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Measurement of the chemical composition, phase abundance, and microstructure of cementitious materials is an increasingly important prerequisite for mixture design, quality control, and troubleshooting of concrete materials. This workshop will provide practical information and guidance on performing chemical and phase analyses of portland cement and portland cement clinker materials, including hands-on practice with analyzing real data. The workshop will address several complementary methods but will focus especially on quantitative X-ray powder diffraction (XRD) and quantitative scanning electron microscopy (SEM) for characterizing unhydrated materials.
Topics
- Quantitative X-ray Powder Diffraction (QXRD): Theoretical basis, instrumentation, specimen preparation, measurement artifacts and sources of error, internal and external standards, interpretation, and detection limits.
- Quantitative Scanning Electron Microscopy (QSEM): Theoretical basis, instrumentation, backscattered electron imaging, X-ray microprobe analysis, measurement artifacts and sources of error, image analysis, phase segmentation, advantages and disadvantages compared to QXRD, and microstructure characterization.
- Practicums on QXRD and QSEM: Participants will receive a complete set of cement-related raw material data sets obtained on portland cement powders, and will be given step-by-step guidance on analyzing the data to quantify the chemical composition and phase abundance using freely available software in the public domain.
- Principles and Applications of
- X-Ray fluorescence spectrometry (XRF)
- Surface topographical analysis
- Solution composition analysis
Who Should Attend
The workshop assumes a general familiarity with concrete materials, but no specialized knowledge of materials characterization is required. Engineers, research scientists, and technicians responsible for cementitious materials characterization, quality control, or testing should find this workshop beneficial for their continuing education and professional development.
Hardware and Software Requirements
To participate in the practicums, each participant should bring a laptop computer (Windows or Mac) with the following free public domain software packages and data files downloaded and installed prior to the workshop:
- ImageJ: download at http://imagej.nih.gov/ij/download.html (link is external)
- MultiSpec©: download at https://engineering.purdue.edu/~biehl/MultiSpec/ (link is external)
- Profex: download at http://profex.doebelin.org/ (link is external)
- MicroChar: download at https://www.nist.gov/services-resources/software/microchar/
- XRD instrument and crystal structure data files: Workshop-2017-XRD.zip
- SEM image data: Workshop-2017-SEM.zip
Brief instructions are provided below for downloading and installing the software. Please consult your system administrator about permissions or other security settings that may prevent you from successfully installing the software.
Other software and material data sets may be provided at the workshop.
Workshop Lecture Slides
Presentation slides may be downloaded here: Workshop-Lectures.zip
- The final agenda is now available.
- Paul Stutzman, Steve Feldman, Jeff Bullard, Alex Brand, LaKesha Perry (NIST)
- Don Broton (CTLGroup)
About the Speakers
Paul Stutzman is a physical scientist in the Inorganic Materials Group of the Materials and Structural Systems Division of the Engineering Laboratory (EL) at the National Institute of Standards and Technology (NIST). His interests include measurement of microstructural features of clinker, cement, and mineral admixtures and developing means to assess the interactions of cement – admixtures on the hydration process through real-time quantitative x-ray powder diffraction and scanning electron microscopy. Paul is a member of ASTM C1 (Cement) and C9 (Concrete) chairs the Compositional Analysis Committee Task Groups on Microscopy and Quantitative X-Ray Powder Diffraction Methods. He is also a member of the C1 Executive Committee and C1 Secretary, and is on the Editorial Board of the ASTM Journal Advances in Civil Engineering Materials. In 2013 Paul was named a Fellow of ASTM and received their International Award of Merit for distinguished service and outstanding participation. Paul received a NIST Bronze award in 2008 for efforts in developing and promoting a powder diffraction method for compositional analysis of cements within ASTM. In 1992 and in 2008, he received the P. H. Bates Award for outstanding papers, "Cement Clinker Characterization by Scanning Electron Microscopy" and "Phase Analysis of Hydraulic Cements by X-Ray Powder Diffraction: Precision, Bias, and Qualification."
Steve Feldman is a Materials Research Engineer at the National Institute of Standards and Technology (NIST) working on improving measurement techniques for determining the state and rate of alkali-silica reaction in nuclear concrete structures. Before coming to NIST in 2015, he worked as Chief Mineralogist for Barrick Gold Corporation, Director of Research for Active Minerals International, LLC, and in consulting activities for academia, major corporations, and regulatory agencies associated primarily with the minerals, petrochemical, and cement/concrete industries. He is the author of a total of 33 published articles including 2 refereed book chapters, 2 published soil survey reports, 14 reports on original research, 4 refereed technical reports, and 5 patents. He received M.S. and Ph.D. degrees in Clay Mineralogy and Soil Physical Chemistry from Virginia Tech.
Jeff Bullard is a materials research engineer in the Inorganic Materials Group (IMG) of the Materials and Structural Systems Division (MSSD) of the Engineering Laboratory (EL) at the National Institute of Standards and Technology (NIST). Dr. Bullard joined the IMG in April 2002. He is working on the application of thermodynamics, chemical kinetics, and digital-image modeling methods to simulate microstructure development during hydration or degradation of cement pastes and concrete. Dr. Bullard is a principal researcher for the Virtual Cement and Concrete Laboratory (VCCTL) Consortium, which was established in 2001 to provide a collaborative research partnership, between NIST and industrial members, for developing and validating computer modeling software for rapid design and optimization of cement and concrete materials. He was a co-recipient of a 2009 Silver Medal Award from the Department of Commerce for hydration modeling research related to VCCTL. He received the NIST Engineering Laboratory's Communication Award in 2008 and 2010 for technical publications that clarified the mechanism of cement hydration. He is a recipient of the 2011 Stephen Brunauer Award for best paper on cement published by the American Ceramic Society. In 2014 he was elected as a Fellow of the American Ceramic Society, and in 2017 he was elected as a Fellow of the Washington Academy of Sciences.
Alex Brand is an NRC Postdoctoral Associate at NIST, where his research is focused on characterizing the kinetics of reactions between cementitious mineral surfaces and water. He received a Ph.D. in Civil and Environmental Engineering from the University of Illinois at Urbana-Champaign in 2016.
LaKesha Perry is a physical scientist in the Inorganic Materials Group and the Polymeric Materials Group within NIST's Engineering Laboratory. She is an expert in the compositional analysis of solutions and the characterization of polymeric material degradation.
Don Broton has been analyzing cement and related geological materials for nearly 30 years. His primary field of interest is the analysis and evaluation of industrial materials using XRF and XRD methods as well as concrete “reverse composition analysis.” He is chair of ASTM C 01.23 on cement analysis and serves on many other sub-committees for cement, concrete and lime and mortar. He has performed analyses that led to the certification of many cements, limestone, silica fume and gypsum standard reference material for NIST. He also serves on the Denver X-ray Conference Organizing Committee and International Cement Microscopy Organizing committee.
Holiday Inn Gaithersburg
Two Montgomery Village Avenue
Gaithersburg, MD 20878
(301) 948-8900
Group Code: NCC
$125/night Book by June 27, 2017
Includes complimentary shuttle service to and from NIST
If you are not registered, you will not be allowed on site. Registered attendees will receive security and campus instructions prior to the workshop.
NON U.S. CITIZENS PLEASE NOTE: All foreign national visitors who do not have permanent resident status must be prepared to supply additional information during registration. Authority to gather this information is derived from United States Department of Commerce Department Administrative Order (DAO) number 207-12.
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Acceptable Photo Identification:
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For US Permanent Residents: Permanent Resident/Green card for photo identification