, and cannot be considered to be a means by which clinker content can simply be determined in isolation from any other constituent. Clinker content is determined ‘by difference’ and other constituents contain, in part, mineral phases similar to those present in clinker and can cause interferences that lead to difficulties in interpretation of the results.
Where apparently anomalous results are obtained, it is recommended that further investigations are undertaken in accordance with the procedure given in Section 6.2.5.4.
Any other method with the same objectives, and intended for use where the constituents are unavailable for separate analysis, can be considered to be an alternative to the method of choice when it is shown that, with appropr

This document specifies the methods for the chemical analysis of cement.
This document describes the reference methods and, in certain cases, an alternative method which can be considered to be equivalent. In the case of a dispute, only the reference methods are used.
An alternative performance-based method using X-ray fluorescence (XRF) is described for SiO2, Al2O3, Fe2O3, CaO, MgO, SO3, K2O, Na2O, TiO2, P2O5, Mn2O3, SrO, Cl and Br. This method is based on beads of fused sample and analytical validation using certified reference materials, together with performance criteria. A method based on pressed pellets of un-fused sample can be considered as equivalent, providing that the analytical performance satisfies the same criteria.
An alternative performance-based method using inductively coupled plasma optical emission spectroscopy (ICP-OES) is described for SO3.
When correctly calibrated according to the specified procedures and reference materials, XRF and ICP-OES provides methods equivalent to the reference methods but has not been validated for use yet as a reference procedure for conformity and dispute purposes. They can be applied to other relevant elements when adequate calibrations have been established.
Any other methods can be used provided they are calibrated, either against the reference methods or against internationally accepted reference materials, in order to demonstrate their equivalence.
This document describes methods which apply principally to cements, but which can also be applied to their constituent materials. They can also be applied to other materials, the standards for which call up these methods. Standard specifications state which methods are to be used.

This document specifies two equivalent test methods to assess the chemical reactivity of a pozzolanic or latent hydraulic cement constituent or concrete addition by measurements of heat of hydration (see Clause 5 and 8.3 Method A, Heat of Hydration) or bound water content (see Clause 5 and 8.4 Method B, Bound Water Content) of hydrated pastes composed of the cement constituent or concrete addition, calcium hydroxide, calcium carbonate, potassium sulfate, and potassium hydroxide cured at 40 °C for 72 h and 168 h (3 days and 7 days).
These two test methods measure chemical reactivity of test specimens intended for use as cementitious materials, such as cement constituents and concrete additions. The test methods do not distinguish between latent hydraulic and pozzolanic reactivity.
The test methods are used for qualification purposes if the cement constituents or concrete additions are tested at the fineness as specified by the respective product standards. In the absence of a product standard or a specification in the product standard, the constituents are tested at the fineness of the intended use.
NOTE   In case the test methods are used for purposes of comparison of intrinsic reactivity, cement constituents are tested at similar fineness, where possible.
The test methods are also used for testing other new constituents that are latent hydraulic or pozzolanic and that are not covered by EN 197 series product standards. However, for such new constituents the validity of the underlying correlations with strength development have not been verified; in consequence the test results can only be used for informative and indicative purposes.
Furthermore, these test methods are used in manufacturing control of cement constituents for assessing their latent hydraulic or pozzolanic reactivity.

This European Standard describes three methods of determining the fineness of cement.  
La présente Norme européenne décrit trois méthodes de détermination de la finesse du ciment.
La méthode par tamisage sert uniquement à détecter la présence de grosses particules de ciment. Cette méthode d’essai convient avant tout à la vérification et au contrôle du procédé de production.
La méthode par tamisage à jet d’air mesure le refus de tamisage et convient aux particules qui passent effectivement à travers un tamis d’essai de dimension d’ouverture 2,0 mm et elle peut être utilisée pour déterminer la granulométrie des grumeaux constitués de particules très fines. Cette méthode fait appel à des tamis d’essais dans une série d’ouverture, par exemple, 63 µm et 90 µm..
La méthode de perméabilité à l’air (Blaine) mesure la surface spécifique par comparaison avec un échantillon d’un ciment de référence. La détermination de la surface spécifique sert avant tout à vérifier la constance du procédé de broyage d’une seule et même installation. Cette méthode ne permet qu’un jugement limité des propriétés du ciment utilisé.
NOTE : La méthode de perméabilité à l’air peut ne pas donner des résultats significatif pour les ciments qui contiennent des matières ultrafines
Les méthodes sont applicables à tous les ciments définis dans l’EN 197.

