University Research Consortium Annual Review Meeting Program

LOCKHEED MARTIN/ Idaho National Engineering Laboratory University Research Consortium Annual Review Meeting Program

Universities Idaho National Engineering Laboratory

Industries IWASTI

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This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufac- turer, or otherwise does not necessarily constitute or imply its endorsement, recom- mendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof. INEL-96/0253 July 1996

LOCKHEED MARTIN^

University Research Consortium Annual Program Review Meeting

July 29-31,1996 Idaho Falls Center for Higher Education Idaho Falls, Idaho

Idaho National Engineering Laboratoiy elcome to the First Annual Program Review meeting of the Idaho National Engineering Laboratory University Research Consortium (INEL/URC). Although our primary purpose is to review the progress of the research, we have structured the Annual Review to enable other important objectives. For those" participants who have never visited the INEL, the meeting is an opportunity to become more familiar with the unique resources of the multiprogram National Laboratory, and to strengthen the research ties we have initiated through the URC Program. Conversely, it is an opportunity for INEL Scientists to become more familiar with the objectives and content of the URC Program.

A significant effort has been invested to make this meeting a productive one for participants. In addition to the Research Project Evaluation Committee and presenters already acknowledged in this Program, I would like to thank and acknowledge the following contributors:

INEL MIT A. B. Denison, Consulting Scientist Professor Mujid S. Kazimi W. J. Toth, Advisory Scientist Dr. Malcolm A. "Weiss R. C. Wilcox, Secretary Professor Jefferson W. Tester T. D. Dixon, Associate Administrator Professor Kenneth A. Smith D. R. Pack, Consulting Administrative Specialist Professor Michael Golay M. I. Valle, Administrative Specialist Professor Thomas W. Eagar B. L. Tracy, Secretary Karen Luxton Bus Operations, Technical Publications, and Printing

Idaho Falls Center for Higher Education Dr. Fred Rose and staff

—Debonny L. Shoaf, Ph.D., Manager Academic and Professional Affairs Department

This project is funded by the Idaho National Engineering Laboratory University Research Consortium. The INEL is managed by Lockheed Martin Idaho Technologies Company for the United States Department of Energy, Idaho Operations Office under Contract DE-AC07-9411D13223." DISCLAIMER

Portions of this document may be illegible in electronic image products. Images are produced from the best available original document. University Research Consortium

Contents

Welcome iv Keynote Speaker v Biographies vi Schedule ix The Consortium Program 1 Universities Conducting URC-Funded Research during FY 1996 .. : 3 Consortium Member Universities as of July 1996 3 Session 1: Biological Processes 5 Session 2: Materials Synthesis 15 Session 3: Reactor Performance, Degradation, and Regulation 25 Session 4: Structures 35 Session 5: Nuclear Medicine Accelerators and Isotopes 43 Session 6: Waste Processing at High Temperatures 55 Session 7: Organic Waste Treatment and Reduction 67 Session 8: Advanced Reactor Technologies 77 Session 9: Site Monitoring and Characterization 85 Session 10: Environmental Sensors and Monitors 93 Session 11: Materials Processing and Control 103 Session 12: Membrane and Adsorption Separation 113 Index of Principal Investigators and Presenters 123

Idaho National Engineering Laboratory iv University Research Consortium

Idaho National Engineering Laboiatoiy University Research Consortium

eynote Speaker Leon M. Lederman as had a long and distinguished career in science and science education, receiving numerous awards and honors. He has been one of the primary explorers in both high-energy physics and the weak interaction. Lederman was awarded the Nobel Prize in Physics (1988) for show- ing the existence of two types of neutri- nos, a key to understanding the weak interaction. He was Director of the Fermi National Accelerator Laboratory from 1979 until 1989. It was here that he and his fellow scientists discovered the fundamental bottom quark for which he was awarded the Wolf Prize in 1983. In 1993 he was presented the Enrico Fermi Prize by President Clinton. He is a supporter of the strength of the United States and its economy through technological innovation. During his term as Director, Lederman emphasized the importance of math and science education. He initiated the Saturday Morning Physics lectures and subse- quently founded the Friends of Fermilab, the Illinois Mathematics and Science Academy, and the Teachers Academy for Mathematics and Science. Dr. Lederman is no stranger to Idaho and the Idaho National Engineering Laboratory. He actively participated in the Idaho Schol- arship Olympics program and was one of the key members in the Prime Program, a workshop for junior high school teachers in the area.

Idaho National Engineering Laboratory VI University Research Consortium John M. Wilcynski Manager, U. S. Department of Energy Idaho Operations Office

John M. Wilcynski became Manager of the U. S. Department of Energy's Operations Office in October of 1994. In this position he directs the activities of the Idaho National Engineering Laboratory (INEL), an operation with approximately 8500 employees and an annual budget of $760M. The missions of the INEL include nuclear reactor research and development, environmental restoration (including waste management and remediation and technology development), and a broad suite of technological research and development programs. Mr Wilcynski has had a long line of key management and administrative experience in the Federal Government. Prior to his present position (October 1991 to October 1994) he was Deputy Manager of the Idaho Operations (1990-1991) and has served as Assistant Manager for Administration at the INEL. At the Richland Operations Office of the U. S. Department of Energy, he served as Director of the Human Resources and Planning Division (1986-1990) and for the period 1981-1985 he was Director of the Procurement Division and the Chief of the Contract Management Branch in the Richland Operations Office. Through 1988, Mr Wilcynski served on a developmental assignment in the Office of Assistant Secretary for Defense Programs in "Washington, D.C. He is a graduate, with honors, from the Boston University Graduate School of Management and Business and has a Bachelors degree in mathematics from Gonzaga University in Spokane, Washington. He completed the Department of Energy Senior Executive Service Candi- date Program, and in 1991 he completed the Program for Senior Managers in Govern- ment at Harvard University.

Warren E. Bergholz Jr. Deputy Manager, U. S. Department of Energy Idaho Operations Office

Warren E. Bergholz, Jr. comes to the Department of Energy's Idaho Operations Office from the DOE's Savannah River Office where he was chief legal counsel. Bergholz sees his role at the INEL as assisting the Idaho Operations Manager, John Wilcynski, in ensuring that die INEL develops new missions while cost-effectively carrying out its existing environmental, national defense, and science and technology roles. As chief counsel at Savanna River, his responsibilities included management of the office's legal functions and providing legal advice and counsel to the manager and senior staff. Bergholz began his federal service in 1976 at the Energy Research and Development Administration headquarters in Wash- ington, D.C. as an attorney in the Office of the General Counsel. He was named deputy assistant general counsel for international development and defense programs in 1982. Bergholz graduated from the University of Pittsburgh and served as an officer in the Navy. He attended the University of Wyoming, where he received his law degree, and he is a member of the Wyoming Bar Association.

Idaho National Engineering Laboratory University Research Consortium vu W.JOHN DENSON President, Lockheed Martin Idaho Technologies Company As President of Lockheed Martin Idaho Technologies Company, W. John Denson brings to the INEL 34 years of experience in managing large complex technical programs. His responsibilities at Lockheed Martin Idaho include providing strategic direction, leadership, and management for all INEL programs, its activities, and employees. Prior to-coming to the INEL, he was presi-

t , dent ofthe Lockheed Environmental Systems & Technologies Company (1992-1994), where he was responsible for the company's DOE, EPA, and commercial environmental engineering, reme- \ * diation, and analytical laboratory operations. Much ofhis career was dedicated to management of * aerospace and space exploration technologies related to Lockheed's responsibility to NASA. From / jjj 1989 through 1992, Denson was program manager for the Shutde Avionics Integration Laboratory at Johnson Space Laboratory, which provided the baseline for NASA to certify the space shutde for initial flight. In 1981, he was program development director to lead the corporation's bid to win the Shutde Processing Contract at Kennedy Space Center. Following that (1982), he became vice president of Lockheed Space Operations Company. Denson earned his bachelor's degree from Mississippi State University in I960 and has taken a number of advanced engineering courses at Rice University, Lockheed, and Ford Aerospace.

Dr. Barton "Bart" Krawetz Director, Idaho National Engineering Laboratory

Dr. Krawerz came to Lockheed Martin Idaho Technologies Company after Lockheed won the contract to manage the INEL in 1993. His responsibilities include planning, evaluating, and managing large complex research and applied engineering development programs for Lockheed Martin and the U.S. government. Prior to joining Lockheed Martin Idaho, Krawetz was vice president of engineering for Lockheed Corporation headquarters, where he developed science and engineering policies and processes, evaluated technical programs, and assisted with problem solving and improving cost effectiveness of engineering across the corporation. From 1987 to 1990, he served as executive vice president and general manager for research, technology, and engineering for the Lockheed Aeronautical Systems Company. Krawetz was vice president and assistant general manager of Lockheed's Skunk Works in 1986 and 1987, assisting with overall management of highly classified research and development of new technologies and prototypes for the U.S. government. For nearly 20 years prior to joining Lockheed, Krawetz held various positions and responsibilities for the U.S. Air Force, primarily with its laboratories. Krawetz has a doctorate in applied science from the University of California, Davis; a master's degree in space physics from the Air Force Institute of Technology at Wright-Patterson Air Force Base; and a bachelor's degree in electrical engineering from the Massachusetts Institute of Technology.

Dr. David P. Caufrman Chief Scientist and Director of Research Products, Lockheed Martin Idaho Technologies

Dr. David P. Caufrman serves as Chief Scientist and Director of Research Products for Lockheed Martin Idaho Technologies Company. As Chief Scientist, he is direcdy responsible for the University Research Consortium, and directs the laboratory discretionary research programs. From 1979 to 1994, Dr. Caufrman was with Lockheed Missiles and Space Company, where for the last six of these years he was manager of the Solar and Astrophysics Laboratory in the company's Palo Alto Research Laboratories. He has directed a number of satellite projects involved in examining the electromagnetic radiation in our solar system. His specialty has been the study of electric fields and plasma convection in the earth's magnetosphere. As program scientist, Dr. Caufrman served for five years (1974-1979) in the Space Plasma Physics Section of the Space Science Division of NASA Headquarters in Washington, D.C., where he played an active role in formulating and gaining approval for a number of unmanned scientific research satellite missions. Dr. Caufrman earned a Ph.D. in space physics from the University of Iowa in 1971, and a BA degree in physics from Haverford College in 1966.

Idaho National Engineering Laboratory viii University Research Consortium

Idaho National Engineering Laboratory University Research Consortium IX

Schedule

Monday, July 29, 1996 9:00 -11:00 a.m. INEL Research Center tours (buses departing form AmeriTel Inn 8:15 a.m.) 11:00 a.m.-1:30 p.m. Registration and INEL and University exhibits (lobby, University Place) 1:30 p.m. Plenary Session (University Place Auditorium) David P. Cauffinan, Chief Scientist, Lockheed Martin Idaho Technologies Company W. John Denson, Lockheed Martin Idaho Barton Krawetz, Lockheed Martin Idaho Jefferson W. Tester, Massachusetts Institute of Technology Warren E. Bergholz, DOE-ID 3:00 p.m. - 4:30 Keynote Address: Leon M. Lederman, Fermi National Accelerator Laboratory 4:30 p.m. Adjourn Plenary Assembly 5:30 p.m. Research Collaboration Meeting, Holiday Inn Westbank

Tuesday, July 30, 1996 8:00 a.m. Three concurrent review sessions 8:00 -11:30 a.m. Session 1: Biological Processes (Tester, Winston) 8:00-11:30 a.m. Session 2: Materials Synthesis (Flemings, Seydel) 8:00-11:30 a.m. Session 3: Reactor Performance, Degradation, and Regulation (Kazimi, Bennett) 11:30 a.m. Lunch 1:00 p.m. Three concurrent review sessions 1:00-4:30 p.m. Session 4: Structures (Flemings, Seydel) 1:00-5:30 p.m. Session 5: Nuclear Medicine Accelerators and Isotopes (Golay, Bennett) 1:00-5:15 p.m. Session 6: Waste Processing at High Temperatures (Smith, Miller) 6:00 p.m. Bus departs form AmeriTel Inn for Mountain River Ranch for dinner 6:30 p.m. Chuckwagon dinner

Wednesday, July 31, 1996 8:00 a.m. Three concurrent review sessions 8:00-11:30 a.m. Session 7: Organic Waste Treatment and Reduction (Smith, Miller) 8:00-11:30 a.m. Session 8: Advanced Reactor Technologies (Golay, Bennett) 8:00-11:30 a.m. Session 9: Site Monitoring and Characterization (Tester, Winston) 11:30 a.m. Lunch 1:00 p.m. Three concurrent review sessions 1:00 - 5:15 p.m. Session 10: Environmental Sensors and Monitors (Tester, Winston) 1:00-5:00 p.m. Session 11: Materials Processing and Control (Hatton, Seydel) 1:00-4:30 p.m. Session 12: Membrane and Adsorption Separation (Smith, Miller)

Idaho National Engineering Laboratory University Research Consortium

Idaho National Engineering Laboratory The Consortium Program

This brochure presents the pro- full formal proposals were extended to selection process. There is now a total gram for the first annual review meet- 133 prospectus writers. Of those proof 15 members of the consortium, listed ing of the University Research Consor- posals, 47 were awarded funds totaling on page 3. tium (URC) of the Idaho National $7.63 million in fiscal 1996, distrib- Although the first purpose of this Engineering Laboratory (INEL). INEL uted among 23 universities in 17 states, annual review meeting is to report and is a multiprogram laboratory with a listed on page 3. The solicitation and evaluate progress on each of the pro- distinctive role in applied engineering. peer review process was managed for jects, there is another important pur- It also conducts basic science research INEL by a team at die Massachusetts pose. That is, the meeting provides an and development, and complex facility Institute of Technology (MIT). Ulti- opportunity for faculty, industry, and operations. INEL addresses national mate funding decisions were made by INEL experts to meet each other in an needs by applying expertise in environ- Lockheed Martin Idaho management informal setting that can encourage mental management research (for after considering the recommendations new and fruitful collaborations for example, pollution prevention, waste of an Oversight Board that included additional work that furthers the mis- remediation, and waste management); representatives of Lockheed Martin sions and business objectives of INEL. applied engineering, and systems inte- Idaho, MIT, and DOE. Those recom- gration; nuclear operations and materials mendations were based both on techni- The general format of the meeting disposition; and transfer of derived-use cal merit of the proposals and on dieir consists of a plenary assembly on Mon- technologies (energy and environmental). relevance to INEL objectives. day afternoon followed by twelve review sessions on Tuesday and In 1994, the U.S. Department of Of the £7 current projects, 25 Wednesday; three sessions will run con- Energy (DOE) selected Lockheed began work on July 1, 1995, and the currendy throughout the two days. Martin Idaho Technologies Company remaining 22 on December 1, 1995. Each session covers three to five pro- to manage the Laboratory. Lockheed Therefore, this review covers research jects on a common topic. Each session Martin Idaho established the URC on projects that have been under way has an MIT faculty chairman, an INEL when it assumed management responsi- for only about half a year, or a year at co-chairman, and at least two other bility. The purpose of the URC is to most. panelists to participate in evaluating the help" INEL in its reorientation to new In late 1995, universities in the projects. One of those panelists is an goals set by DOE for its national labo- Intermountain region were invited to INEL director or his designee, and the ratories. Those goals include develop- join as official members of the URC. other is on die faculty of a Consortium ing new technologies useful in our Our expectation is mat Consortium member university. competitive economy or in meeting members will advise INEL on fruitful In this program, summaries and national needs such as environmental research topics for future solicitation management. participant lists for each project are and funding, and will participate more presented as received from the principal The URC program consists of a actively in the proposal review and investigators. They may be found in portfolio of research projects funded by INEL and conducted at universities in the United States. In order to help reorient the Laboratory and to ensure Questions about the Consortium are welcome. commercial relevance, each project is For information you may communicate with eidier MIT or INEL: intended to have at least one active collaborator on the INEL staff, and at . INEL URC Program Office Dr. Debonny L. Shoaf, Manager least one active collaborator from the Energy Laboratory, Room E40-391 Academic and Professional Affairs private sector; INEL collaboration has Massachusetts Institute of Technology Department not yet been fully realized because of Cambridge, MA 02139-4307 Lockheed Martin Idaho Technologies funding limitations. Company Phone: (617)253-1402 Current URC projects are the out- PO Box 1625 Fax: (617)253-8531 come of a solicitation and review Idaho Falls, ID 83415-2214 e-mail: [email protected] process that began in February 1995. Phone: (208)526-0430 In response to a published solicitation, Fax: (208)526-5327 620 prospectuses (3-page informal proposals) were received from 80 universi- e-mail: [email protected] ties in 41 states. Invitations to submit

Idaho National Engineering Laboratory University Research Consortium the pages immediately following the blank, leaving space for your notes. An schedule for the session in which that index at the end of this program lists project is reported. Many pages facing the principal investigators and report the project summaries are deliberately presenters for each of the 47 projects.

