Evaluating Applications of Field Spectroscopy Devices to Fingerprint Commonly Used Construction Materials (2013)

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TRANSPORTATION RESEARCH BOARD WASHINGTON, D.C. 2013 www.TRB.org RepoRt S2-R06B-RR-1 The Second S T R A T E G I C H I G H W A Y R E S E A R C H P R O G R A M Evaluating Applications of Field Spectroscopy Devices to Fingerprint Commonly Used Construction Materials AdAm ZofkA, mAriA ChrysoChoou, iliyA yut, And ChAd Johnston Department of Civil and Environmental Engineering, University of Connecticut montgomery shAw And shih-Po sun Chemical, Materials & Biomolecular Engineering Department, University of Connecticut JAmes mAhoney Connecticut Transportation Institute, University of Connecticut stuArt fArquhArson And miChAel donAhue Real-Time Analyzers, Inc.

Subscriber Categories Construction Highways Materials

SHRP 2 Reports Available by subscription and through the TRB online bookstore: www.TRB.org/bookstore Contact the TRB Business Office: 202-334-3213 More information about SHRP 2: www.TRB.org/SHRP2 SHRP 2 Report S2-R06B-RR-1 ISBN: 978-0-309-12937-4 Library of Congress Control Number: 2013931920 © 2013 National Academy of Sciences. All rights reserved. Copyright Information Authors herein are responsible for the authenticity of their materials and for obtaining written permissions from publishers or persons who own the copy- right to any previously published or copyrighted material used herein. The second Strategic Highway Research Program grants permission to repro- duce material in this publication for classroom and not-for-profit purposes. Per- mission is given with the understanding that none of the material will be used to imply TRB, AASHTO, or FHWA endorsement of a particular product, method, or practice. It is expected that those reproducing material in this document for educational and not-for-profit purposes will give appropriate acknowledgment of the source of any reprinted or reproduced material. For other uses of the material, request permission from SHRP 2. Note: SHRP 2 report numbers convey the program, focus area, project number, and publication format. Report numbers ending in “w” are published as web documents only. Notice The project that is the subject of this report was a part of the second Strategic Highway Research Program, conducted by the Transportation Research Board with the approval of the Governing Board of the National Research Council. The members of the technical committee selected to monitor this project and review this report were chosen for their special competencies and with regard for appropriate balance. The report was reviewed by the technical committee and accepted for publication according to procedures established and overseen by the Transportation Research Board and approved by the Governing Board of the National Research Council. The opinions and conclusions expressed or implied in this report are those of the researchers who performed the research and are not necessarily those of the Trans- portation Research Board, the National Research Council, or the program sponsors. The Transportation Research Board of the National Academies, the National Research Council, and the sponsors of the second Strategic Highway Research Pro- gram do not endorse products or manufacturers. Trade or manufacturers’ names appear herein solely because they are considered essential to the object of the report. The Second Strategic Highway Research Program America’s highway system is critical to meeting the mobility and economic needs of local communities, regions, and the nation. Developments in research and technology—such as advanced materials, communications technology, new data collection technologies, and human factors science—offer a new oppor- tunity to improve the safety and reliability of this important national resource. Breakthrough resolution of significant trans- portation problems, however, requires concentrated resources over a short time frame. Reflecting this need, the second Strategic Highway Research Program (SHRP 2) has an intense, large-scale focus; integrates multiple fields of research and technology; and is fundamentally different from the broad, mission-oriented, discipline-based research programs that have been the mainstay of the highway research industry for half a century. The need for SHRP 2 was identified in TRB Special Report 260: Strategic Highway Research: Saving Lives, Reducing Congestion, Improving Quality of Life, published in 2001 and based on a study sponsored by Congress through the Transportation Equity Act for the 21st Century (TEA-21). SHRP 2, modeled after the first Strategic Highway Research Program, is a focused, time- constrained, management-driven program designed to comple- ment existing highway research programs. SHRP 2 focuses on applied research in four areas: Safety, to prevent or reduce the severity of highway crashes by understanding driver behavior; Renewal, to address the aging infrastructure through rapid design and construction methods that cause minimal disrup- tions and produce lasting facilities; Reliability, to reduce conges- tion through incident reduction, management, response, and mitigation; and Capacity, to integrate mobility, economic, envi- ronmental, and community needs in the planning and designing of new transportation capacity. SHRP 2 was authorized in August 2005 as part of the Safe, Accountable, Flexible, Efficient Transportation Equity Act: A Legacy for Users (SAFETEA-LU). The program is managed by the Transportation Research Board (TRB) on behalf of the National Research Council (NRC). SHRP 2 is conducted under a memorandum of understanding among the American Associa- tion of State Highway and Transportation Officials (AASHTO), the Federal Highway Administration (FHWA), and the National Academy of Sciences, parent organization of TRB and NRC. The program provides for competitive, merit-based selection of research contractors; independent research project oversight; and dissemination of research results.