This document specifies the methods for determining standard consistence, setting times and soundness of cements.
The method applies to common cements and to other cements and materials, the standards for which call up this method. It may not apply to other cement types that have, for example, a very short initial setting time. The method is used for assessing whether the setting time and soundness of a cement is in conformity with its specification.
This document describes the reference methods and allows the use of alternative procedures and equipment, as indicated in notes, provided that they have been calibrated against the reference methods. In the event of a dispute, only the reference equipment and procedures are used.

This European Standard specifies the method for the determination of the water-soluble chromium (VI) content of cement.
A reference method is described consisting of two stages, an extraction procedure and an analysis of the filtered extract. Guidance on other extraction procedures, suitable for screening tests, for factory production control or other purposes, is given but in case of dispute or failure to comply with a regulatory limit only the reference method is used. The reference method has alternatives whereby the filtered extract may be subjected to an oxidation step or not. The criteria by which the appropriate procedure is selected are set down. Other instrumental procedures may be used for the analysis of the filtered extract provided they are calibrated against the analysis of the filtered extract using the reference procedure. In the case of a dispute, only the reference method is used.
Annex A sets out a normative procedure to be followed in case this test method is used as the basis for evaluation of conformity of a cement with the regulatory limit in Directive 2003/53/EC.
This European Standard describes a method that applies to cements. It may have wider applicability but this would need to be verified by testing on a product-by-product basis. Guidance in the possible application of this European Standard to the determination of the water-soluble chromium (VI) content of cement-containing preparations is given in Annex B.
Annexes C and D provide information on other test procedures based on paste extraction and thus depart from the performance of cement in its normal conditions of use. They may be carried out with or without the oxidation process. Users should be aware that results using these methods might be significantly different to those obtained by the reference method. In the case of dispute or failure to comply with the regulatory limit only the reference method is used.

This document describes the method for the determination of the compressive and, optionally, the flexural strength of cement mortar. The method applies to common cements and to other cements and materials, the standards for which call up this method. It may not apply to other cement types that have, for example, a very short initial setting time.
The method is used for assessing whether the compressive strength of cement is in conformity with its specification and for validation testing of a CEN Standard sand, EN 196-1, or alternative compaction equipment.
This document describes the reference equipment and procedure and allows alternative compaction equipment and procedures to be used provided that they have been validated in accordance with the appropriate provisions in this document. In the event of a dispute, only the reference equipment and procedure are used.

This document specifies the methods for the chemical analysis of cement.
This document describes the reference methods and, in certain cases, an alternative method which can be considered to be equivalent. In the case of a dispute, only the reference methods are used.
Any other methods may be used provided they are calibrated, either against the reference methods or against internationally accepted reference materials, in order to demonstrate their equivalence.
This document describes methods which apply principally to cements, but which can also be applied to their constituent materials. They can also be applied to other materials, the standards for which call up these methods.
Standard specifications state which methods are used.

This document specifies the method of measuring the pozzolanicity of pozzolanic cements conforming to EN 197-1. This document does not apply to Portland pozzolana cements or to pozzolanas.
This method constitutes the reference procedure.

This document specifies the methods for determining standard consistence, setting times and soundness of cements.
The method applies to common cements and to other cements and materials, the standards for which call up this method. It may not apply to other cement types that have, for example, a very short initial setting time. The method is used for assessing whether the setting time and soundness of a cement is in conformity with its specification.
This document describes the reference methods and allows the use of alternative procedures and equipment, as indicated in notes, provided that they have been calibrated against the reference methods. In the event of a dispute, only the reference equipment and procedures are used.