Idaho National Engineering Laboratory University Research Consortium

Universities Conducting URC- Consortium Member Universities Funded Research during FY 1996 as of July 1996

Colorado Colorado Colorado School of Mines Colorado School of Mines Georgia Colorado State University Institute of Paper Science and Technology Idaho University of Colorado Idaho State University Idaho University of Idaho Boise State University Illinois Idaho State University University of Illinois University of Idaho Indiana Massachusetts Purdue University University of Notre Dame* Massachusetts Institute of Technology Massachusetts Montana Harvard University* Montana State University Massachusetts Institute of Technology Montana Technology of the University of Montana Minnesota University of Montana University of Minnesota Utah Missouri University of Missouri* Brigham Young University Montana University of Utah Montana State University Utah State University New York Washington State University of New York-Stony Brook Washington State University North Carolina Wyoming North Carolina State University Rhode Island University of Wyoming Brown University* South Carolina This university is collaborating with another listed uni- Clemson University versity that holds the primary subcontract with the URC. Texas Texas A&M University* Utah Brigham Young University University of Utah Utah State University Vermont University of Vermont Washington University of Washington Washington State University

* This university is collaborating with another listed university that holds the primary subcontract with the URC.

Idaho National Engineering Laboratory University Research Consortium

Idaho National Engineering Laboratoty University Research Consortium

Session 1. Biological Processes

Tuesday, 8:00 a.m. to 11:30 a.m.'

Jefferson ~W. Tester (MIT), chair Rebecca A. Winston (INEL), co-chair Dale R. Ralston (U of I), panelist Bob Snelling, Shirley Sandoz (INEL), panelists

8:00 a.m. V220 James N. Petersen Development of Techniques for Bioremediation of Soil Washington State University and Groundwater Contaminated wida Toxic Heavy Metal Ions

8:45 a.m. V258 Ernest L. Brannon Fish Farm Effluent Treatment for Improving Wastewater University of Idaho Quality

9:30 a.m. — Break

10:00 a.m. V07 Ronald L. Crawford In Situ Biological Destruction of Nitroaromatic University of Idaho Contaminants in Groundwater

10:50 a.m. V177 Mary E. Watwood Specific Labeling of Microorganisms Capable of Idaho State University Oxidative Biotransformation of Toxic Chlorinated Ethylenes widi Enzyme-Activated Chemical Probes

11:30 a.m. Adjourn

Idaho National Engineering Laboratory University Research Consortium

Development of Techniques for Bioremediation of Soil and terize the sorption characteristics of a Groundwater Contaminated with Toxic Heavy Metal Ions (V220) cell immobilization matrix that will be used in later portions of the work, and (b) develop methods which will James N. Petersen, "Washington State University allow the bacterial systems used to accomplish contaminant reduction to Co-PIs and University: be characterized. In the latter, techniques that will allow the determina- David R. Yonge and Donald L. Johnstone, tion of the concentration of dead and Washington State University live biomass, and the determination of the level of nitrite reductase activi- Postdoctoral Research Associates: ty in the cell broth are being devel- Yared Bereded-Samuel, Mahesh Rege oped. The activity of this enzyme is important because it has been impli- Research Associate: David Mills cated by others as the biological catalyst responsible for reducing the cont- Graduate Students: Chris Johnson, Donny Mendoza, 11m Ross, Eric aminants to less hazardous states. Schmeiman, Dyane Sonier During the next year, the follow- Industrial Collaborators and Companies: Carl E. Camp, DuPont Central ing milestones will be met: Research & Development; Brian Peters, Foster Wheeler Environmental An Invention Disclosure describ- Corp.; Charles L. Meyer, Shell Development Company; Paul T. Sun, ing a method devised to biologically Shell Development Company reduce contaminants and then sepa- INEL Collaborators: William A. Apel, Ms. Joni Barnes, rate the reduced material from a process stream will be filed by Charles Turick 10/1/96. Presenter: James N. Petersen All experiments needed to determine the kinetics of contaminant reduction with common bacteria will be completed by 1/9/97. Contamination of subsurface tion of kinetic expressions needed to groundwaters and process wastewaters facilitate the design of ex situ reactors At its quarterly meeting on by toxic and/or mutagenic mineral and in situ remediation strategies. 1/10/97, the project team will deter- and metal ions is widespread. One Experiments will then be performed mine the target waste site for Cr technology which could be used to to test the reactors and in situ reme- treatment. It is anticipated that this • remediate contaminated soils and diation strategies that are devised will be a DOE site. groundwaters, and to clean contami- using core samples from contaminat- A method for determining the nated waste streams in a cost effective ed sites and process waste streams ratio of active to inactive biomass in a obtained from the industrial partners. fashion, is bioremediation. The bio- culture will be developed by 1/15/97. logical treatment of solutions that Further, the technologies that are contain ions of two particularly toxic developed will be passed to the indus- Appropriate parameters needed elements, chromium and selenium, trial partners for commercialization to describe die kinetics of the bacteri- are being addressed in diis work. and implementation. al reduction of the contaminants using common subsurface bacteria Previous studies have shown diat During this first phase of the will be determined by 5/1/97. various species of bacteria can reduce research, analytical systems have been these ions to less toxic, more stable devised that allow the accurate deter- Appropriate parameters needed states. However, most of these previ- mination of all compounds of inter- to describe the kinetics of the bacteri- ous studies have not addressed system est, and experiments designed to al reduction of the contaminants specific conditions that would be nec- determine the biological reaction using specialized bacterial systems will essary for their application to site kinetics have been started. Further, be completed by 9/15/97. and/or waste streams. Hence, in this based on the advice from our indus- work, experiments are being per- trial partners, we have begun other formed that will allow the determina- experimental programs to (a) charac-

Idaho National Engineering Laboratory University Research Consortium This page is for notes.

Idaho National Engineering Laboratory University Research Consortium

Fish Farm Effluent Treatment for Improving Wastewater Quality (V258)

Ernest L. Brannon, University of Idaho, Aquaculture Research Institute

Co-PI and University: Ron W. Hardy, University of Washington; Keya Collins, University of Idaho

Graduate Students: Steven Todd and Joel Green, University of Idaho

Industrial Collaborator and Company: Bill Jones, Owner of Bill Jones' Trout Farm of Hagerman, Idaho

INEL Collaborator: Bob Cherry

Presenters: Ernest L. Brannon, Keya Collins, Steven Todd and Joel Green

Following petroleum, fish prod- from the nutritional standpoint is to ucts are the second largest valued nat- formulate balanced, nutrient rich, ural resource imported into the Unit- high energy diets to conserve protein ed States. Over 65% of the fish con- and lower waste phosphorus. Low sumed in the US are imported, dissolved oxygen in the rearing envi- accounting for nearly $10 billion of ronment tends to reduce food conver- the US annual trade deficit. The sion. Therefore, waste reduction is potential for die US aquaculture also approached by researching meth- industry to supply that market, there- ods to elevate the level of dissolved fore, is very good, but the greatest oxygen in the rearing environment. restraint is the impact of the fish farm Once the waste load is generated, effluent on water quality. High-density however, we are attempting further rearing environments generate a reduction by increasing the stability of pound of waste for every two pounds the fecal pellet to reduce disintegra- of feed fed, and discharge of that tion prior to waste extraction in rou- waste-stream in public waters is per- tine cleaning operations. Finally, waste ceived as the major limitation to load reduction is also being industry expansion. If effective tech- approached mechanically by examin- nology for the reduction of fish farm ing methods to enhance waste inter- waste can be developed, the ability to ception. These improvements in expand the aquaculture industry with- waste management technology on fish out negative impacts on water quality farms are expected to markedly lower will provide the greatest incentive for nutrients in the waste-stream and growdi of the aquaculture industry. allow the expansion of fish farming in Research on waste management, there- the US with no net increase in efflu- fore, is being pursued through devel- ent waste load. opment of diet formulations for salmonids with reduced waste nutrient loads, increased efficiency of diet utilization, increased stability of the fecal solids generated, and improved methods to capture fish waste before rearing water is discharged. Our approach

Idaho National Engineering Laboratory

K?-rs*^ Zf^wtt-x University Research Consortium This page is for notes.

Idaho National Engineering Laboratoty 10 University Research Consortium

In Situ Biological Destruction of Nitroaromatic Contaminants in Groundwater (V07) Ronald L. Crawford, University of Idaho

Co-PI and University: None

Graduate Students: Terry Hammill, David Duncan

Industrial Collaborator and Company: Gerald Mead, Vice President for Research and Product Development, J. R. Simplot Company, Pocatello, Idaho

INEL Collaborator: Daphne Stoner, Advanced Sciences Biotechnology Group

Presenter: Ronald L. Crawford

Our project concerns the clostridia spores to this dinoseb biodegradation of 2-sec-butyl-4,6- plume with concomitant monitoring dinitrophenol (dinoseb) and 2,4,6- of contaminant concentrations to trinitrotoluene (TNT) by strains confirm the efficacy of in situ Clostridium bifermentans, and has as destruction of the nitroaromatic pol- a primary goal the use of one or more lutants. We are negotiating with a of these anaerobic bacteria for the in variety of site owners to also test our situ remediation of nitroaromatic- technology at a TNT-contaminated contaminated groundwater. Strain site, probably next year. If successful, KMR-1 was isolated from a chemo- this technology will be commercial- stat that was fed 2,4,6-trinitrotoluene ized through our collaboration with (TNT) as its sole carbon and nitro- the J. R. Simplot Company. gen source. Strain TBH-1 was isolated from environmental samples collected from an aquifer contaminated with dinoseb. Strain TBH-2 was isolated from a soil consortium used to bioremediate surface soils contaminated with dinoseb. We have determined that these strains are capable of degrading dinoseb at environmental temperatures (110°C), convert both dinoseb and TNT into products that are degradable to carbon dioxide when conditions are changed from anoxic to aerobic, and can be introduced as spores into aquifers and transported into regions of nitroaromatic contamination. Transport experiments have been performed in an actual dinoseb-contaminated aquifer at the University of Idaho. Present work involves additions through injection wells of fer- mentable carbon sources and

Idaho National Engineering Laboratory University Research Consortium 11 This page is for notes.

Idaho National Engineeruig Laboratoty 12 University Research Consortium

Specific Labeling of Microorganisms Capable of indole cause bacterial colonies to Oxidative Biotransformation of Toxic Chlorinated Ethylenes form pigments that are reproducible with Enzyme-Activated Chemical Probes (V177) for a given strain. Toluene analogues (including phenylacetylene) are trans- formed to yield colored products, Mary E. Watwood, Idaho State University providing a basis for colorimetric assays to screen chemical inducers of Co-PI and University: William K. Keener, Idaho State University degradative pathways that are less toxic than toluene or phenol. Prelim- Graduate Students: None inary experiments indicate that bacte- Industrial Collaborator and Company: David Phelps, Director of Tech- ria with toluene monooxygenase nology, Molecular Probes, Inc. pathways (e.g., B. cepacia G4) transform hydroxylated toluene analogues INEL Collaborator: William A. Apel more readily than nonhydroxylated versions, whereas bacteria with Presenters: Mary E. Watwood and William K. Keener toluene dioxygenase padiways (e.g., P. putida Fl) prefer the latter sub- strates. These observations provide a The accurate detection of envi- involved in TCE degradation. There. means of rapidly identifying path- ronmental microorganisms that is particular interest in bacteria with ways in isolated bacteria. degrade toxic chlorinated solvents, cometabolic TCE oxidation capacity such as trichloroethylene (TCE), is due to enzymes associated with Probe syntheses for the TCE critical for refining bioremediation toluene degradation pathways. degraders Nitrosomonas europaea efforts. Most probes available for Methods for isolating and rapidly (ammonia oxidizer) and Methylosi- bacterial detection are based on bac- screening bacteria for TCE oxidation nus trichosporium OB3b (methane terial characteristics that are only activity, specific toluene degradative oxidizer) are nearing completion. indirecdy associated with TCE oxida- pathways, and pathway control Probes and methods for all 8 toluene tion (e.g., genetic or protein specific mechanisms will facilitate bioremedi- degraders will be tested and refined probes), are very expensive, and ation feasibility studies. within the next year. Preliminary involve complex laboratory proce- mediods for labeling N. europaea and A method for fluorescent label- dures. The primary objective of this M. trichosporium are expected by ing P. putida Fl has been developed project is to develop enzyme-activated December 1996. New syntheses will which involves exposure of cells fluorescent probes to detect TCE likely be required for improved label- trapped on 0.2 mm-pore size mem- degrading bacteria. With this ing. All methods will be tested using brane filters to gaseous phenylacety- approach the activity of the TCE bacterial isolates from the TCE cont- lene (a structural analogue of degrading enzymes actually triggers aminated Test Area North (TAN) site toluene). Eight toluene-degrading or enhances probe fluorescence, of the INEL. These studies will be bacteria using 5 different pathways (7 which is detected spectrophotometri- completed by September 1997. strains degrade TCE) have been col- cally or with fluorescent microsocpy. lected; methods for selectively label- Activity-dependent probes will allow ing these organizms are being pur- direct and selective enumeration of sued. Obstacles currendy addressed TCE degrading bacteria without the include natural fluorescence of intact use of enrichment cultures which cells (autofluorescence), bleaching of alter relative numbers of indigenous stain under light, diffusion of stain bacterial populations. This approach from the vicinity of active cells, and should yield probes that are specific, degradative pathways unsuited to sensitive, relatively inexpensive, and labeling with phenylacetylene (e.g., have broad applicability. P. mendosina KR1). The second project objective is Semi-solid media are being for- to develop probes or methods to mulated for the isolation and differ- facilitate isolation of bacteria from entiation of the 8 toluene degraders. environmental samples and to screen For example, agar media containing these isolates for catabolic pathways

Idaho National Engineering Laboratory University Research Consortium 13 This page is for notes. *

Idaho National Engineering Laboratoiy 14 University Research Consortium

Idaho National Engineering Laboratoiy University Research Consortium 15

Session 2. Materials Synthesis

Tuesday, 8:00 a.m. to 11:30 a.m.

Merton C. Flemings (MIT), chair James A. Seydel (INEL), co-chair Joel Dubow (Uof U), panelist Barry Short, Dave Cauffinan (INEL), panelists

8:00 a.m. G05 Herbert Herman Plasma Processing of Functionally Gradient Materials: State University of New York, Diagnostics, Characterization, and Modeling Stony Brook

8:55 a.m. G01 F. H. (Sam) Froes Direct Production of Low-Cost High-Quality Titanium University of Idaho Powder by Mechanical Alloying

9:35 a.m. — Break

10:05 a.m. G23 Patrick R. Taylor Plasma Syn diesis of Nano-Sized Metallic Powders University of Idaho

10:45 a.m. G146 Anne M. Mayes Towards Viable Lithium Solid Polymer Electrolyte MIT Batteries: An Integrated Materials Approach

11:30 a.m. Adjourn

Idaho National Engineering Laboratory 16 University Research Consortium

Plasma Processing of Functionally Gradient Materials: Diagnostics, Characterization, and Modeling (G05)

Herbert Herman, State University of New "Kirk— Stony Brook (SUNY)

Co-PIs and Universities: Sanjay Sampath, SUNY; Chris Berndt, SUNY; Subra Suresh, MIT

Graduate Student: William Smith

Industrial Collaborator: M. B. Beardsley, Caterpillar, Inc.

INEL Collaborators: Richard Wright, James Fincke, Barry Rabin

Presenters: Herbert Herman, Sanjay Sampath

This interdisciplinary research Inc., who is using plasma spray FGM program examines the fundamentals technology for the manufacture of associated with processing, diagnostics energy efficient diesel engine compo- and materials properties associated nents and earth moving machinery. with plasma spraying (high velocity It is expected that this fundamental melt spraying) of functionally gradient research program will provide the materials (FGMs). Metal-ceramic basis for improved design and manu- FGMs are being processed using facturing processes, thereby enhanc- simultaneous injection of metal and ing the applicability of FGMs at ceramic particles into a plasma flame Caterpillar, Inc., as well as other ener- at given ratios to produce various gy based industries. gradient profiles. Complexities associ- During this first year, working ated with mixing of two (or more) with collaborators at INEL, we have different materials within the plasma built and tested a computer con- are being investigated using modeling trolled FGM delivery system for plas- and advanced diagnostic tools in col- ma spray torches. Diagnostic experi- laboration with INEL researchers. ments have been conducted on a vari- The deposits will be characterized for ety of injection protocols and the compositional uniformity, and underlying issues have been identi- microstructural attributes, linking fied. The particle size effects have these to the processing conditions been identified. Working with the and FGM properties such as residual mechanics group at MIT, experimen- stress distributions, mechanical tal and modeling efforts have been behavior and high temperature oxida- formulated and initial results are tion/ corrosion properties. extremely promising. The second It is anticipated that the program year program will focus on optimiz- will yield methodologies for hardware ing the processing procedures and to development for multiple injection of develop methods for fabrication of feedstock with dissimilar physical FGMs with different layer geome- properties and lead to analytical and tries. Caterpillar, Inc., has provided empirical models with which to syn- materials and specification input to thesize the processing-microstructure- both INEL and Consortium property relationships in plasma spray researchers. The program is progress- formed FGMs. A close industrial ing as originally planned. collaboration exists with Caterpillar,

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Idaho National Engineering Laboratory 18 University Research Consortium can be almost completely removed, Direct Production of Low-Cost High-Qualily (<10 ppm) the market which opens Titanium Powder by Mechanical Alloying (GOl) up will be even larger than if a low cost salt containing (-100 ppm) product is produced. Work is contin- F. H. (Sam) Froes, University of Idaho uing to optimize processing conditions so that the matrix is the salt, Co-PI and University: K. Prisbrey, University of Idaho embedded widi titanium. This will Visiting Scientist: E. G. Baburaj allow removal of the matrix by leach- ing or vacuum distillation to produce Graduate Student: Carl Powell a high quality titanium product (work with the University of Western Industrial Collaborators and Companies: D. Suciu, ERAD; Australia [Paul McCormick] is V. Moxson, ADMA; C. F. Yolton, Crucible Steel already addressing this issue, at no cost to the program). Interstitial lev- INEL Collaborator: B. Detering els are being lowered to acceptable Presenters: F. H. Froes, K. Prisbrey levels by improved sealing arrange- ments, and possible use of a glove box to contain the MA equipment.