The National Academy of Sciences is a private, nonprofit, self-perpetuating society of distinguished scholars engaged in scientific and engineering research, dedicated to the furtherance of science and technology and to their use for the general welfare. On the authority of the charter granted to it by Congress in 1863, the Academy has a mandate that requires it to advise the federal government on scientific and technical matters. Dr. Ralph J. Cicerone is president of the National Academy of Sciences. The National Academy of Engineering was established in 1964, under the charter of the National Academy of Sciences, as a parallel organization of outstanding engineers. It is autonomous in its administration and in the selection of its members, sharing with the National Academy of Sciences the responsibility for advising the federal government. The National Academy of Engineering also sponsors engineering programs aimed at meeting national needs, encourages education and research, and recognizes the superior achieve- ments of engineers. Dr. Charles M. Vest is president of the National Academy of Engineering. The Institute of Medicine was established in 1970 by the National Academy of Sciences to secure the services of eminent members of appropriate professions in the examination of policy matters pertaining to the health of the public. The Institute acts under the responsibility given to the National Academy of Sciences by its congressional charter to be an adviser to the federal government and, on its own initiative, to identify issues of medical care, research, and education. Dr. Harvey V. Fineberg is president of the Institute of Medicine. The National Research Council was organized by the National Academy of Sciences in 1916 to associate the broad community of science and technology with the Academy’s purposes of furthering knowledge and advising the federal government. Functioning in accordance with general policies determined by the Academy, the Council has become the principal operating agency of both the National Academy of Sciences and the National Academy of Engineering in providing services to the government, the public, and the scientific and engineering communities. The Council is administered jointly by both Academies and the Institute of Medicine. Dr. Ralph J. Cicerone and Dr. Charles M. Vest are chair and vice chair, respectively, of the National Research Council. The Transportation Research Board is one of six major divisions of the National Research Council. The mission of the Transportation Research Board is to provide leadership in transportation innovation and progress through research and information exchange, conducted within a setting that is objective, interdisci- plinary, and multimodal. The Board’s varied activities annually engage about 7,000 engineers, scientists, and other transportation researchers and practitioners from the public and private sectors and academia, all of whom contribute their expertise in the public interest. The program is supported by state transportation departments, federal agencies including the component administrations of the U.S. Department of Transporta- tion, and other organizations and individuals interested in the development of transportation. www.TRB.org www.national-academies.org

ACKNOWLEDGMENTS This work was sponsored by the Federal Highway Administration in cooperation with the American Asso- ciation of State Highway and Transportation Officials. It was conducted in the second Strategic Highway Research Program, which is administered by the Transportation Research Board of the National Acad- emies. The project was managed by Dr. Monica Starnes, Senior Program Officer for SHRP 2 Renewal. The research reported on herein was performed by the University of Connecticut (UConn), supported by Real-Time Analyzers, Incorporated (RTA, Inc.). Adam Zofka (Assistant Professor, Department of Civil and Environmental Engineering, UConn) was the principal investigator. Maria Chrysochoou (Assistant Professor, Department of Civil and Environmental Engineering, UConn), Montgomery Shaw (Profes- sor of Research, Chemical, Materials & Biomolecular Engineering Department, UConn), James Mahoney (Director, Connecticut Transportation Institute, UConn), Stuart Farquharson (President, RTA, Inc.), and Michael Donahue served as co-principal investigators. Graduate research assistants Iliya Yut and Chad Johnston performed laboratory and field experiments with spectroscopic instruments and also contrib- uted to this report. The authors acknowledge the help of Shi-Po Sun (a former Ph.D. student at the Materi- als & Biomolecular Engineering Department, UConn) and Xiaolong Zhiang (a former Master’s student at the Department of Civil and Environmental Engineering, UConn) for conducting part of the laboratory experiments. The research team is grateful to Fred Morris with Bruker Optics, Inc., for his assistance with the infrared equipment. Innova X Systems and inXitu, Inc. are acknowledged for their contributions to the analysis of X-ray data. Finally, the research team thanks all manufacturers for voluntarily providing samples of their materials. SHRP 2 STAFF Ann M. Brach, Director Stephen J. Andrle, Deputy Director Neil J. Pedersen, Deputy Director, Implementation and Communications James Bryant, Senior Program Officer, Renewal Kenneth Campbell, Chief Program Officer, Safety JoAnn Coleman, Senior Program Assistant, Capacity and Reliability Eduardo Cusicanqui, Financial Officer Walter Diewald, Senior Program Officer, Safety Jerry DiMaggio, Implementation Coordinator Shantia Douglas, Senior Financial Assistant Charles Fay, Senior Program Officer, Safety Carol Ford, Senior Program Assistant, Renewal and Safety Elizabeth Forney, Assistant Editor Jo Allen Gause, Senior Program Officer, Capacity Rosalind Gomes, Accounting/Financial Assistant Abdelmename Hedhli, Visiting Professional James Hedlund, Special Consultant, Safety Coordination Alyssa Hernandez, Reports Coordinator Ralph Hessian, Special Consultant, Capacity and Reliability Andy Horosko, Special Consultant, Safety Field Data Collection William Hyman, Senior Program Officer, Reliability Michael Marazzi, Senior Editorial Assistant Linda Mason, Communications Officer Reena Mathews, Senior Program Officer, Capacity and Reliability Matthew Miller, Program Officer, Capacity and Reliability Michael Miller, Senior Program Assistant, Capacity and Reliability David Plazak, Senior Program Officer, Capacity Monica Starnes, Senior Program Officer, Renewal Onno Tool, Visiting Professional Dean Trackman, Managing Editor Connie Woldu, Administrative Coordinator Patrick Zelinski, Communications/Media Associate

