Quantitative Energy-Dispersive X-Ray Microanalysis of Chlorine in Cement Paste
Publication: Journal of Materials in Civil Engineering
Volume 28, Issue 1
Abstract
Energy dispersive X-ray spectroscopy (EDS) is a microanalysis technique for material characterization that can provide accurate quantification of elemental composition while maintaining high spatial resolution. EDS microanalysis studies on cementitious materials can face several challenges essentially due to the complex chemical and mineralogical characteristics of cement hydration products. Furthermore, EDS microanalysis is widely carried out in “standardless analysis” mode, which relies on the internal standards of the microanalysis software. This can lead to highly erroneous analysis results because standardless analysis typically normalizes total to 100% without taking chemically bound water into account. In the case of quantifying chlorine content of a cement paste, such normalization is unacceptable because it can lead to overestimation. For accurate determination of elemental concentrations, X-ray spectra collected from minerals or glasses with known chemical compositions are necessary as references. This paper examines the performance of six different minerals containing a wide range of chlorine concentrations as standards for quantitative EDS microanalysis. Also, the influence of experimental conditions such as beam current, accelerating voltage, dwell time, and scanning mode on the obtained results is discussed. It was found that among the minerals investigated, scapolite [(Na,Ca)4(Al3Si9O24)Cl] stands out as the most favorable microanalysis standard for quantifying chlorine content in cement paste.
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Acknowledgments
Financial support by the Dutch Technology Foundation (STW) for the project IS2C 10978-Measuring, Modelling, and Monitoring Chloride ingress and Corrosion initiation in Cracked Concrete (M3C4) is gratefully acknowledged. The authors would like to thank also Mr. Nicholas B. Winter from WHD Microanalysis for interesting discussions on the topic.
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Published In
Journal of Materials in Civil Engineering
Volume 28 • Issue 1 • January 2016
Copyright
© 2015 American Society of Civil Engineers.
History
Received: Jul 21, 2014
Accepted: Mar 16, 2015
Published online: May 15, 2015
Discussion open until: Oct 15, 2015
Published in print: Jan 1, 2016
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