Titanium and its alloys are The procedure used is to agitate In the next year of this program extremely attractive materials for use the reactants in a SPEX mill contain- the quality of the powder will be eval- in many aerospace and terrestrial sys- ing steel balls. Reaction times and uated in conjunction with our collab- tems. However, a major impediment products have been measured using orator at INEL and industrial partners to more wide-spread use of titanium temperature, ED AX, X-ray diffrac- (the number of which have grown). based materials, for example in die tion, and SEM. The system was also Key issues are salt content and control cost-conscious automobile industry, is modeled with differential equations of the interstitial elements. Three the inherent high cost. Historically, derived from population balances. other approaches will also be evaluated: die amount of titanium used in the The result was a fine titanium powder (a) use of hydrogen to enhance the final design of many military and at a projected price well below current process, (b) low temperature process- commercial systems is considerably product levels (a realistic estimate of ing with solid TiC14 (presendy at the cost is currendy being determined). lower dian initially planned in large ambient temperature the TiC14 is liq- part because of diis high cost. To The modeling is being conducted uid) and (c) production of alloy pow- enter the high-volume automobile to aid in scale-up of die process to be der such as Ti-6A1-4V, direcdy; the marketplace (16 million vehicles per a continuous (radier than batch) latter an even more cost-effective year in die USA alone) would require process. The model involves the product. Preliminary mechanical getting die cost of titanium down to design of a neural network based, property testing will also be conduct- $1-2 per pound. But even 1 lb per model predictive, advanced, multiple ed on compacted materials, with automobile would increase titanium input/multiple output control system emphasis on low cycle fatigue which is sensitive to the presence of the salt use by 50%. Thus die program has which is also being applied to parallel particles. the potential of revolutionizing the work on die W system. This W work has already resulted in an order for titanium industry. The objective of Thus the program is proceeding 400,000 lbs of tungsten product this work is to substantially reduce on track with commercialization as using a continuous implementation. cost by optimizing a new titanium close as 18 months away. powder production process, based on This early success widi the W system die emerging mechanical alloying omens well for die early commercialization of the titanium process. (MA) technique of displacement reaction—die replacement of one element The product titanium is currendy in a compound by another during under evaluation with key issues MA at ambient temperatures. In being (a) whether die titanium pro- Phase 1, die solid state reaction duced can be separated from the shown below has been studied: MgCl2 salt byproduct and (b) control of the interstitial content (oxygen and TiCl4 + 2Mg -> 2MgCl2 + Ti. nitrogen) of die product. If the salt

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Idaho National Engineering Laboratory 20 University Research Consortium

Plasma Synthesis of Nano-Sized Metallic Powders (G23) sized powders of a variety of metals and the engineering of a system to Patrick R. Taylor, University of Idaho handle the product powders in an inert atmosphere. Co-PI and University: F. H. (Sam) Froes, University of Idaho The major obstacles encountered Graduate Students: Weinxan Zhu, Xiaofu Chen to date are related to the incomplete vaporization of the feed materials and Industrial Collaborators and Companies: Shahid Pirzada, Nanomaterials the product consolidation without Research Corporation; Jianxing Li, Johnson Matthey Electronics grain growth. Research is being performed to overcome both of these INEL Collaborator: Peter C. Kong obstacles. The milestones planned Presenters: Patrick R. Taylor, P.E.; F. H. (Sam) Froes for next year are (a) exploratory experiments for Johnson Matthey Electronics to see if their required products can be obtained; (b) opera- The overall objective of the pro- Other product samples have been tion of the reactor to provide kilo- ject is to develop a thermal plasma subjected to hot isostatic pressing and gram quantities of product for con- reactor system to generate nanocrys- characterization and progress has solidation testing; (c) the develop- talline metallic and intermetallic been made in using lower tempera- ment of methods to consolidate the powders. This overall objective may tures to retain nanometered sized product and retain nanometer sized be divided into several subsidiary grains with near full censification. grains and the measurement of struc- objectives: (a) the development of The value of the project, if the overall tural properties; and (d) preliminary methods to assure complete vaporiza- objective is achieved, is the develop- economic evaluation of capital and tion of the feed materials; (b) the ment of innovative technology to operating costs, comparison to com- development of a fundamental under- provide a new process for the produc- peting technologies and initial market standing of the reactor heat, mass and tion of nanometer sized metal and evaluation. momentum transfer and particle intermetallic powders, at reduced cost nudeation and growth kinetics; (c) and with greater flexibility compared the development of methods for to physical vapor deposition and product collection and handling in an other competing processes. Jonhson inert atmosphere; (d) the detailed Matthey Electronics has shown an characterization of the product pow- interest in the production of several ders for size, shape, crystallinity and nanometer sized metal powders as purity; (e) the performance of experi- feed to their electronic solder indus- ments to evaluate the consolidation try market. Nanomaterials Research of the product powders, including Corporation has shown an interest in characterization and structural prop- the potential commercialization of erties; and (f) the demonstration of the process for a variety of new mate- technological advantages of this rials processes. process over competing technologies (reduced costs, enhanced properties The approach being used is to and identification of markets). inject coarse metal powders into a plasma flame, inducing vaporization, A novel plasma system has been followed by rapid quenching through designed, built and operated. Experi- a deLaval nozzle. The product pow- ments have shown the ability to gen- ders are collected in a secondary erate nanometer sized metal powders. quench and high temperature filter Samples of the product powders have system and handled in a glove box. been subjected to characterization The product powders are character- using X-ray diffraction (XRD), scan- ized and subjected to consolidation ning electron microscopy (SEM), tests. The major accomplishments, transmission electron microscopy to date, are: the demonstration of (TEM) and wet chemical methods. the ability to generate nanometer

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Idaho National Engineering Laboratoty 22 University Research Consortium

Towards Viable Lithium Solid Polymer Electrolyte Batteries: materials exhibiting the layered An Integrated Materials Approach (G146) NaFeO2 structure, die chemistry and heat treatment of lithium-metal-oxides have been related to battery operating Anne M. Mayes, Massachusetts Institute of Technology voltage and intercalation range. Specifically, the relationship between Co-PIs and University: Donald R. Sadoway, Gerbrand Ceder, and voltage and choice of transition metal Yet-Ming Chiang, Massachusetts Institute of Technology has been established. Based on these calculations, several promising new Graduate Students: Patrick Tepesch, Philip Soo, Erin Lavik IC materials have been identified. Postdoctoral Associates: Mehmet I. Aydinol, Mackenzie E. King, Chemical precipitation routes are Gregory J. Kellogg being explored for the preparation of ultra-fine particles of these candidate Industrial Collaborator and Company: Robert Higgins, Manager, New IC materials. Product Development, Eagle-Picher Industries, Inc., Joplin, MO 64802 Milestones for the next year INEL Collaborator: Gary L. Hunt, Automotive Systems and Technology include fabrication of a first genera- Department tion ACC incorporating a dispersion of ultra-fine IC particles, followed by Presenters: Anne M. Mayes and Donald R. Sadoway structural characterization and elec- trochemical testing. First battery prototypes are anticipated for 6/97, The market potential for new candidate polymer electrolytes to be built in collaboration with rechargeable lithium solid polymer for the ionically conductive compo- Eagle-Picher. electrolyte (SPE) batteries is conserva- nent of the ACC. The conductivity tively estimated to be $1 billion per of this polymer has been measured by year by the turn of the century. a.c. impedance methods and found to Impediments to commercialization of be significandy higher dian that of this technology are almost entirely poly(ethylene oxide) at room temper- materials related. To address materials ature, while maintaining dimensional challenges in the cathode, we have stability. Sulfonated polyaniline formed a research team of materials (sPAN) has also been successfully scientists with expertise in the subdis- synthesized as a candidate material ciplines of polymer science, ceramics, for the electronically conductive com- electrochemistry and computational ponent of the ACC. This material materials science. The objective of has a reported conductivity of 0.2 our program is to fabricate an S/cm and can be processed readily advanced composite cathode (ACC) into films by casting from common operable in the service temperature solvents. We have additionally pre- range of-10 to +70°C, and resistant pared a first-generation bicontinuous to failure beyond 1000 cycles. This polymer matrix material by casting new robust cathode will have a mixtures of sPAN and a candidate microstructure consisting of fine ionically conductive polymer from intercalation particles pinned at the solution. The microstructures have interface between ionically and elec- been characterized by optical tronically conductive interpenetrating microscopy, transmission electron polymer networks. First principles microscopy and electron diffraction. computational modelling techniques Model oxide particles have been are being employed to identify incorporated into the mixed polymer superior-performance, low-cost inter- system, and appear to localize at the calation compounds (ICs). interface between the two polymer phases. Major accomplishments to "date include the successful synthesis of Using first principles computational methods (LMTO-ASA) on

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Idaho National F.ngimwing Laboratoty 24 University Research Consortium

Idaho National Engineering Laboratory University Research Consortium 25

Session 3. Reactor Performance, Degradation, and Regulation

Tuesday, 8:00 a.m. to 11:30 a.m.

Mujid S. Kazimi (MIT), chair Ralph G. Bennett (INEL), co-chair David M. Woodall (Uof I), panelist Jim Lake (INEL), panelist

8:00 a.m. N06 Neil E. Todreas Improvement in Nuclear Power Plant Capacity Factors MIT Through Longer Cycle Length Operation

8:50 a.m. N121 K. L. Murty Stress-Strain Microprobe for Assessing Degradation of North Carolina State Nuclear Piping and Vessels University

9:35 a.m. — Break

10:05 a.m. N07 George Apostolakis Software Dependability and Its Impact on Risk-Based MIT Regulation

10:50 a.m. N212 Michael W. Golay Integrated Models, Data Bases, and Practices Needed MIT for Performance-Based Safety Regulation

11:30 a.m. Adiourn

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Improvement in Nuclear Power Plant Capacity Factors Category A or B items will sup- Through Longer Cycle Length Operation (N06) port an extended cycle. Category C items require additional engineering work to resolve. Neil £. Todreas, Massachusetts Institute of Technology . Accomplishment in the core Co-PIs arid University: Prof. Michael J. Driscoll and Prof. Michael W. design area is the development of a 48-month core design for an existing Golay, MIT PWR plant using UO2 fuel enriched

Graduate Students: Feng Li, Robert McHenry, Michael McMahon, to 7 w/o U-235 and Gd2O3 and Thomas Moore, Hideki Masui IFBA (Integral Fuel Burnable Absorbers—a thin ZrB2 fuel pellet Industrial Collaborators and Companies: Kord Smith, Studsvik of coating) as burnable poisons. America; William Kline, Boston Edison Co. (Pilgrim Nuclear Power Achievements in the area of reliability Station); Joe Vargas, North Atlantic Energy Service Corp. (Seabrook include the completion of compre- Nuclear Station); Edward Pilat, Yankee Atomic Electric Company hensive analyses of the PWR Con- densate and Feed and Main Turbine INEL Collaborators: Jerry L. Judd, Nathan Siu Generator systems and the develop- Presenter: Neil Todreas (Michael Driscoll will be present) ment of a framework for reducing forced outage rates through the analysis of key plant components. In the area of surveillance intervals, a sys- The objective of this project is to Electric Company. tematic surveillance resolution proce- develop tools to enable nuclear power dure to prepare for extended cycle To develop a strategy for attain- plants to adopt extended (four-year) lengths was developed, and all sur- ing required plant levels of reliability operating cycles between refuelings. veillances which currendy preclude a and forced outage rates, detailed Tasks to be completed include: long- 48-month operating cycle have been models of plant systems are being cre- lived core designs for both PWRs and analyzed and categorized at both a ated to analyze the relationship BWRs; strategies for attaining the PWR and BWR power plant. To between component failure and repair plant levels of reliability and availabil- date, no obstacles to project comple- rates, system capacity factor, and ity needed to make a 48-month refu- tion exist. overall plant capacity factor. Addi- eling interval attractive, and strategies tionally, thorough analyses of indus- for rationalizing current surveillance Project milestones for July 1996 try-wide component failure databases requirements to a 48-month fuel to June 1997 are PWR systems avail- (NPRDS, GADS, etc.) are performed cycle. ability enhancement; BWR core to determine current component fail- design. An extended cycle will result in ure and repair rates. an improvement in plant capacity Work will continue on: develop- To rationalize surveillances, factor. A net economic benefit can ing a quantitative basis for establish- researchers identify and analyze each result if the cost penalty of the ing optimum surveillance intervals; regulatory and investment protection longer-lived core can be offset by BWR systems availability enhance- based surveillance which currently improved plant operational availability. ment; finalizing PWR fuel/core per- precludes a 48-month cycle. Classifi- formance assessment. In the core design effort, state-of- cations are: the-art nuclear and thermal design Category A: Candidates for on-line codes are used to establish the feasi- performance; bility and costs of a 48-month fuel cycle in PWR and BWR units. Neu- Category B: Must be performed tronic analyses are conducted using while shutdown but are candi- the CASMO-3/TABLES-3/SIMU- dates for administrative exten- LATE-3 reactor analysis suite devel- sion to 48 months or more; oped by Studsvik. Fuel thermal and mechanical performance is evaluated Category C: Must be performed with ESCORE from EPRI and with while shutdown and do not FROSSTEY from the Yankee Atomic • support a 48-month cycle.

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Idaho National Engineering Laboratory 28 University Research Consortium cialization companies for adopting Stress-Strain Microprobe for Assessing Degradation of our Stress-Strain Probe for remote Nuclear Piping and Vessels (N121) operation so that property changes of reactor vessels and others can be Prof. K. I.inga (KL) Murty, North Carolina State University made in situ. • The proposed research is expect- Co-PI and University. None ed to lead to the development of appropriate methodologies for assess- Graduate Students: Peter Miraglia, Ed Preble ing the in-service damage and the Industrial Collaborator and Company: Fahmy Haggag, Advanced Technol- remaining life of the components in ogy Corporation nuclear power plants. The technology can be applied for verification and INEL Collaborator: Vikram Shah quantification of the effectiveness of thermal annealing of embritded Presenter: Prof. K. Linga Murty nuclear reactor pressure vessels. Once the technology is developed, the adaptation of the system for in-situ The major objective of the pro- ordered (Applied Test Systems Inc.) application will be made in collabora- gram is to utilize the recently devel- and will be delivered by the middle of tion with utility companies. oped stress-strain microprobe (SSM) July. A number of steels were pro- to first demonstrate its capabilities in cured from ORNL with the help of assessing die degree of degradation of our technology partner (Fahmy Hag- die mechanical and fracture properties gag of ATC) which included weld of various structural alloys used in and HAZs also. The delays in getting nuclear power technology. The second the allocated funds to the full amount major objective is to develop the sys- precluded us in ordering the equip- tem into an in-situ nondestructive ment at the proposed start of the pro- microprobe for characterization of the ject (in Dec '95); however, the ATC aging degradation of the nuclear was able to get the equipment as soon power plant components, in particu- as we ordered the machine (in mid- lar, the nuclear pipes, pressure vessels Feb). The subsize tensile specimens and reactor supports, turbine blades, are now being fabricated in the etc. The proposed microprobe is machine shop at NCSU from the based on the principle of automated various steels and as soon as they are ball indentation which is rapid, non- ready, the tests will be made. Mean- destructive, adaptable for in situ test- while, INEL collaborator (Vik Shah) ing, and could be made operator- is getting the cast stainless steel speci- insensitive. In addition, the probe mens procured from various vendors provides a localized direct stress-strain for long term (6 months and more) curve determination. The same sys- thermal aging which will be used for tem will also be used in obtaining . characterizing aging effects on these properties using the traditional mechanical properties of these steels. destructive tests (such as tensile, etc.) on subsize specimens and for correlat- Meeting the second research ing them with those obtained from objective involves adaptation of our conventional size specimens. probe for remote testing, and initially the magnetic attachments were sug- The ABI machine was procured gested and tested by our industrial from the Advanced Technology collaborator (ATC). While these tech- Corporation in April 1996 and typi- niques are promising, they are not cal tests were performed to verify its adaptable for in-reactor use of all the operation. The chamber and control materials, many of which are non- systems for testing at low and high magnetic. We are also in the process temperatures have recendy been of investigating various Robotics spe-

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Idaho National Engineering Laboratory 30 University Research Consortium

