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1.1 This guide provides information for the examination of hardened concrete using scanning electron microscopy (SEM) combined with energy-dispersive X-ray spectroscopy (EDX). Since the 1960s, SEM has been used for the examination of concrete and has proved to be an insightful tool for the microstructural analysis of concrete and its components. There are no standardized procedures for the SEM analysis of concrete. SEM supplements techniques of light microscopy, which are described in Practice C856, and, when applicable, techniques described in Practice C856 should be consulted for SEM analysis. For further study, see the bibliography at the end of this guide.
This guide is intended to provide a general introduction to the application of SEM/EDS analytical techniques for the examination and analysis of concrete. It is meant to be useful to engineers and scientists who want to study concrete and who are familiar with, but not expert in, the operation and application of SEM/EDS technology. The guide is not intended to provide explicit instructions concerning the operation of this technology or interpretation of information obtained through SEM/EDS.
It is critical that petrographer or operator or both be familiar with the SEM/EDX equipment, specimen preparation procedures, and the use of other appropriate procedures for this purpose. This guide does not discuss data interpretation. Proper data interpretation is best done by individuals knowledgeable about the significance and limitations of SEM/EDX and the materials being evaluated.
1.2 The SEM provides images that can range in scale from a low magnification (for example, 15×) to a high magnification (for example, 50 000× or greater) of concrete specimens such as fragments, polished surfaces, or powders. These images can provide information indicating compositional or topographical variations in the observed specimen. The EDX system can be used to qualitatively or quantitatively determine the elemental composition of very small volumes intersecting the surface of the observed specimen (for example, 1-10 cubic microns) and those measured compositional determinations can be correlated with specific features observed in the SEM image. See Note 1.
Note 1—An electronic document consisting of electron micrographs and EDX spectra illustrating the materials, reaction products, and phenomena discussed below is available at http://netfiles.uiuc.edu/dlange/www/CML/index.html.
1.3 Performance of SEM and EDX analyses on hardened concrete specimens can, in some cases, present unique challenges not normally encountered with other materials analyzed using the same techniques.
1.4 This guide can be used to assist a concrete petrographer in performing or interpreting SEM and EDX analyses in a manner that maximizes the usefulness of these techniques in conducting petrographic examinations of concrete and other cementitious materials, such as mortar and stucco. For a more in-depth, comprehensive tutorial on scanning electron microscopy or the petrographic examination of concrete and concrete-related materials, the reader is directed to the additional publications referenced in the bibliography section of this guide.
1.5 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with the use of electron microscopes, X-ray spectrometers, chemicals, and equipment used to prepare samples for electron microscopy. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
2. Referenced Documents (purchase separately) The documents listed below are referenced within the subject standard but are not provided as part of the standard.
C125 Terminology Relating to Concrete and Concrete Aggregates
C294 Descriptive Nomenclature for Constituents of Concrete Aggregates
C295 Guide for Petrographic Examination of Aggregates for Concrete
C457 Test Method for Microscopical Determination of Parameters of the Air-Void System in Hardened Concrete
C856 Practice for Petrographic Examination of Hardened Concrete
C1356 Test Method for Quantitative Determination of Phases in Portland Cement Clinker by Microscopical Point-Count Procedure
ICS Number Code 91.100.30 (Concrete and concrete products)
UNSPSC Code 30111500(Concrete and mortars)