Quality control of materials used during construction is an important issue routinely affect- ing highway agencies across the United States. Evaluating whether the materials delivered at the construction site agree with those specified can be resolved by existing testing techniques. Spectroscopy technologies have recently been used for typical transportation materials on a limited basis but there is the potential for much broader use of these technologies for quality assurance tests. Furthermore, recent advances in the development of portable equipment could allow evaluation of the materials at the construction site before or during their use. This report presents the evaluation of portable spectroscopy devices and their capabilities to “fingerprint” typical construction materials. Fingerprinting of typical materials requires developing acceptable spectra of the specific chemical compositions with laboratory-based equipment and then comparing the material being fingerprinted against those spectra. On the basis of this requirement, the project developed a library of reference spectra for com- mon materials used in highway and road construction. The evaluation of the spectroscopy devices was conducted through laboratory testing and field testing. Field testing verified the feasibility of field quality assurance/quality control procedures for the material–testing method combinations found successful in the labora- tory research phase. From this work the project also developed relatively simple and easy- to-use nondestructive testing procedures and protocols that inspectors could use in the field to ensure quality construction. An additional phase was recently added to this project to develop specifications and pilot them in collaboration with two transportation agencies. Once completed, the results from this additional scope of work will be published as an addendum to this report. F O R EWO R D Monica A. Starnes, Ph.D., SHRP 2 Senior Program Officer, Renewal

C O N T E N T S 1 Executive Summary 5 CHAPTER 1 Background 5 Renewal Focus Area 5 Problem Statement 5 Research Objectives 6 CHAPTER 2 Methodology 6 Literature Review 6 Surveys and Workshop 6 Development of Testing Matrix 7 Laboratory Analyses 7 Field Verification 7 Data Analysis Methods 8 Repeatability and Reproducibility of Test Results 8 Project Deliverables 9 References 10 CHAPTER 3 Findings and Applications 10 Review of Spectroscopic Applications to Construction Materials 13 Survey and Workshop Results 15 Fingerprinting of Pure Materials 18 Identification and Quantification of Additives and Contaminants in Complex Materials 32 Reliability of Portable Spectroscopic Measurements 36 Field Verification of Laboratory Results 38 Summary of Technical Performance of Portable Instruments 38 Reference 39 CHAPTER 4 Conclusions and Suggested Research 39 Applicability of Portable Spectroscopic Equipment to Field Evaluation of Construction Materials 40 Project Deliverables 40 Further Research 41 Appendix A Laboratory Equipment and Testing Protocols 56 Appendix B Generic Spectroscopic Testing Procedures 60 Appendix C Proposed AASHTO Standards of Practice 67 Appendix D Field Operation Manuals 71 Appendix E Literature Review

89 Appendix F Summary of Preliminary Survey and Workshop 94 Appendix G Field Needs Survey 109 Appendix H Links to Material Safety Data Sheet 111 Appendix I ATR FTIR Spectra 125 Appendix J Raman Spectra 142 Appendix K XRF Data 162 Appendix L GPC Chromatograms 177 Appendix M NMR Spectra 204 Appendix N Quantitative Analysis of ATR FTIR Spectra 207 Appendix O Quantitative Analysis of GPC and NMR Data 212 Appendix P Reliability of Spectroscopic Measurements 228 Appendix Q Field Verification Results