Software Dependability and Its Impact on nique in which a digraph model Risk-Based Regulation (N07) expressing logical and temporal characteristics of the system, included in George Apostolakis, Massachusetts Institute of both the software and the hardware Technology with which it interacts, is used to construct fault trees identifying paths Co-PI and University: None which can lead to critical system events. Graduate Students: Christopher J. Garrett, Andrew P. Gnau, Xanhui Chen These research issues are being Industrial Collaborator and Company: Stephan J. Hetrick; Supervisor, investigated in the context of our first Computer Engineering; San Onofte Nuclear Generating Station case study, the MIT-SNL Period- Generated Minimum Time Control INEL Collaborator: Nathan Siu Law experiment, which utilizes a Presenter: Prof. G. Apostolakis closed-loop digital control system for the time-optimal adjustment of a reactor's neutronic power. Objectives for next year involve the completion The overall objective of this pro- Review Plan. The primary objectives of our work on the case study in early ject is the development of a method- of die criteria they've proposed are to fall, identifying the strengths and ology, tools and case studies which verify that an applicant has an ade- weakness of the three different support Risk Informed Performance quate software development plan, approaches, and-using that knowl- Oriented Regulation (RIPOR) of dig- with a well defined life cycle, and to edge to set the groundwork for ital I & C systems in nuclear power verify that sufficient documentation methodology development. plants. This project is using case is produced to support review of the studies to develop a methodology for process as well as the product. The establishing performance-based objec- lack of evident quantitative goals or tives and criteria in light of the objectives raises the question of how uncertainties that the increasing use such regulatory guidelines could be of digital software and its interaction integrated into a RIPOR framework. with operators introduce. The major Current activities are being directed products of this work will be the at evaluating the proposed guidelines, development of the right mix of as well as similar guidelines and stan- deterministic and probabilistic crite- dards currendy being applied in other ria that can be verified by acceptable industries, to identify, in detail, the methods, as well as the identification research needs that need to be of appropriate actions in case the cri- addressed in order to develop a teria are not satisfied, so that the RIPOR framework for digital I&cC. overall objectives will be met. The other two research activities We are currendy pursuing three are applications of two proposed parallel courses of research aimed at V&V techniques, namely, formal identifying the strengths and limita- methods and DFM, to our first case tions of some current and proposed study. Formal methods use mathe- practices, from a RIPOR perspective, matical or logic-based ideas and tech- in order to develop a basis of issues to niques in the specification, design, be addressed during methodology analysis and assurance of computer development. The first of these is a software. Using formal methods to critical review of the NRC's current perform V&V involves the construc- approach to digital I&C. Over the tion of rigorous, mathematical proofs previous quarter we have been exam- that each stage of the software design ining Lawrence Livermore National and is logically consistent and com- Laboratory's (LLNL) proposed plete with respect to the previous update to Chapter 7 of the Standard stage. DFM is a model-based tech-

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Idaho National Engineering Laboratory 32 University Research Consortium

Integrated Models, Data Bases and Practices Needed for EDGs require frequent surveillance Performance-Based Safety Regulation (N212) testing and mandatory maintenance, as required by the technical specifica- Michael W. Golay, Massachusetts Institute of Technology tions, with the objective basis of these requirements never having been Co-PI and University: None established; and (c) Potential improvements in terms of both safety Graduate Students: Sarah Abdelkadar, Jess Iversen and economics can be achieved by basing future requirements in these Industrial Collaborator and Company: Sunil Weerakkody, Northeast Util- areas upon risk-based arguments. ities Services Corporation (NUSCO) In this work one of the project's INEL Collaborator: Nathan Siu two Research Assistants has been Presenter: M. W. Golay assigned to play the role of the utility licensee, identifying practices and requirements which should be changed, devising arguments and The purpose of die project on Since this project began its substitute requirements and practices Integrated Models, Data Bases and importance has increased for reasons for the current ones and proposals to Practices Needed for Performance- which include the following: the be submitted to the NRC to justify Based Safety Regulation is to investi- NRC and nuclear industry have con- these changes. The other RA has gate and demonstrate the potential tinued working together to formulate been assigned the role of the NRC, benefits of performance-based safety policies and procedures for imple- formulating PBR regulatory bases regulation (PBR), or as it has become mentation of the performance-based and practices which can be used to known more recendy risk-informed, Maintenance Rule, which went into evaluate proposals which may be sub- performance-based regulation. These effect in July 1996.; and the new mitted by licensees in the EDG area. goals are explained further in the NRC Chairman, S. A. Jackson, has To do this we have undertaken study abstract from the project proposal, as given a priority to moving the NRC of the NRC's standard review plan follows: to using what she terms "risk- and criteria (SRP) and the history of informed performance-based regula- "It is proposed to develop tools, die development of its criteria. We tion." In order to speed this transi- methods and practices to support are also studying the inspection and tion she has directed the NRC staff both the USNRC and nuclear power enforcement practices of the NRC to reformulate its Standard Review industry in structuring a practical regional offices concerning EDGs. Plan and to issue corresponding Reg- approach to performance-based safety ulatory Guides for the use of In performing this work we are regulation. Success in diis work will licensees, to incorporate use of PBR. focused upon the tasks described in improve the safety of operating our original proposal, which are the nuclear power plants and permit In our work we are focusing following: much more efficient use of nuclear upon use of an on-line PRA, a Risk power plant resources. The project's Monitor, for use in planning plant Task 1. Evaluation of the merits results can improve the capabilities of maintenance and revising the opera- and potential uses of the Risk the INEL and enable the NRC to . tional, surveillance and maintenance Monitor. build the foundations and framework requirements of the plant. We are Task 2. Investigation of replacing for performance-based regulation. focusing upon the example of the the relevant prescriptive regula- The tools and practices developed in plant's emergency diesel generator tions by proposed PBR alterna- this work will demonstrate that the (EDG) system. The reasons for diis tives. framework is realistic, and that the choice are that (a) The EDGs are goals are achievable. At all stages of very important for safety, having the At this point our work proceeds the project emphasis will be given to highest value of the Fussel-Vesely risk well and on schedule. We have iden- insights gained from industry experi- importance measure for core damage tified several potential improvements ence. This is likely to produce results frequency (CDF) at that plant— in EDG procedures and require- having a high acceptance level with meaning that failure of die EDGs ments, and are now developing the not only the NRC but also with the would contribute more to core dam- arguments to justify changes in their nuclear industry." age risks than would failure of any regulatory treatments. other system in the plant.; (b) The

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Idaho National Engineering Laboratory University Research Consortium 35

Session 4. Structures

Tuesday, 1:00 p.m. to 4:30 p.m.

Merton C. Flemings (MIT), chair James A. Seydel (INEL), co-chair Joel Dubow (Uof U), panelist Bill Blume, Bob Chaney (INEL), panelists

1:00 p.m. G212 Christopher Leung Optical Fiber Sensors for Concrete Structures MIT

1:50 p.m. G229 Timothy A. Reinhold Wind Loading and Capacities of Components, Clemson University Connections, and Systems

2:50 p.m. — Break

30:20 p.m. G35 M. Nafi Toksoz Spatial Variability of Earthquake Ground Motions and MIT Their Contributions to the Failure of Major Structures

4:30 p.m. — Adjourn

Idaho National Engineering Laboratory 36 University Research Consortium

Optical Fiber Sensors for Concrete Structures (G212) mance based on the theoretical model, (c) further development of Christopher K.Y. Leung, Massachusetts Institute of Technology sensor installation techniques, (d) fabrication of novel fibers for strain and temperature measurements, and Co-PI and University: Theodore E Morse, Brown University (e) further durability tests for optical Graduate Students: Niell Elvin, MIT; Noah Olson, MIT; Yi-Fei He, fibers in the concrete environment. Brown University

Industrial Collaborator and Company: Barrie Sellers, Geokon Inc.

INEL Collaborators: Judy Partin, Mark Stone, Rick Farnswort

Presenter: Christopher Leung

The objective of this four year optical signal with crack opening research program is to develop optical along the fiber is therefore developed fiber systems for die automatic con- based on a combination of mechani- tinuous monitoring of concrete struc- cal and electromagnetic wave analysis. tures. Specifically, we are developing An experimental set-up is also (a) a novel sensor to monitor flexural designed to simulate crack opening in cracking in concrete bridges and concrete members and to measure grouted barrier structures, (b) Bragg both crack opening and optical signal grating strain sensors at 800 nm loss. Theoretical predictions are then which can be used with low cost compared with experimental results. lasers and electronics, (c) sensor for To couple the crack sensor to an combined strain/temperature sensing. existing concrete bridge or grouted The successful achievement of the concrete barrier, special installation research goals can lead to substantial techniques are required. To monitor savings in manual inspection costs as flexural cracks at the bottom of well as improved safety of concrete bridge decks, optical fibers are first structures. embedded into a thin polymeric In FY-96, the research focus is to sheet, which is then glued to the develop a crack sensor for concrete structure. For cracking in the grout- structures which can detect and mon- ed barrier, optical fibers are wound itor a number of cracks widi a single helically around a rod which can be optical fiber, without requiring a-pri- embedded into the hole before grout- ori knowledge of crack locations. ing takes place. These sensing sheets The sensitivity and range of die sen- and rods have been made and tested sor, as well as die number of cracks it in our laboratories. Preliminary can monitor, depend on a large num- results appear to be promising. ber of parameters including (a) die Besides research work related to mechanical properties, optical proper- the crack sensor, preliminary durabili- ties and size of the glass fiber, (b) the stiffness and size of the surrounding ty studies of optical fibers in the plastic coating, (c) the properties of cementitious environment have also concrete, as well as (iv) the fiber lay- been carried out. out in the structure. Widi so many Research tasks planned for FY-97 parameters that can vary, the design include (a) further work on the theo- of an effective sensor based on empir- retical model for signal loss vs crack ical testing is not practical. A theo- opening, (b) design and verification retical model which relates the loss of of crack sensors with optimal perfor-

Idaho National Engineering Laboratory

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Idaho National Engineering Laboratory 38 University Research Consortium tasks are proceeding according to the Wind Loading and Capacities of modified schedule submitted to MIT Components, Connections and Systems (G229) as a result of the late project start date. The second year will focus on Timothy A. Reinhold, Clemson University simulation of flow around buildings to. insure that testing of roof coverings Co-PIs and Universities: Ben L. Sill, Clemson University; Ahsan Kareern, can be properly simulated. The per- Notre Dame University; Dale C. Perry, Texas A&M University; Norris formance of components for the full- scale facility will also be evaluated to Stubbs, Texas A&M University assist INEL in the selection of the Graduate Students: Edward Sutt, Clemson University; Muralidhar Kallem, most effective alternatives. A concept Clemson University; Jefferey Sciaudone, Clemson University; Sang Hwun for a smaller scale roofing test facility Choi, Texas A&M University; Sooyung Park, Texas A&M University will be investigated. The multiple actuator system will be extended to Industrial Collaborator and Company. Edward Laatsch, State Farm Fire simulation of nonlinear non-gaussian and Casualty Co. loads. The cost benefit and risk INEL Collaborator: Cheryl O'Brien, ACETS assessment methodology will be evaluated against field data on losses Presenter: Timothy A. Reinhold obtained from insurers for recent hur- ricane-events. Successful completion of the A full-scale test facility is critically obtained from a full-scale experimental three year project will provide the needed for assessing the performance building tested at Texas Tech Univer- foundations for creation of a state-of- of buildings subjected to extreme sity. Preliminary results indicate that the-art full scale wind test facility. winds. The objective of this project the concept is technically feasible but The cost benefit studies will help to is to determine the technical feasibility that it will probably require addition- focus the initial testing to be con- of constructing such a facility and to al lateral turbulence generation ducted in the facility to insure that determine critical elements required devices. the facility provides rapid value to the to produce desired profiles of mean The project is also evaluating the government and potential user indus- wind speed and the turbulence struc- feasibility of using multiple actuators tries. Creation of this facility will ture of the wind and/or the magni- in a feedback control system to pro- help to improve the performance of tude, spatial distribution, and correla- duce simulated wind loads for testing houses and commercial structures in tion of wind loading. A secondary of components and connections. The severe wind events. The reduction in objective is to formally develop a cost hardware and software has been losses from future storms is critical to benefit analysis methodology which assembled for this system and initial the economic health of the United will provide focus to the building per- testing has been completed. The pro- States. formance studies in such a facility. ject presentation will describe the In the first year, the project has accomplishments to date including developed a 1:25 scale model of a proof of concept through matching of proposed high wind test facility. This target and monitored time histories. facility concept, named the Wall-of- Development of the cost benefit Wind, would involve an array of fans analysis methodology is well under (either turbo prop or electric) to create way using fuzzy analysis methodologies. peak winds of about 200 miles per " Results of risk analyses for individual hour. Each fan would operate under properties and groups of properties a control system which would allow have been completed and results of separate control of the wind velocities sensitivity studies will presented at being produced by each fan. The the annual meeting. objective is to produce a variety of wind field conditions and subsequent The project is on schedule to loadings on buildings. Results are provide the basic aerodynamic design being compared with field data on requirements for the Wall-of-Wind by wind conditions and surface pressures the end of the fiscal year. The other

Idaho National Engineering Laboratory University Research Consortium 39 This page is for notes.

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Idaho National Engineering Laboratory 40 University Research Consortium

Spatial Variability of Earthquake Ground Motions and Their and 6-9 have either been accom- Contributions to the Failure of Major Structures (G35) plished or are near completion, and their results are being presented at the M. Nafi Toksoz, Massachusetts Institute of Technology INEL Summer Review Meeting. Key milestones achieved in 1995 Co-PIs and University: Emmanuel Chaniotakis and Eduardo Kausel, and 1996 were die evaluation of the MIT ground motion and structural Graduate Students: None response data to define the necessary performance characteristics and limi- Industrial Collaborator and Company: Steve Fairfax, Failure Analysis tations of the simulator, the favorable Associates feasibility analysis of the power system and the EM driver, the design of a INEL Collaborator: Thomas K. Larson scale-model (table-top) EMSS sched- Presenters: Prof. M. Nafi Toksoz, Emmanuel Chaniotakis, Dr. Steve Fairfax uled to be implemented by June 1996, and the development of a detailed, conceptual design for the test facility. Another important mile- The overall objective of this pro- experiments, and would be a major stone has been die flexible design of ject is the improved earthquake-resis- national resource. the power system to accommodate tant design of man-made structures The purpose of this project is to the requirements of other ACETS to significandy mitigate the severe perform the design work necessary test facilities such as the "Wall of effects of destructive earthquakes in for the construction of a full-size, Wind." The specific goals planned urban areas. The severe human and electromagnetic seismic simulator for 1997 are (a) to perform computer economic losses resulting from recent (EMSS) capable of faithfully repro- modeling to generate the 3-D ground earthquake disasters near urban areas ducing the large and complex ground motion simulations for the site geolo- demonstrate the need for better seismic motions generated by destructive gy at the INEL facility to estimate the modeling to improve building design earthquakes. To accomplish this, we seismic wave propagation generated by codes for both new construction and have assembled a multi-disciplinary the EMSS; (b) to design die soil box in retrofitting older structures. The team of scientists expert in the fields for die seismic simulator; and (c) to Kobe earthquake alone caused over of seismology, civil, electrical, and complete the engineering design for 5,500 deaths, thousands of injuries mechanical engineering, and electro- the EMSS. and widespread homelessness, magnetic energy systems. This team destruction and damage to thousands has identified ten key tasks to complete of buildings, and disrupted major the design work including: (1) evalu- transportation systems. The direct ation of ground motion from recent economic cost of this earthquake was large destructive earthquakes to estab- about $200 billion. Obtaining lish the criteria for the motions gen- knowledge about the performance of erated by the EMSS; (2) analysis of new earthquake-resistant designs and the simulator base/ground interac- retrofitting techniques before future tion; (3) computer modeling of catastrophic eardiquakes occur is crit- earthquake motions using 3-D ical to gready reducing the enormous heterogeneous earth models (4) test human and economic losses caused building/simulator platform interac- by such events. One of the most tion; (5) soil box testing to study effective approaches to meet this soil/building interaction; (6) EM objective is to develop a full-scale, driver feasibility; (7) EMSS conceptual three-dimensional seismic motion design; (8) a performance and cost simulator to test experimental earth- comparison between EM and quake-resistant designs in natural- hydraulic simulator systems; (9) scale structures. A full-scale seismic analysis of the power system required simulator has the potential to over- for the EMSS; and (10) engineering come the limitations of sub-scaled design of the EMSS. Tasks 1, 2, 4,

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Idaho National Engineering Laboratoiy 42 University Research Consortium

Idaho National Engineering Laboratory University Research Consortium 43

Session 5. Nuclear Medicine Accelerators and Isotopes

Tuesday, 1:00 p.m. to 5:30 p.m.

