ISO/TC 74 - Cement and lime

ISO 29581-2:2010 describes a performance-based method for the chemical analysis of cement for SiO2, Al2O3, Fe2O3, CaO, MgO, SO3, K2O, Na2O, TiO2, P2O5, Mn2O3, SrO, Cl and Br using X-ray fluorescence (XRF). It can be applied to other relevant elements when adequate calibrations have been established. ISO 29581-2:2010 describes an alternative method for analyses of cement for conformity and information purposes, based on beads of fused sample and analytical validation using certified reference materials, together with performance criteria. A method based on pressed pellets of unfused sample can be considered as equivalent, providing that the analytical performance satisfies the same criteria. The use of fused beads generally improves the accuracy of analysis for non-volatile elements since it eliminates variability arising from differences in mineralogical forms or oxidation states. Pressed pellets generally improve the accuracy of analysis for volatile elements and can give adequate accuracy for the routine analysis of non-volatile elements. The presence of sulfide in a sample also leads to restrictions on the scope of the analysis that can be undertaken using the XRF technique based upon fused beads. In particular, sulfate (SO3) cannot be determined directly from such a fused bead because of the contribution to the analysis from the unknown amount of sulfide. In addition, sulfide cannot be determined directly (or accurately, indirectly) because of the contribution of the unknown amount of sulfate to the analysis and from the possibility that some sulfide can be lost by volatilization during fusion. Consequently, the method of ISO 29581-1, included as Annex D of ISO 29581-2:2010, is the reference method for determining the sulfate content of samples containing sulfide species. Other methods can be used, provided they are calibrated, either against the reference method or against internationally accepted reference materials, in order to demonstrate their equivalence. In the case of dispute, unless otherwise agreed by all parties, only the reference method in ISO 29581-1 can be used. ISO 29581-2:2010 describes methods that apply principally to cements, but which can also be applied to their constituent materials and to other materials, the standards for which call up these methods.

ISO 29582-1:2009 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. ISO 29582-1:2009 is applicable to cements and hydraulic binders whatever their chemical composition.

ISO 679:2009 specifies a method of determining the compressive and, optionally, the flexural strength of cement mortar containing one part by mass of cement, three parts by mass of ISO standard sand and one half part of water. ISO 679:2009 applies to common cements and to other cements and materials, the standards for which call up this method. ISO 679:2009 might not apply to other cement types that have, for example, a very short initial setting time. ISO 679:2009 describes the reference equipment and procedure and specifies the method used for validation testing of ISO standard sands and of alternative equipment and procedures.

ISO/TS 12389:2009 describes the results of the inter-laboratory testing of the chemical analysis of cement by x-ray fluorescence. In the first instance, the inter-laboratory testing was carried out in Japan and Asian countries in accordance with JIS R 5204:2002. A total of 30 laboratories, 16 in Japan and 14 outside Japan, participated in the original testing programme. A further 12 European laboratories participated in tests with the same materials in 2005 in accordance with EN 196-2, a development by CEN/TC 51/WG 15/TG 1 of JIS R 5204. The latest version, developed as ISO 29581-2, is, as of the date of publication of this Technical Report, in the process of being circulated for technical enquiry. The test samples used were Portland cement conforming to CEM I of EN 197-1 and a mixture of Portland cement and blast furnace slag. The mixture corresponded to the composition of Portland blast furnace slag cement, class B, specified in JIS R 5211 and CEM III/A of EN 197-1. Cement reference materials for x-ray fluorescence analysis (No. 601A) are used for the calibration standards, and certified reference materials JCA-CRM-1 and JCA-CRM-2 are used as the validation materials. Constituents analysed include SiO2, Al2O3, Fe2O3, CaO, MgO, SO3, Na2O, K2O, TiO2, P2O5, MnO and SrO. The loss on ignition is also determined. The ISO round robin is a method-performance study conducted under close to optimum conditions with clear calibration and measurement guidelines. This is conducive to producing “best practice” values representative of the ideal situation. However, ISO 29581-2 is intended for use under everyday conditions in laboratories that operate to “good practice”. The results are presented for some international round robins carried out by a large number of laboratories demonstrating the suitability of ISO 29581-2 as a means for comparing the everyday performance of laboratories.

ISO 29581-1:2009 specifies the methods for the analysis of cement by wet chemistry. ISO 29581-1:2009 gives the reference methods and, in certain cases, an alternative method that can be considered to be equivalent. In the case of a dispute, only the reference methods are used. It is permitted to use other methods provided they are calibrated, either against the reference methods or against internationally accepted reference materials, in order to demonstrate their equivalence. In case of dispute, only the reference methods are used. ISO 29581-1:2009 describes methods that 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.

ISO 863:2008 describes the method of measuring the pozzolanicity of pozzolanic cements. It does not apply to Portland pozzolana cements or to pozzolanas. ISO 863:2008 constitutes the reference procedure.

ISO 9597:2008 specifies the methods for determining standard consistence, setting times and soundness of cements. ISO 9597:2008 applies to common cements and to other cements and materials, the standards for which call up this method. It might 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. ISO 9597:2008 describes the reference methods and allows the use of alternative procedures and equipment, as indicated, provided that they have been calibrated against the reference methods. In the event of a dispute, only the reference equipment and procedures described in ISO 9597:2008 can be used, excluding any alternatives.

ISO 29582-2:2009 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. ISO 29582-2:2009 is applicable to all cements and hydraulic binders, whatever their chemical composition, with the exception of quick-setting cements.

Describes the procedures for the chemical analysis of cement. Gives the reference procedures and, in certain cases, an alternative method which can be considered as giving equivalent results. Applies to cements, and also to their constituent materials such as clinker and blastfurnace slag.

Describes the reference procedure. The setting time is determined by observing the penetration of a needle into cement paste of standard consistence until it reaches a specified value. The soundness is determined by observing the volume expansion of cement paste of standard consistence as indicated by the relative movement of two needles.

Specifies a method of determining the compressive and flexural strengths of cement mortar and describes the reference procedure. Allows the use of alternative procedures only in well defined cases. Covers laboratory and equipment, mortar constituents, preparation of mortar and test specimens, curing of test specimens, and test procedures.