Michael W. Golay (MIT), chair Ralph G. Bennett (INEL), co-chair David M. Woodall (Uof I), panelist Jim Lake (INEL), panelist

1:00 p.m. N215 Jay F. Kunze Laser Separation of Isotopes for Nuclear Medicine Idaho State University Applications

1:35 p.m. N200 George H. Miley Compact Neutron Source Based on Accelerator-Plasma University of Illinois Target Technology

2:20 p.m. N01 Lawrence M. Lidsky Application of High Power Electron Accelerators to MIT Isotope Production

3:05 p.m. Break

3:35 p.m. N21 Jacquelyn C. Yanch Boron Neutron Capture Synovectomy (BNCS): MIT Treatment of Rheumatoid Arthritis with the 10B(n, a) Nuclear Reaction 4:35 PM N24 Frank Harmon Compact Accelerator Neutron Sources for BNCT Idaho State University Using Near Threshold Charged Particle Reactions

5:30 p.m. Adjourn

Idaho National Engineering Laboratory 44 University Research Consortium

Project Title: Laserl Separation of Isotopes for been measured for the M0F6 mole- Nuclear Medicine Applications (N215) cule. The next major experimental step will involve developing a small supersonic flow path so that the CO2 Project PI and University: Jay F. Kunze, Idaho State University laser can more effectively separate isotopes as a result of the narrower Co-PIs and Universities: JeffW. Eerkens, University of Missouri; Thomas vibrational frequency spread at the LaHann, Idaho State University cooled expansion temperatures. Graduate Students: Chris Hunt, Idaho State University; Greg Anderson, University of Missouri; Donald Puglisi, University of Missouri

Industrial Collaborator and Company: Malinckrodt Medical, Inc.

INEL Collaborators: Steve Laflin, John Braisier

Presenter: Jay F. Kunze

The laser enrichment process CAMECO opted to no longer support being developed involves selective the research. Isotope Technologies, molecular excitation of a hexafluoride Inc. then donated the equipment and molecule using lasers, and then allow- their share of the patents to the ing chemical reaction of the excited University of Missouri. isotopic species to occur, resulting in With the potential of the ATR the precipitation of the reacted iso- and of accelerators to make medical tope from the flowing gas stream. isotopes of various kinds, it became The process has been designated apparent that separation of small CRISLA (Chemical Reaction of Iso- quantities of isotopes, primarily for topes by Selective Laser Activation). , The process is somewhat like the Los targets, would be a major need. The Alamos MOLIS process, except that Calutrons at Oak Ridge had been MOLIS used several dozen molecular shut down, and USA supplies of activation steps to obtain complete many separated isotopes were in short dissociation of the desired hexafluoride supply. The use of the CRISLA molecule. In the case of CRISLA, process to produce gram to kg quan- chemical reaction energy does most tities of an isotope seemed more rea- of the work, rather than laser energy, sonable than the goal for enriching since the laser merely excites the mol- uranium, which would demand out- ecule to a relatively low excited state. puts of many tons per day. The experimental work on sepa- The process has been privately ration of molybdenum isotopes has funded, for die intended purpose of been under way at the University of uranium enrichment, in the USA Missouri for over a year. ISU will be since 1978, and was most recendy a looking at the potential and future cooperative effort between die inven- need for other isotopes, and of die tor, the USA company (Isotope Tech- toxicity of radio parmaceuticals diat nologies, Inc.) and die large Canadian are currendy being made without the uranium mining company, CAMECO. use of separated target isotopes. The However, when the uranium enrich- experimental work has proceeded ment market became unprofitable as through the phase of accurate mea- a result of Russia putting large quan- surement of vibrational lines of the tities of enriched uranium from various isotopes, and chemical raction decomissioned weapons and from rates at several temperatures have stockpiles into world markets,

Idaho National Engineering Laboratory University Research Consortium 45 This page is for notes.

Idaho National Engineering Laboratory 46 University Research Consortium to design a 1015 D-T n/s device ulti- Compact Neutron Source Based on mately desired for high-yield applica- Accelerator-Plasma Target Technology (N200) tions. Intermediate-yield units developed in the phased scale-up plan will George H. Miley, Fusion Studies Laboratory, University of provide near-term "pay-offs" in terms Illinois, Urbana-Champaign of providing commercially attractive units for expanded activation analysis Co-PI and University: None applications and local isotope produc- Graduate Students: Yibin Gu, John M. DeMora, Blair P. Bromley tion use.

Industrial Collaborators and Companies: John Sved, Deutsche Aero- *• space/Daimler-Benz; Tumay Turner, NOVA, Inc.; Larry Jacobson, Hal- liburton; Bart Czirr, Mission Support, Inc.

INEL Collaborators: J. Harwell, R. A. Anderl

Presenter: G. H. Miley

The objective of this research obtained marketing license rights to project is the development of a sell demonstration units for activation unique accelerator-plasma target neu- analysis of coal impurities. tron source. Neutron-generating However, to expand the range of devices are enabling technologies for a potential applications, this technology variety of industrial and medical must be extended along two distinct applications, including non-destruc- paths: the development of devices tive testing of hazardous and mixed based on alternate geometries for spe- wastes and assay of fissile materials cific applications and the optimiza- for nuclear safeguards and arms con- tion of the concept to higher-yield trol. A variety of first-step applica- sources. For example, potential med- tions, such as activation analysis of ical applications, with immense mar- coal impurities, currendy use kets in fast neutron cancer therapy radioisotope sources (e.g., Cf-252) or and boron neutron capture therapy accelerator-solid target neutron (BNCT), require a source capable of sources with a strength of 107 n/s. significandy higher neutron rates for However, use of radioisotopes human treatment. Thus, UI workers involves cosdy licensing and shielding, recendy invented a variation of the and currendy available accelerator- original IEC, a unique compact cylin- solid target neutron sources are drical (C-) device. It potentially expensive and unreliable, due to the offers higher yields while eliminating rapid deterioration of the target. internal wire-grid electrodes and asso- Recendy, University of Illinois (UI) ciated problems of grid erosion, thus workers have developed a unique extending the device lifetime. Neu- plasma target source that avoids these tron emission simulates a "line problems. It employs an inertia! elec- source," making it especially attractive trostatic confinement (IEC) device for applications requiring broad neu- diat produces fusion neutrons by an tron coverage. A prototype C-device accelerator-plasma target method, has demonstrated D-D yields up to thus avoiding target deterioration and 107 n/s. The goal of the present offering competitive yields in the 107 work is to scale up the C-device, (in n/s range. Strong interest has already multiple steps of 102 increase in developed in commercialization of yield) to obtain the database needed this device, e.g. one company recently

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Idaho National Engineering Laboratory 48 University Research Consortium

Application of High Power Electron Accelerators production, we have developed an to Isotope Production (N01) interactive database based on the National Nuclear Data Centers Table Lawrence M. Lidsky, Massachusetts Institute of Technology of Isotopes. We have added nuclear decay systematics to the database, Co-PI and University: Richard Lanza, Massachusetts Institute of Technology induding decays to and from excited states whenever feasible. For any Graduate Students: David Chichester, Randy Tompot chosen isotope in the database, it is Industrial Collaborator and Company: Richard Testa, Thermo Technology possible to determine the precursor Ventures Inc. and descendant isotopes for an arbitrary number of generations, and to INEL Collaborator: Ralph G. Bennett quickly determine the identity and natural abundance of those stable iso- Presenter: Lawrence M. Lidsky topes in the neighborhood of each precursor which could be used as a target. We have also compiled evaluated This project is an investigation of mental results tracked the predicted photonudear reaction cross-section sets the use of photonuclear reactions to values within a few percent over an for several isotopes of potential interest. produce radionudides of medical and order of magnitude in specific activity. Major milestones for next year industrial interest. We use electron- This cross-section set is being used to include the choice of commercial tar- beam generated bremsstrahlung to design several versions of production get design and operating parameters, produce intense radiation fluxes with targets, based on parametric studies and subsequent thermal-hydraulic photon energy in the Giant Dipole of the design space. The first version tests under full heat load. Resonance range of various target iso- stresses design simplicity and uses a topes. Radionudides are generated passive aluminum structure to mini- by (g,n), (g,p), (g,np), and higher- mize electron heat loading of the Mo- order reactions, depending on target 100 target slugs. The second version isotope and beam energy. This tech- uses magnetic fields to sweep the nique is usually complementary to electron beam but allows low energy the more commonly used schemes for photons to reach the target. Both radionuclide production (ion beams, versions use a helium cooled sintered neutron absorbtion, fission product) tungsten convenor plate. We are in but there are some notable cases the process of determining the opti- where several techniques are capable mum operating point as a function of of producing a given radionuclide. linac operating map and target power In such cases, the choice of the most handling capabilities. economical production method often depends on a complex interplay of In support of the assessment of physics, technological capabilities, commercial potential, we have devel- and existing medical-industrial infra- oped a buildup/decay model for the structure. Our program is focused on relevant isotopes which is capable of one such isotope, Tc-99m, but we are modeling an arbitrary schedule and also investigating a range of other efficiency of technetium separation radionudides of potential commercial from the irradiated target slugs. We interest. have also investigated potential vendors of isotopically enriched molyb- We have developed the capability denum to provide data for economic to predict the Mo-99 production rate optimization. We have procured and for targets of potential commercial verified the composition of a sample interest. We have performed two lot of very highly enriched Mo-100 benchmark irradiations using the that will be used for irradiation studies. electron linacs at NIST (at 28 MeV) In support of the study of other and at RPI (at 40 MeV). The experi- isotopes suitable for photoneutronic

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Idaho National Engineering Laboratory 50 University Research Consortium

Boron Neutron Capture Synovectomy (BNCS): Treatment of Rheumatoid Arthritis with the 10B(n,a) Nuclear Reaction (N21)

Jacquelyn C. Yanch, Massachusetts Institute of Technology

Co-PI and University. None

Graduate Students: Emanuela Binello, An Lu

Industrial Collaborators and Company: R.E. Shefer and R. E. Klinkowstein, Newton Scientific, Inc.

INEL Collaborator: David Nigg

Presenter: J. C. Yanch

The potential for the boron neu- involve studies assessing in vivo tron capture reaction to be effective uptake of the boronated compounds in treating rheumatoid arthritis is using a rabbit model of human under investigation. Dubbed "Boron arthritis. These will be followed by Neutron Capture Synovectomy" this studies to assess the efficacy of BNCS potential new therapy procedure will (i.e. boron administration followed involve the injection of a boronated by neutron irradiation) in the rabbit compound direcdy into the arthritic model. joint followed by joint irradiation by Additional work in the area of a beam of low-energy neutrons. This optimal neutron beams for BNCS is called 'synovectomy1 since the goal has been carried out and the ideal is to destroy the inflamed synovium, neutron energy range (0.025 eV - die cause of the pain and ultimate 100 eV) has been identified. This disability associated with rheumatoid information has been used as input to arthritis. Working with researchers at the neutron beam design study cur- the Harvard Medical School, studies rendy underway. This study, carried using live human arthritic synovium out by Monte Carlo simulation, obtained from the operating room focuses on optimal moderator and have been carried out. Three reflector materials to produce the boronated compounds have been most useful neutron beam. Current evaluated in terms of dieir ability to results suggest diat a heavy water be taken up by the arthritic tissue. moderator surrounded by a graphite Uptake measurements were carried reflector will provide high therapeutic out using prompt gamma neutron ratios and will allow therapy to be activation analysis. Results indicate completed very quickly. All mile- that, using a compound 100% stones have been met to date, with enriched in lOBoron, 10B concentra- the exception of modifications to the tions of 1500-2500 ppm are easily INEL treatment planning software obtained. Similar concentration which could not be accomplished due ratios are expected to be achieved in to lack of funding for the INEL col- vivo due to the phagocytic action of laboration. Milestones originally synovial lining cells, and as a result of scheduled for FY-98 (not funded) are the synovial physiology. Uptake planned for FY-97. studies are underway to assess uptake of boron by articular cartilage in the joint. The next phase of work will

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Idaho National Engineering Laboratory 52 University Research Consortium

Compact Accelerator Neutron Sources for BNCT Using Near Threshold Charged Particle Reactions (N24) important and will be the basis for next year's work. In the next year, we will (1) systematically compute the Frank Harmon, Idaho State University epithermal fluxes achievable by near threshold reactions for various target Co-PI and University: Xiao-Lin Zhou, MIT materials, (2) select target material based on thermo-mechanical consid- Graduate Student: Charles Lee (MIT) erations and design and test the target, and (3) experimentally demonstrate Industrial Collaborator amd Company: Robert Hamm, AccSys Technology, intense epithermal neutron produc- Inc. tion using the target design. Step (3) INEL Collaborators: Yale Harker, David Nigg will be conducted at ISU and INEL. Obviously, the tasks for the next year Presenters: Frank Harmon (ISU), Xiao-Lin Zhou (MIT) will be key to the success of this project as a whole.

The objective of the project is to In the past year of the project, develop a commercializable design of we have completed three major tasks compact, transportable neutron at MIT. (Work at ISU and INEL source for BNCT suitable for the will be summarized by Harmon and hospital environment. Past effort in Harker separately.) First, we have accelerator neutron source for BNCT conducted an extensive survey and has not been successful because of the study of experimental reaction data difficulty in target design to withstand on p-LLand p-Be reactions and iden- high current and the need of high tified the areas where measurements current which cannot be easily met are needed to obtain key data for by compact commercial accelerators these reactions. The result is com- diat produce low average current. piled into a report which will be the Our project proposes to use the key basis for neutronic studies for target idea of near-threshold charged-partide design in the next year. Second, we reactions to solve the difficulty and have established a computation setup remove the limitations. In a near- and software for neutron transport threshold reaction, epithermal neu- studies and charged particle reaction trons are produced direcdy without calculations. Using this setup, I have the need for moderation. Although trained Charles Lee, a Ph.D. candi- the total neutron yield is lower than date, to conduct MCNP transport that at high charged-partide energies, computation and nuclear reaction the overall useful neutrons at epither- analysis in the past year for this pro- mal energies will be much higher at ject. Third, Lee and I have carried near threshold. As a result, the need out a series of reaction and neutronic of proton current can be significandy computations and reaction analyses reduced such that a compact accelera- and obtained preliminary results tor can be used and the lower current which showed important properties need will also make target design of near-threshold reactions. These much easier. In addition, the beam results indicated that 100 mA of contains no fast neutron contamina- current seemed to be sufficient for tion, which is an advantage over reac- producing 109 n/cm2s epithermal tor beams. If the project is successful, flux based on near-threshold reac- it will lead to the first commercializable tions. This amounts to a factor of design of compact neutron source for 100 reduction in die need on proton BNCT based on current commercial current compared to the traditional accelerator technology. mode of neutron production at high proton energies. These results are

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Idaho National Engineering Laboratory 54 University Research Consortium

Idaho National Engineering Laboratoty University Research Consortium 55

Session 6. Waste Processing at High Temperatures

Tuesday, 1:00 a.m. to 5:15 a.m.

Kenneth A. Smith (MIT), chair David L. Miller (INEL), co-chair Edwin W. House (ISU), panelist Barry Short, Bob Snelling, Arvid Jensen, Jim VanVliet (INEL), panelist

1:00 p.m. V16 Adel F. Sarofim Application of Solution Thermodynamics and Aerosol MIT Dynamics to Enhance Residue Segregation in Molten Metal Waste Processing State

1:55 p.m. V39 C. M. Wai Supercritical Fluid Extraction System for Toxic Metal University of Idaho Contaminated Environmental Matrices

2:40 p.m. — Break

3:10 p.m. V246 H. Jeff Empie Incremental Kraft Recovery Capacity Using Mixtures of Institute of Paper Science Black Liquor and Bleach Plant Effluents and Technology

3:55 p.m. V22 Scott S. Hughes Chemical and Petrographic Characterization of Idaho State University Vitrification Products

4:40 p.m. V242 Gary Lowe Correlation of SREX and TRUEX Equilibrium Data University of Idaho for Use with the ASPEN Model

5:15 p.m. Adjourn

Idaho National Engineering Laboratory 56 University Research Consortium

Application of Solution Thermodynamics and Aerosol Dynamics surface as compared to that through to Enhance Residue Segregation bubbles. Samples taken from the in Molten Metal "Waste Processing (VI6) melt at discrete time intervals were analyzed using inductively coupled plasma/mass spectrometry (ICP/MS). Adel E Sarofim, Jefferson W. Tester, Merton C. Flemings, Once the theoretical model is validat- Massachusetts Institute of Technology ed, the simultaneous evaporation of several elements will be considered. Co-PI and University: None Since special emphasis is directed Research Staff: Anthony Modestino to the aerosol formation mechanism, the aerosol will be collected by using Post Doctoral Associate: Gokhan I. Senel a sampling probe/cascade impactor system and this ten-stage impactor Graduate Student: Jose Benavides will be used to size segregate the par- Industrial Collaborator and Company: Christopher J. Nagel, Executive ticles ranging from 0.056 mm to 18 Vice President, Molten Metal Technology Inc. mm. The composition of the particles will be determined using a com- INEL Collaborator: Paul A. Lessing bination of methods including scan- ning and transmission electron Presenter: Prof. Merton C. Flemings microscopy and ICP/MS.

The ability of several available thermodynamic databases will be The use of molten metal process- merged lance is used to improve the quantitatively investigated to predict ing of mixed wastes has die advan- reaction kinetics. tages of destroying organic hazardous measured phase composition for the In order to select proper feed- components and the partitioning of similar conditions to what is antici- stocks, the evaporation rate of differ- the inorganic residue between metal, pated for molten metal/slag process- ent impurities from iron and copper ceramic, and aerosol phases. The ing. The development of improved melts was theoretically studied and a variation of the temperature and predictive models will also be model describing kinetics and mecha- composition of the metal and ceramic attempted. nisms of removal was proposed. The phases permits a wide range of lati- contribution of the liquid, interface tude in the distribution of toxic met- and gas mass transfer coefficients on als such as lead and radionudides. The objective is to maximize the vol- the overall process was evaluated. In ume reduction of the disposal waste, this model, several elements having die recycling of elements of value, various physical properties such as and the delisting of the ceramic vapor pressure and activity coefficients phase. The mediods for estimating were considered. Estimations were thermodynamics of the ceramic phases carried out in several ranges of para- will be refined and die characteriza- meters including argon gas injection tion of the dynamics of the aerosol' rate, and number and size of the gas produced during processing will be injection orifices. investigated in sufficient detail to Based on the model, several achieve the above objective. solutes were selected for experimental investigation. The evaporation rates The research is based on the of (1 wt %) cadmium, bismuth and studies of small size melts at MIT zinc from copper melts at 1473°K, and on the pilot plant facilities at and lead and bismuth from iron Molten Metal Technology, Inc. The melts at 1873°Kwere measured. In construction of the 10-pound capaci- some cases, the top surface of the ty induction furnace system at MIT melt was covered with a slag layer to has been completed. In this system, determine the fraction of the evapora- argon gas injection through a sub- tion that takes place through the top

Idaho National Engineering Laboratory University Research Consortium 57 This page is for notes.

Idaho Nattonal Engineering Laboratory 58 University Research Consortium Kellogg, Idaho. The extraction pro- Supercritical Fluid Extraction System for files generally show a rapid initial Toxic Metal Contaminated Environmental Matrices (V39) removal of metals from the soil followed by a gradual low level metal C. M. Wai, University of Idaho extraction from the solid matrix. The extraction efficiencies increase with Co-PI and University: T. E. Carleson, University of Idaho increasing pressure (100-300 atm) Graduate Student: R. D. McMurtrey and have little effect by temperature in the range 40°C to 60°C. These Industrial Collaborator and Company: Neil G. Smart, British Nuclear organophosphorus reagents are also Fuels pic (BNFL) effective for SFE of heavy metals (As, Pb, Hg), precious metals (Au, Pd, INEL Collaborators: D. M. Ginosar, R. V. Fox Pt), and uranium from acidic solu- Presenter: Ryan D. McMurtrey tions. The industrial partner, BNFL, has sent a senior scientist (Neil Suprecritical fluid extraction cal scale, to be quite effective for Smart) to Idaho to work with us in (SFE) offers several advantages over removing toxic metals including Cd, the development of this SFE technol- conventional solvent extraction, Pb, Hg, and U direcdy from solid ogy. Our research group is also work- including the minimization of organic materials. Our work in SFE at the ing closely with the INEL collabora- liquid waste generation and exposure University of Idaho has advanced to a tor Bob Fox as demonstrated in a of personnel to organic vapors. The stage where scale-up of this technolo- joint paper to be presented at the high difrusivity, low viscosity, and T-P gy for treating industrial wastes "Spectrum 96" meeting this August. dependence of solvent strength are becomes possible. A US patent derived from our some attractive properties which In the past year, we have evaluat- research has been filed in July, and make superciriitcal fluids excellent ed a number of commercially avail- two manuscripts have been submitted candidates for extraction and recovery able chelating agents for extraction of for publication. Continuation of this of organic compounds from solid heavy metals (As, Cd, Cr, Pb, and work for a technology demonstration materials. Carbon dioxide is a gas of Hg) and actinides (U and Th) from at INEL is proposed for the next year. choice for SFE because of its moder- different matrices including soil, ate critical constants (T = 31°C and c wood, and aqueous solutions. Our P = 73 atm), inertness, and availabil- c calculations indicate that alkyl substi- ity in purified form. After extraction, tuted ligands with a chain length of the fluid phase is depressurized to approximately 8 carbon units, prefer- separate solutes from carbon dioxide ably branched, have the most favor- and the gas can be recycled for able properties in terms of achieving repeated use. The SFE technology high solubilities in supercritical car- has been applied to industrial scale bon dioxide. A number of commer- operations such as the preparation of cially available ligands with alkyl decaffeinated coffee and hop extracts. chain lengths of between 8 and 10 Direct extraction of metal ions carbon units were chosen for SFE in by superciritcal carbon dioxide is investigation in this study. Several highly inefficient because of the organophosphorus reagents under the charge neutralization requirement and trade names Cyanex 301, Cyanex the weak solute-solvent interactions. 302, and D2EHTPA show high effi- One approach of extracting metal ciencies for SFE of a range of heavy ions by supercritical carbon dioxide is metals from a variety of matrices. to convert the charged metal species Real-world samples include arsenic- into neutral metal chelates using a contaminated soil samples from a complexant dissolved in the fluid copper smelter in Tacoma, Washing- phase. This in situ chelation-SFE ton, and lead contaminated soils from technique has been shown, in analyti- the Coeur d'Alene Mining District in

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Incremental Kraft Recovery Capacity Using Mixtures of ery efficiency for the liquors, the total Black Liquor and Bleach Plant Effluents (V246) energy recovered from the BPES is 0.0001 Quads/yr. Valuing the H. Jeff Empie, Institute of Paper Science & Technology process steam that is generated at $4/MM BTU, this amounts to over Co-PI and University: None $300,000/yr. savings for the mill. The avoided cost of lime kiln fuel (based Graduate Students: None on typical operating parameters of 6 Industrial Collaborator and Company: Karl Morency, Georgia Pacific MM BTU/ton of CaO produced, 1 Corp. ton of CaO required for every 4 tons of pulp produced, and a $3/MM INEL Collaborator: Dean Harding BTU fuel) amounts to about $3 MM/yr. This assumes that causticiz- Presenter: Jeff Empie ing requirements for BPES and BLS are the same. This is not a bad assumption, since the BPES and BLS Closed-cycle operation of kraft Autocausticization of die sodium bodi have a ratio of organics to inor- paper mills is expected to be legislated carbonate produced by black liquor ganics of about unity and both origi- for environmental reasons. Combina- combustion has been demonstrated nated with the brown stock washers. tion of bleach plant effluents (BPEs) in sulfur-tree systems using Fe2C>3, It is crucial to establish, at typical with black liquor has been proposed but not for the kraft liquors that gasification temperatures, the desired as an attractive solution to the efflu- dominate world paper production. chemistry; i.e., formation of solid ent disposal problem posed by closed Sulfur combines with the bi-valent sodium metallite and H2S gas, but cycle operation. Unfortunately, this metal oxide to put it in a stable sul- negligible condensed phase sulfides. will increase the liquor solids flow to fide form, rendering it useless for This is being shown in a relatively be handled by the present recovery autocausticizing. This research will simple and inexpensive, electrically process equipment. Since most kraft show how to temporarily remove the heated reactor patterned after one mills are already capacity limited by sulfur from the sodium chemicals in developed for coal hydrogenation and their kraft recovery boiler and the liquor prior to carrying out the subsequendy used for black liquor. because incremental recovery capacity autocausticizing reaction. The key feature of diis configuration is prohibitively expensive, combining is a rapid initial liquor heating rate of bleach plant effluents with black The equipment needed for com- about 500°C/sec, followed by an liquor presents a serious technical and mercial production would be available extended time at the final reaction economic problem. in sizes and costs that are consistent with the needs of incremental capacity. temperature of 700°C, all in an Research is under way that, if In recovering the chemicals, calcination atmosphere of flowing steam. The successful, will enable kraft pulp mills in a lime kiln would be eliminated, time-temperature history of the reac- to move toward environmentally hence removing die need for an tants should closely simulate what a mandated closed-cycle operation by external supply of fossil fuel. The liquor particle would experience in a developing a chemical recovery fuel gas generated from the organic commercial fluidized bed gasifier process based upon gasification tech- fraction of the feed liquor would be under typical process conditions. nology that will combine BPE's with used to raise process steam as well as The focus this quarter has been black liquor and recover die chemical cogenerate power. on detailed design, procurement, and and energy values contained in them An estimate of the incremental fabrication of the laboratory scale in an economical, safe, and environ- energy recoverable from the BPEs has gasification reactor. Concept feasibil- mentally acceptable manner. Fluidized been calculated, assuming die ratio of ity depends upon obtaining reaction bed gasification, combined with auto- bleach plant effluent solids (BPES) to rate, selectivity, and conversion data, causticization using an amphoteric black liquor solids (BLS) to be about including the composition of gaseous salt, will provide the incremental 0.01, and die Higher Heating Value and condensed phase products. recovery capacity by converting the of BPES to be about 90% of that for Because of die corrosive nature of the feed liquor to kraft white liquor and BLS. For a 2,000 tons pulp/day kraft chemicals involved, several pieces process steam to be used internally in mill and assuming 65% energy recov- must be fabricated out of high purity the mill.

Idaho National Engineering Laboratory University Research Consortium . 61 alumina, which proved to have a long ing element made of nichrome wire Milestones for completion of the delivery time, as dictated by the has the required heat-up characteris- project are: Reaction conversion and ceramic vendor. The electrical heat- tics and corrosion resistance. rate data (Sept.); Hydrolysis rate data (Dec); Final report (Mar.).

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Chemical and Petrographic Characterization tered was with an HP workstation of Vitrification Products (V22) which affected milestone dates. The problems stemmed from the combi- Scott S. Hughes, Idaho State University nation of late vendor delivery, incomplete operating system, and insuffi- cient documentation. The company Co-PI and University: None recendy delivered a complete operating system so we see no reason at this Graduate Students: None time to suggest changes in overall Industrial Collaborator and Company: None objectives odier than to reassess milestone dates. During the coming year, INEL Collaborators: James D. Herzog, Thomas P. O'Holleran, Bruce Sta- we plan to investigate further the dif- ples, Richard A. Callow fusion rates of specified radionuclides and heavy elements. Using surrogate Presenter: Linda L. Davis, Post-Doctoral Research Associate, Idaho State elements, such as Th and U for University transuranics, various compounds will be added to crucible vitrification charges at specified locations to deter- Chemical and phase variations in directions of fractures. A crystalline mine their reactivity during the melt- vitrification products are being studied reaction rim 1.5-mm thick extends ing process. We hope that informa- to understand properties that will into the glass from the crucible. Vit- tion thus obtained will lead to better affect long-term storage or disposal. reous slag is vesicular, nearly opaque, compositions or methods used for Elemental mobility and incipient and appears to be strongly devitrified vitrifying hazardous waste. crystallization are evaluated in order or altered to clay minerals. At least to measure the degree of homoge- one sample has a network of long, nization and elemental diffusion. trellis-like, quenched crystals. Analyses by instrumental neutron Chemical analyses indicate a activation and inductively-coupled large degree of heterogeneity in trace plasma emission spectroscopy are element abundances within the glasses used in conjunction with polarizing while most major elements are uni- microscopy to construct three- form. Results also indicate large dis- dimensional maps of melter-treated crepancies between reported analyses materials. Samples that were analyzed of prepared mixtures and our actual during initial phases of the project analyses. Chemical co-variation consisted of (a) plasma hearth and arc between specific elements is as striking melter furnace test glasses to develop as the overall range in trace elements. analytical methodology, (b) black vit- Although there is crystallization, reous slag, actually Fe-enriched basalt, there is no removal of crystals from and (c) glass Zr-127, melted in a the melt in the crucible. These ceramic crucible, which is die focus intriguing results have prompted us of much of our experimental work. to begin designing tests to determine Zr-127 is made specifically for vitrifi- the source of the inhomogeneities. cation of calcined waste and consists Such co-variations of elements in a of high concentrations of Zr, F, B, crucible of Zr-127 melt cannot be and Li that would normally be found related to melt extraction from a solid as trace elements in rock or soil. source or crystal segregation from Petrography indicates that Zr- liquid. 127 contains as much as 50 volume Chemical analysis of the synthet- percent radiating crystals smaller than ic glasses is challenging with respect 0.1 mm and less than one percent to unusual spectral interferences and skeletal crystals (0.8-mm diameter). small sample sizes. Nevertheless, the Distribution of crystals is irregular most significant setback we encoun- suggesting potential for preferred

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Correlation of SREX and TRUEX Equilibrium Data cessfully imported into ASPEN. for Use with the ASPEN Model (V242) Comparisons to experimental data are under way. There are some differ- Thomas E. Carleson, University of Idaho ences between the earlier version and the current one that are not yet Co-PI and University: None resolved. Previous work indicates up Graduate Student: Gary Allen Lowe to 60% error between ASPEN predictions and experimental data for Industrial Collaborator and Company: None organic phase compositions. Work is continuing in an attempt to obtain INEL Collaborator: Arlin Olson, Lockheed Martin Idaho Technologies better agreement between the experi- Company mental results and ASPEN predic- Presenter: Gary A. Lowe tions. Milestones for This Year Progress is expected to continue Liquid-liquid extraction tech- extraction. Resulting subroutines with the SREX simulation and refine- niques to remove heavy and radioactive could also be useful to governmental ment of the subroutine, completion metals have been developed in recent laboratories such as Pacific Northwest of data regression to obtain UNIFAC years to reduce die volume of Laboratory, Oak Ridge, and Savan- coefficients, and comparison with radioactive waste. Methods to extract nah River. recent experimental data obtained strontium (the SREX process) and The Approach Taken from Law, Wood, and Herbst at transuranics (the TRUEX process) Idaho Chemical Processing Plant have been successfully tested and Project methods include writing (ICPP). found useful. ASPEN, a simulation a FORTRAN subroutine to predict A TRUEX model subroutine is program widely used to simulate distribution coefficients and using also expected to be developed to yield chemical processes, is equipped with this as a subroutine for ASPEN; cor- transuranic distribution coefficients. die capability to handle compounds relating experimental results (for both Extraction simulation using the not in its data Banks. SREX and TRUEX processes) to allow estimation of UNIFAC coeffi- TRUEX subroutine with ASPEN Objectives cients for species not in ASPEN's should be accomplished within the Overall project objectives include data bank; and comparing these year. Comparisons will be made with writing a subroutine used with results with an existing EXCEL the GTM to show accuracy of ASPEN to estimate distribution coef- spreadsheet for SREX and the Gener- ASPEN|s prediction of oudet stream ficients (Kd), using the ASPEN data alized TRUEX Model (GTM). Some compositions. regression package to predict UNI- of this work has been accomplished Milestones for the Future QUAC (Universal Quasi-Chemical) (see below). Functional Group Activity Coeffi- Regression of TRUEX experi- Major Accomplishments and Obstacles cients (UNIFAC), and comparing mental data should be done to obtain results with ASPEN's unaided estima- ASPEN Plus Release 9.2 was UNIFAC coefficients. Data from tions of the same system. obtained and installed on a computer regression results should be used in in the Chemical Engineering Depart- ASPEN to estimate exit concentra- Value of Project if Overall Objectives ment. A liquid extraction example (a tions in the ASPEN EXTRACT Are Achieved three stage water-acetone-ethyl model. Comparison should be made Successful completion of this acetate extraction) was performed in with GTM to show a correlation project will allow LITCO to use sub- ASPEN and compared to literature with existing estimation methods. routines and data generated at ICPP (Henley and Seader's "Equilibrium Future preparation of an ASPEN to model the required mass and ener- Stage Separation Operations in EXTRACT block for evaluation in gy balances necessary for RCRA Part Chemical Engineering" text) and ear- the ICPP process would be a benefi- B permits. ASPEN's optimization lier (1994) work with ASPEN. The cial milestone. These tasks will be and cost estimation programs could results agreed with earlier work. Cal- the subject of a future proposal to the then be used in implementing large culated distribution coefficients from INEL URC or a private company. scale operations of contaminant the SREX subroutine were also suc-

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Session 7. Organic Waste Treatment and Reduction

Wednesday, 8:00 a.m. to 11:30 a.m.

Kenneth A. Smith (MIT), chair David L. Miller (INEL), co-chair Edwin W. House (ISU), panelist Lloyd McClure (INEL), panelist

8:00 a.m. V29 Chikashi Sato Photo-Sololysis of Toxic Organics Using Ultraviolet Idaho State University Irradiation-Ultrasonication (UV7US) Processes

8:50 a.m. V228 Jeffrey J. Rosentreter Photo-Catalytic Assisted Chemical Treatment of Idaho State University Aqueous Cyanide Wastes

9:30 a.m. — Break

10:00 a.m. V12 Jackie Y. Ying Photocatalytic Decomposition of Halogenated Organics MIT Over Nanocrystalline Oxide Catalysts

10:45 a.m. V04 T. Alan Hatton Polymeric Solvents for Minimizing Pollution in Chemi- MIT cal Synthesis, Separations, and Cleaning Operations

11:30 a.m. Adiourn

Idaho National Engineering Laboratory 68 University Research Consortium

Photo-Sonolysis of Toxic Organics Using Ultraviolet Irradiation- Ultrasonication (UV/US) Processes (V29)

Chikashi Sato, Idaho State University

Co-PIs and University: Solomon Leung and B.K Lao, Idaho State Universit

Postdoctoral Research Associate: Jingshi Wu

Graduate Students: John S. Kirkpatrick, Mamunure Rashid

Industrial Collaborator and Company: Tom Dekker, Water Department, Pocatello, ID

INEL Collaborators: Bill Motes, Steven Hartenstein

Presenter: Chikashi Sato

The overall objective of the pro- sion well and a UV lamp, and c) a ject is to explore photo-sonolysis sonicator with a 139.7-mm cup horn. technology for the destruction of The system was so designed that the organic compounds in an aqueous contaminated solution is UV-irradiat- phase. The technology to be devel- ed from the inside (immersion well) oped would be used by both indus- and exposed to acoustic waves from tries and government agencies to treat the bottom. The contaminated solu- industrial wastewater and leachate tion is introduced into the bottom of from landfill/waste sites, and to clean the reactor, and the treated water is up surface and subsurface water cont- removed from the top of the reactor. aminated with biorefractory toxic Data will be collected soon. organics. Remaining tasks for FY-96 The batch photo-sonolysis reac- include the enhancement of the tor was constructed, which consists of UV/US treatment efficiency using

(a) an 800-ml quartz reactor vessel, hydrogen peroxide (H2O2) and/or (b) a photo-reactor chamber, and (c) titanium dioxide (TiO2). An attempt sonicator with a 12.7-mm horn. The will be made to identify intermediate system was so designed that the cont- byproducts using a GC/MS. aminated solution is UV-irradiated The milestones planned for the from the outside of the reactor vessel next year are completion of the and exposed to acoustic waves from design and construction of the pilot- the inside (in solution). We observed scale treatment unit, and market sur- photo-sonolysis of PCE as compared vey for the potential commercializa- with photolysis and sonolysis in the tion of the technology. reactor. With the solution containing PCE at 100 mg/L, more than 90% of the PCE was decomposed within 20 min.

The construction of a continuous flow reactor is in progress. The flow system consists of (a) a 1860 mL quartz reactor vessel to which contaminated solution is continuously introduced by a pump, (b) an immer-

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Photo-Catalytic Assisted Chemical Treatment of Aqueous Cyanide Wastes (V228)

Jeffrey J. Rosentreter, Idaho State University

Co-PI and University: None Graduate Students: Renee L. Bunde, H. Swantje Quarder Industrial Collaborators and Companies: G. Ryan Pattie, Laboratory Manager of Intermountain Analytical; John Dunkle, Applications Chemist, Greenspan Technology Ltd. INEL Collaborator: Kevin Gering Presenter: Jeffrey J. Rosentreter

The treatment and handling of All reactions utilized alkaline solu- acutely toxic aquatic cyanides are of tions in following the prescribed safe significant interest in industrial handling and storage procedures of process control and environmental the potentially hazardous cyanide protection. Our research has focused wastes. The investigation has imple- on the development and evaluation of mented various light sources includ- anionic cyanide treatment systems for ing far and near ultraviolet and a sim- aqueous waste streams. The treatment ulated solar source. Preliminary data technology is based on the homoge- has been evaluated to identify the neous and heterogeneous photochem- waste treatment product as a non- ical reactivity of solvated cyanide com- hazardous, non-regulated oxidation pounds. Many of these compounds product, cyanate. possess high stability constants and as An analytical device capable of a result are not amenable to routine sensitive real time analysis of cyanide oxidative treatment mediods such as ions has been designed, fabricated, chlorination and ozonation. Yet, and tested. This work became neces- these same chemical species have sary as a means of monitoring the proved to be readily photo-reactive. reaction products of our irradiation The treatment system incorporates the experiments. The detector is based use of semiconductor oxides as photo- on the use of quartz crystals. These catalysts. Through the use of cat- crystals display the piezoelectric effect alyzed photolysis, even highly stable when a d.c. potential is applied. anionic metal cyanide complexes have Using a recently developed flow cell been successfully dissociated. These and gold electrodes on the crystal, the dissociated anions are then oxidized system essentially produced a small utilizing either photo-catalytic or tra- and sensitive microbalance. Imple- ditional processes. mentation of selective reaction kinet- To date, the project has focused ics has produced a cyanide specific on the design and construction of a detection device. The result is a laboratory scale flow injection photo- detector capable of real time analysis chemical reactor, the identification of of cyanide solution concentrations. candidate photo-active cyanide An invention disclosure report has species, characterization of reactivity been initiated for this novel detection variables, and the investigation of var- system. ious semiconductor oxide catalysts.

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Photocatalytic Decomposition of Halogenated Organics Over Nanocrystalline Oxide Catalysts (V12) superior advantage in gas phase reactions due to its extremely high surface area and novel pore structure. The Jackie Y. Ying, Massachusetts Institute of Technology detailed study of effects of morphology, non-stoichiometry, Pt dispersion, Co-PI and University: None and pore structure on both liquid phase and gas phase reactions are also Graduate Students: Chen-chi Wang, Zhibo Zhang in progress. These fundamental stud- Industrial Collaborator and Company: Dan Chen, 3M ies will have critical impact on the successful development of photocatal- INEL Collaborator: Stuart Janikowsk ysis as a viable technology for solving pollution problems associated with Presenter: Prof. Jackie Y. Ying mixed waste and industrial volatile organic chemical waste streams.

Treatment of chemical wastes addition. Pure anatasc, rutile, or represents a significant challenge to mixed phase materials were also both the defense and commercial sec- derived. Photoreactivities of the vari- tors of the United States. Photocatal- ous TiC>2 samples were quantitatively ysis is an attractive low-temperature, evaluated by photocatalytic decompo- non-energy-intensive approach for sition of CHCB using an immersion- treating halogenated organics. This type batch reactor. Nanocrystalline project seeks to develop superior pho- TiO2 showed superior photoreac- tocatalytic materials with increased tivites, and 10 nm was found to be surface reactivity and reduced charge the optimum particles size for pure carrier recombination rate. Major TiO2 in decomposition of halogenat- emphasis is placed on the designing ed compounds. Fe^+ dopants in of a novel nanostructured TiO2-based quantum-sized (~5 nm) particles and system with tailored size, phase, dop- Pt loading on intermediate-sized (10- ing, stoichiometry, and Pt dispersion 30 nm) particles were found to sub- to substantially improve the quantum stantially enhance the overall quan- efficiency of the overal photoprocess. tum efficiency.

Nanocrystalline TiC^ with well A versatile projection type flow controlled size (5-100 nm) has been reactor has been constructed, which successfully synthesized through wet- allows us to flexibly control photon chemical methods such as chemical intensity and select desired photon precipitation and hydrothermal treat- wavelength. Combined with a mass ment. Transition metal dopants of spectrometer, the detailed kinetic controlled concentrations were intro- study in both liquid phase and gas duced to tailor the electronic struct phase reactions will be carried out ture of TiO2. Non-stoichiometric and all by-products can be carefully TiO2-x was also prepared by reducing measured. Photocatalytic decomposi- nanocrystalline TiC^ under flowing tion of CHC13> C1CH=CC12 (TCE), H2 at high temperature and by inert and CCI4 in gas phase are being gas condensation method. Pt metal examined using diis new optical set- dispersion on TiO2 particles was up. A novel hexagonally packed achieved by reducing FLjPtClg widi mesoporous TiOj material has been hydrogen, and citrate reduction was synthesized, and the processing vari- also exploited. TIO2 with different ables are exploited to make this mate- morphology such as sphere, spheroid, rial more stable and more suitable for and rod were generated in hydrother- photocatalysis applications. It is mal synthesis with different mineral believed that this material will have

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Polymeric Solvents for Minimising Pollution in Chemical an intelligent reaction/separation Synthesis, Separations, and Cleaning Operations (V04) sequence that improves upon currently used sequences in terms of both environmental impact and productivity. T. Alan Hatton, Massachusetts Institute of Technology Over the next year, we plan to Co-PI and University: None (a) synthesize a broader range of solvents with different chemical moieties Postdoctoral Associate: Minghui Zhang (started December 1996) and/or polymer backbones, (b) characterize these solvents in terms of Graduate Students: Linda Molnar (Graduated May 1996), Julie Sherman their solvation and transport proper- (Started January 1996) ties, specifically heats and entropies of Industrial Collaborator and Company: Michael P. Thien, Merck and Co. solvation, micro- and macroviscosities, micropolarities, and diffusion coeffi- INEL Collaborator: Robert Cowan cients of different components, (c) demonstrate a range of model reac- Presenter: T. Alan Hatton tions in these solvents, (d) develop process system models to assist in the optimization of the reaction/separa- Most processes used in the phar- lems must be avoided so that more tion sequence, and (e) conduct pilot- maceutical industry are, by necessity, efficient recovery of solvents is scale testing using these new solvents carried out in organic solvents. In facilitated. in collaboration with Merck (under many cases these solvents are volatile Facile synthetic methods have discussion); this will provide the ulti- and sufficiendy water-soluble to cont- been developed for both low molecu- mate test as to their utility in pharma- aminate air emission and aqueous lar weight and polymer bound deriva- ceutical and fine chemical processing. discharge streams, adding to the envi- tives of THF for use as replacement ronmental burden and the cost of solvents for THF. We have identified downstream processing and recovery one step in the synthesis of the orally operations. One example is the use active HIV-1 protease inhibitor of tetrahydrofuran (THF) as the sol- L-735,524 as a suitable model reac- vent for Grignard reactions which tion to use in the evaluation of these must be carried out under anhydrous novel solvents. This reaction is conditions. The desired product is known to be very sensitive to the sol- often obtained by aqueous precipita- vent medium and therefore represents tion, which gives rise to other pro- a critical test of our replacement sol- cessing problems owing to the solu- vents. Reaction kinetics, as well as bility of THF in the water phase, possible separation schemes necessary with which it forms an azeotrope. for regeneration of the low molecular Thus, THF must be recovered by weight and polymer-bound solvents azeotropic distillation. Solvent have been investigated. Both types of switches are also frequendy required solvent replacement have been very during processing, adding to the . successful in the replacement of THF. complexity of the overall process. The low molecular weight derivatized It is suggested that solvent solvents can be carried through sever- replacements combined with recovery al reaction steps thereby avoiding and recycling will be important in the cosdy solvent switches because of development of benign chemical their minimal water solubility and processes. For this approach to be volatility. The polymer-bound sol- successful it is crucial that appropri- vents, which are dissolved in a rela- ate solvation properties be attained in tively benign continuous phase, can the replacement solvent while ensuring be recovered from the process stream that the potential for environmental by ultrafiltration and regenerated for contaminations be minimized. Fur- re-use. Thus, it is envisioned that our thermore, difficult separation prob- replacement solvents can be part of

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Idaho National Engineering Laboratory University Research Consortium 77

Session 8. Advanced Reactor Technologies

Wednesday, 8:00 a.m. to 11:30 a.m.

Michael W. Golay (MIT), chair Ralph G. Bennett (INEL), co-chair David M. Woodall (Uof I), panelist Jim Lake (INEL), panelist

8:00 a.m. N14 Thomas Downar Advanced Spatial Kinetics Methods for RELAP5 Purdue University

8:45 a.m. N20 John H. Lienhard V Cooling Modules for Extremely High Heat Fluxes MIT

9:30 a.m. — Break

10:0 a.m. N19 Mamoru Ishii Development of Multi-phase Flow Sensors and Purdue University Diagnostic Systems

11:30 a.m. _ Adjourn

Idaho National Engineering Laboratory 78 University Research Consortium

Advanced Spatial Kinetics Methods for RELAP5 (N14) ly 100% were achieved. Overall the computational burden was reduced Tom Downar, Purdue University by over an order of magnitude and for a typical three-dimensional PWR model and a practical reactor tran- Co-PI and University: Paul Turinsky, North Carolina State University sient problem, much better than real Post-Doctoral Student: Hisham Sarsour, North Carolina State University time performance was obtained. In Graduate Students: Douglas Barber, Purdue University; Ugur Meryurek, July, testing was begun on the inte- North Carolina StateUniversity grated RELAP/NESTLE simulator at die Cooper BWR in Nebraska. Industrial Collaborators and Companies: Ashok Arora, SAIC, Reston, VA; K. C. Wagner, SAIC, Albuquerque, NM Continuing work on NESTLE includes the development of a multi- INEL Collaborators: R. J. Beelman, Jerry Judd grid acceleration method and an adaptive spatial mesh capability. The Presenters: Tom Downar, Paul Turinsky incorporation of the Multigrid (MG) acceleration method has been essentially completed and full solution High fidelity nuclear power plant deployment of the RELAP/Mod 3.2 capability at all spatial grid levels is simulators with advanced nodal neu- R/T as a training simulator. This will now possible. Testing of the mediod tron spatial kinetics methods pose a improve operator training by provid- is currendy in progress. formidable computational burden. ing a more accurate and realistic Work on time adaptive spatial INEL has recendy developed description of reactor behavior. Also, gridding capability has been initiated. RELAP5/Mod 3.2 R/T: a real-time this will provide an engineering quali- The specific activity undertaken best estimate neutronics/thermal- ty simulator on which proposed involves adding die capability to hydraulics simulator which utilizes design and emergency procedures NESTLE to complete a NEM consis- die NESTLE nodal kinetics code changes can be accurately and quickly tent collapse. It builds upon MG which was developed at North Car- assessed prior to implementation. capabilities, such as data structure for olina State University. The overall For the first time the nuclear industry different grids and determination of objective of the work in this project will be able to consolidate die com- coarse mesh homogenized group has been to investigate advanced putational basis for plant licensing cross-sections. The additional capa- computational methods that can sub- and operator training. bility required involves determination stantially reduce die execution time The primary focus of the of coarse node discontinuity factors of die NESTLE neutronics module in research here is on the NESTLE neu- (CNDFs). In addition, some early RELAP/Mod 3.2 R/T. The specific tronics code. During the past year an work on obtaining spatial discretiza- goal of this work is to achieve better advanced Krylov sub-space method tion error bounds associated widi die than real-time simulation capability NEM approximation has been com- with an incomplete domain decom- on a multi-processor computer. pleted. position preconditioner was devel- Successful completion of this oped and implemented in NESTLE. Completion of this continuing work will result in considerably more This method employs the Bi-Conju- work on NESTLE should further accurate and efficient predictions of gate Gradient Stabilized (BiCGSTAB) reduce the computational burden of reactor core performance widiin the method as idle base algorithm and is the spatial kinetics module in context of the overall system simula- accelerated by a preconditioner based RELAP/Mod 3.2 R/T and release tion. For operating plants this will on diree-dimensional incomplete LU more execution time that can be used remove conservatism used in past factorization. Parallelism is intro- to further improve die fidelity of the analyses that can be taken advantage duced via an innovative incomplete thermal-hydraulics module. of by increasing operating flexibility domain decomposition method. and thereby reducing operating costs. On a single processor, a substan- For plants under design such as the tial performance improvement was advanced LWR concepts, less conser- achieved compared to die standard vatism can be translated into reduced nested iterative (Chebyshev Outer- capital costs via improved design fea- LSOR Inner) method. On the DEC tures. However, the immediate bene- Alpha 2100 (250 MHz) multi- fit of this work will be dirough the processor, parallel efficiencies of near-

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Cooling Modules for Extremely High Heat Fluxes (N20) approach to reach a design that appears to overcome these difficulties. John H. LienhardV^ Massachusetts Institute of Technology In addition, coefficients of thermal expansion for the faceplate and the Co-PI and University: None heater must be closely matched to avoid fracture or delamination of the Graduate Students: R. Dahbura, H. Younis resistance heater. Industrial Collaborator and Company: S. J. Kim, IBM, Tuscon, Arizona In the year ahead, we will test and optimize the prototype at increas- INEL Collaborator: Chang H. Oh ingly high heat fluxes. Initial tests at 2 Presenter: John H. Lienhard V fluxes up to 20 MW/m will be used to prove-out the concept. Higher fluxes will then be attempted, probably using a second-generation module. We are developing cooling mod- the faceplate and to evaluate a num- Factors limiting the fluxes attainable ules that support heat fluxes in the ber of candidate materials for the with these modules will be identified range of 10 to 100 MW/m2. The faceplate. Among the most promis- and design rules for jet array cooling modules will use an array of high ing materials are certain refractory modules will be constructed. A few pressure impinging liquid jets and metals and copper-based metal-matrix areas that we expect will receive sig- will be self-contained, apart from a composites. Finite element simula- nificant attention are ( a) instrumen- liquid pumping/low flux cooling tions of the thermal and mechanical tation for power and temperature system. The jets cool the rear side of stresses are being used to optimize the measurement; (b) local convection a faceplate that absorbs the heat load faceplate thickness and the mechanical coefficients beneath the jet array, par- of interest. The faceplate will be a constraints applied to the faceplate. ticularly for high wall temperatures; thin, high conductivity surface, possi- Fluid flow simulations of the liquid (c) the use of metal matrix materials bly a refractory metal or a metal jet array are being used to assess the for the faceplate; (e) control of the matrix composite. This plate must be nozzle configurations. A prototype of stresses within the faceplate, and carefully designed to accommodate the cooling module is now nearing issues related to the plate's service life, both diermal stresses and the completion. The prototype module such as creep. mechanical load from die impinging uses small diameter water jets run- jet array. Development of these mod- ning at maximum speeds of 50 rn/s. ules involves experimental testing of (Past studies have used high speed the liquid cooling and manifolding water jets to remove fluxes of more performance and analysis of die ther- than 100 MW/m2 in the stagnation mal and mechanical stresses on the zone.) The faceplate is a dispersion- face plate. Potential applications strengthed copper alloy 2.5 mm include cooling semiconductor laser thick. The total cooled area is 10 cm2 arrays, microwave or RF components, and the design heat flux is 40 MW/m2. high-end microprocessors, x-ray opti- The module's lower liquid manifold cal components, and plasma diverters. and jet array are completed, and the Our objective is diat these modules upper manifold and faceplate should will be useful in a range of applica- be finished by mid-summer 1996. In tions without the need for any signifi- addition, we have built a flow loop to cant redesign. pump water through the cooling modules. The loop has been calibrat- Our approach is to apply analyti- ed and fully instrumented. The high cal and computational tools to design flux resistance heater has posed par- a prototype module. This module ticular challenges. Among these are will then be tested experimentally, the need to eliminate any contact using electrical resistance heating to resistance between the heater and the simulate the heat load. Analytical faceplate while providing electrical studies of the thermal stresses have isolation of the heat from,the face- been used to evaluate various plate. We have applied a thin film mechanical boundary conditions on

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Development of Multi-phase Flow Sensors conducted research for the feasibility and Diagnostic Systems (N19) of using impedance void-sensor and neural networks to obtain the void Mamoru Ishii, Purdue University distribution information. The preliminary results are promising. For the measurement of void wave veloci- Co-PI and University: L. H. Tsoukalas, Purdue University ty, the results are consistent with the Graduate Students: Ye Mi, Mulan Li, Zheng Xiao, theoretical prediction by the drift flux model. Industrial Collaborators and Companies: Bill Mortimer, Honeywell; Alexander G. Lissow, Scientech- The experimental and theoretical works have been carried out to mea- INEL Collaborators: Jim Anderson, Keith Condie sure characteristics of slug flow, such as averaged void fraction of both Tay- Presenters: M. Ishii, L. Tsoukalas, Y. Mi lor bubbles and liquid slugs, film thickness along Taylor bubbles, slug frequency, and slug and Taylor bub- The objective of the proposed The hardware of the system, ble lengths. It has been shown that research is to develop non-intrusive which is composed mainly of imped- the impedance void-sensor can be multi-phase flow sensors and diagnos- ance void-sensor and magnetic flow- used to measure most geometric tic systems applicable to advanced sensor, was successfully developed. information. light water nuclear reactor systems. The theoretical foundations of die In new generation nuclear power impedance void-sensor and magnetic The analytical solution of the reactors utilizing passive safety sys- flow-sensor have been established. response of electrical magnetic flow- tems, the development of reliable An experimental loop with a vertical sensor for some simple geometric ver- non-intrusive multiphase flow diag- 2-inch test section was built along tical two-phase flow has been nostic systems to monitor the func- with a PC-based data acquisition/ obtained and compared to the experi- tions of passive safety systems will be analysis system. The tests show that mental results. It is proved that the of crucial significance. The non- the hardware of the diagnostic system application of the magnetic flow-sen- intrusive systems can measure two- and the testing loop function veiy sor can be extended to slug flow. phase flow void fraction, perform well and can be operated under a In the next year, we will conduct flow pattern identification and output wide range of flow conditions to sat- our investigation in horizontal two- liquid mass flow by exploiting the isfy our research requirements. phase flows. mapping and flexible modeling capabilities of fuzzy and neural systems. For flow pattern classification, we Such non-intrusive multiphase flow have investigated and implemented sensor diagnostic systems would be of several kinds of neural networks or interest to the petroleum, refining, neural-fuzzy approaches, such as a food, and chemical industries as well, supervised neural network and a self- where not only the void fraction but organizing neural network, as well as also a measurement of the interracial a hybrid neural-fuzzy system. The structure could be achieved through capability of these neural networks to the proposed systems. classify flow patterns is tested and verified. During die past year, our major The application of the imped- efforts were focused on vertical two- ance void-sensor to measure some phase Jlows according to the project important two-phase flow characteris- schedule. Significant advancements tics is intensively investigated. The have been made in the theoretical, theoretical predictions and experi- computational and laboratory investi- mental results for the area-averaged gations of the project, based on hard- void fraction show very good agree- ware and equipment developed and ment, which is also cross-calibrated procured. They are documented by other techniques for averaged void briefly as follows. fraction measurements. We have also

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Idaho Nattonal Engineering Laboratory University Research Consortium 85

Session 9. Site Monitoring and Characterization

"Wednesday, 8:00 a.m. to 11:30 a.m.

Jefferson W. Tester (MIT), chair Rebecca A. Winston (INEL), co-chair Dale R. Ralston (Uof I), panelist Dave Caufrman, Bob Snelling (INEL), panelist

8:00 a.m. V219 Peter R. Griffiths Inexpensive Open-Path Atmospheric Monitoring with a University of Idaho Low-Resolution FT-IR Spectrometer

8:45 a.m. N10 William A. Hoff Evaluation of Interactive Techniques for the Creation Colorado School of Mines and Updating of Site Models for Remote Operations and Inspection 9:30 a.m. — Break

10:00 a.m. G14 Roger Turpening Borehole Seismology in Support of INEL's Ultra-Long, MIT Multi-Sensor Array Project

11:00 a.m. Adiourn

Idaho National Engineering Laboratory 86 University Research Consortium

Inexpensive Open-Path Atmospheric Monitoring monitor. The key difference will be with a Low-Resolution FT-IR Spectrometer (V219) the interferometer which will operate at a rate of 1000 scans per second. Since a car traveling at 70 miles per Peter R. Griffiths, University of Idaho hour will travel about 3 cm in the time of a single scan (1 ms), it will be Co-PI and University: None possible to measure a spectrum of the emissions from each car's tail-pipe Graduate Students: Robert L. Richardson (Mr. Richardson was awarded his immediately after it passes through Ph.D. on May 18 and will remain on the project as a postdoc), Brian K. Hart the IR beam. Using rapid digital sig- Industrial Collaborator and Company: J. D. Tate, Dow Chemical nal processing technology, it should Company, Freeport, Texas be possible to obtain the concentration of the major components of each INEL Collaborator: John G. Jolley car's exhaust by the time that the next car's exhaust gases are interrogat- Presenter: Peter R. Griffiths ed. (This is just one example of the type of application that can be attacked with an instrument of this There are two goals to this pro- main drawback to the use of a type: many more can be cited.) The ject. The primary goal is the devel- DLATGS detector is its low sensitivi- interferometer has been designed and opment of an instrument for open- ty relative to that of MCT. To allow an order placed for the key compo- padi atmospheric monitoring by most atmospheric species to be deter- nents; the first prototype should be Fourier transform infrared (FT-IR) mined at the low parts-per-billion fabricated by the end of the year. spectrometry. This instrument has level, the optical efficiency will be several features that differ radically increased by about a factor of 20 from existing designs. All contempo- through the use of a high-tempera- rary instruments incorporate a mer- ture infrared source fabricated from cury cadmium telluride (MCT) pho- MoSi2, highly efficient, short focal toconductive detector that operates at length transmitting and receiving 77K. These detectors are either telescopes, and a novel retroreflector cooled with liquid nitrogen (LN2) or that has been designed in our labora- by a Stirling cycle cooler. The former tory. Spectra will be measured at low method of cooling requires the dewar (about 8 cm-1) resolution, which also to be refilled regularly, while the life- results in a significant gain in sensi- time of Stirling cycle coolers is usual- tivity, especially for the determination ly about 3000 hours; thus completely of many volatile organic compounds unattended operation is precluded with molecular weights between 100 with either approach. We have also and 200. The study of all design demonstrated that MCT detectors parameters has been completed. Cus- usually respond in a very nonlinear tom-designed retroreflectors and tele- fashion to incident radiation, result- scope mirrors have been fabricated in ing in severe photometric errors. By our laboratory by spin-casting an contrast, our system is based on an epoxy resin as it sets. We expect to inexpensive deuterated L-alanine have a working prototype of this sys- doped triglycine sulfate (DLATGS) tem by the end of the year (December, pyroelectric bolometer which operates 1996). at ambient temperature or with ther- moelectric cooling. The photometric In the second part of this project, response of diis detector is not only is a new type of instrument for measur- far more linear than that of MCT ing automobile emissions traveling at but, by avoiding the need for LN2, highway speeds is to be built. This the instrument should operate for instrument will incorporate some, but several months unattended. The not all, of the optical components being developed for the open-path

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Idaho National Engineering Laboratory 88 University Research Consortium

use a stereo viewing system on a Evaluation of Interactive Techniques workstation, along with a 6 degree of for the Creation andUpdating of Site Models freedom input device. We are con- for Remote Operations and Inspection (N10) ducting evaluations to quantify the William A. Hoff, Colorado School of Mines benefits and tradeoffs associated with the interactive modeling techniques. For example, overly constraining Co-PI and University: Robert King, Colorado School of Mines many of the degrees of freedom of the Graduate Students: Frederick W. Hood, Khoi N. Nguyen, Torsten M. model improves the fit, but it may Lyon, Lin A. Xia overly burden the operator. * Industrial Collaborator and Company: Robert Taussig, Bechtel Corp.

INEL Collaborator: Mark McKay

Presenter: 'William A. Hoff

Graphical models are a useful human and machine can improve the tool for operators in the safe and effi- robustness and flexibility of computer cient planning and control of remote vision tasks. robots. With graphical programming The value of this work is that it systems, the operator can visualize can lead to productivity aids to lower and understand the result of complex the cost and improve the speed of commands before moving any remote operations. For large scale machinery. For diese systems, there is remediation operations, the cost sav- a need to dynamically create and ings can be significant. The results of update site models which accurately this work will transfer into INEL represent the 3D locations and other applications for remote characteriza- properties of objects at the site. tion and buried waste remediation. Unfortunately, automatic techniques The results will also potentially be for creating and updating models commercialized by Bechtel Corpora- from vision data traditionally have tion for use in their environmental been limited in performance and reli- remediation and construction field ability. It is possible to greatly operations. improve the performance of modeling systems by having the operator pro- Our approach is to use range vide constraints and guidance to the images from a stereo vision sensor, vision system. A key issue is to have although other range sensors can be the operator provide enough input to used. Our system allows the human the sensing system to achieve good operator to provide high level con- performance without requiring straints to the system, such as select- unnecessary effort by the operator. ing the type of object model to be The objective of the proposed work is used, and an indication of die to develop and evaluate a number of approximate location of the object. interactive techniques for fitting We then use automatic model fitting models of geometric primitives (such algorithms, based on simulated as cylinders, parallelepipeds, and annealing, to complete the exact fit- spheres) to objects in range images, in ting of the model to the data. The terms of performance (accuracy and user watches the graphics depicting reliability) and cost (time and effort the model fitting process and can by the operator). The goal is to show intervene if necessary to correct the how sharing of intelligence between fit or provide further constraints. We

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Idaho National Engineering Laboratory 90 University Research Consortium

Borehole Seismology in Support of INEL's Ultra-Long, Approach Multi-Sensor Array Project (G14) There are various numerical modeling techniques that are suited Roger Turpening, Massachusetts Institute of Technology for the computation of the seismic wave field in and around a fluid-filled Co-PI and University: Prof. M. Nafi Toksoz, MIT borehole. All methods have their advantages and their limitations but Research Scientist: Richard Gibson, Jr., MIT the finite difference method (FD) emerges as the most general. This is Graduate Students: None particularly true when a variable grid Industrial Collaborator and Company: Larry Walters, Bolt Technology, Inc. size is used and attenuation is included in the algorithm. The FD tech- INEL Collaborators: James R. Fincke; David M. Weinberg nique is computationally intensive and thus is only practical when used Presenter: Roger Turpening on a massively parallel computer. Industry support has installed a 512 node nCUBE with 100 gigabytes of Background of Technology has made major con- disc space at ERL and we in turn will tributions in this branch of seismolo- apply this computational power for The Idaho National Engineering gy with theoretical and experimental INEL's tasks. Laboratory (INEL) is undertaking a studies in borehole acoustics, logging, three-year project to design, engineer, vertical seismic profiling, cross-well Accomplishments build, and test a new downhole array tomography, and single-well imaging. of seismic sensors. The novel feature This is a new project just enter- of the project is that this array will Objective ing its second quarter. Therefore contain a large number (approximate- coordination activities have been the With this background ERL will ly 100) of individual sensor pods focus of this early phase. We have provide seismological support to (sondes). Each one of these sondes made some preliminary studies of INEL's engineering effort of the will carry a three-component geo- tube wave damper design. downhole array of seismic sensors. phone and will have the capability of This support impacts both the design Milestones Planned for Next Year clamping itself to the borehole wall. and testing phases of the array. Dur- We will focus on the tube wave This is a monumental undertaking ing the design phase, ERL will problems in the next year, in particu- and INEL should be applauded for pursuing this goal. 1. Numerically model seismic wave lar the design of tube wave dampers. propagation phenomena that This is a difficult problem since one The geophysical community impact the design of a sonde and wants a damper that indeed functions needs such a tool. A very promising its interconnecting cable/coiled as a damper and does not reflect the geophysical technique—single well tubing segments energy into a nearby sensor. imaging, much in demand by the industry—will not be commercially 2. Use numerical modeling to assist viable until a noise-free, long array in the design of tube wave exists. dampers

The fluid-filled borehole is a 3. Demonstrate the fundamental complex seismic waveguide that geophone/hydrophone processing affects not only seismic wave propa- techniques for tube wave rejection. gation and the behavior of noise sig- nals, but-also the response of seismic During the testing phase ERL will sources and receivers in the borehole. 1. Make our test site available for These problems are so distinct from field testing of the prototype those of layered earth models that tool; and they led to the development of a sub- discipline called borehole seismology. 2. Compute reception patterns of The Earth Resources Laboratory receivers in various borehole (ERL) of the Massachusetts Institute environments.

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Idaho National Engineering Laboratory University Research Consortium 93

Session 10. Environmental Sensors and Monitors

"Wednesday, 1:00 p.m. to 5:15 p.m.

Jefferson W. Tester (MIT), chair Rebecca A. Winston (INEL), co-chair Dale R. Ralston (Uof I), panelist Bill Blume, Dave Cauffinan, Bob Snelling (INEL), panelists

1:00 p.m. VI8 Harold E Hemond Remote Monitoring of In Situ Contamination Using MIT Optical Spectroscopy

2:00 p.m. V27 Kent R. Mann Synthesis and Characterization of Vapochromic University of Minnesota Materials for Environmental Sensors. Detection and Identification of Volatile Organic Compounds

3:00 p.m. — Break

3:30 p.m. V03 Joel Dubow Chemical Sensing Subsystem Components University of Utah

4:30 p.m. G219 Robert W. Gunderson Intelligent Fully Autonomous Micro-Robotic Control Utah State University Systems for Hazardous Waste Site Characterization

5:15 p.m. Adjourn

Idaho National Engineering Laboratory 94 University Research Consortium

Remote Monitoring of In Situ Contamination We have recendy completed Using Optical Spectroscopy (V18) assembly of a prototype probe that includes the microchip laser and optics to collect any fluorescence or Harold E Hemond, Massachusetts Institute of Raman scattered light for transmis- Technology sion via optical fiber to a distant data acquisition system. Initially, we have Co-PI and University: None examined the optical signatures of dilute aqueous solutions of contami- Graduate Student: Joe Sinfield nants. However, the signal character- Industrial Collaborators and Companies: Terry Hawk, EG&G Environ- istics will depend on the surrounding mental, Inc.; Joda Wormhoudt, Aerodyne, Inc. soil matrix. Therefore, we have also constructed a laboratory apparatus to INEL Collaborator: Judy K. Partin test the probe with different soil types at varying levels of contamination. In Presenters: Nathan Newbury, MIT Lincoln Laboratory; Joe Sinfield parallel with these laboratory tests, we will shortly perform preliminary field tests to determine the probe durability Millions of acres of soil and instead by detecting the Raman scat- and background signal levels. After groundwater within the United .States tered photons, which are laser pho- these tests, we plan to deploy the are potentially contaminated with tons scattered from the molecule and probe in a well-characterized contam- wastes, including, for example, petro- shifted in energy by a characteristic inated site the summer of 1997 in leum based hydrocarbons (e.g., amount. Both LIF and Raman spec- order to characterize the probe BTEX compounds) and chlorinated troscopy are amenable to in situ performance under real operating solvents. All clean-up of these conta- screening of sites since remote fiber- conditions. minated lands requires quantitative optic probes can be delivered down assessment of the degree of contami- existing wells or in cone penetrometer nation both before and during reme- shafts. Unfortunately, the few exist- diation efforts. Conventional sensing ing efforts in remote fiber spec- techniques, which require sample troscopy all suffer from the same extraction and subsequent on-site or drawbacks, namely the lasers are laboratory analysis, are too slow and bulky, expensive instruments and sys- labor intensive for the vast amount of tem ranges are limited because UV land targeted for evaluation. Thus, radiation does not propagate well in there is an acute need for a reliable, optical fibers. inexpensive, and real-time method to measure chemical concentrations in The objective of our research is situ in die soil and water environment. to develop and deploy a remote sensor that overcomes the aforemen- In recent years, remote optical tioned limitations by exploiting a spectroscopy has evolved to address recendy developed UV microlaser. this need. The techniques most often The laser consists of a near-infrared employed are laser induced fluores- 1-Watt diode pump coupled, via cence (LIF) and Raman spectroscopy. multi-mode silica fiber, to a series of In LIF, chemicals such as the BTEX small (millimeter-scale) crystals, compounds are excited by an ultravi- which produce short pulses of ultraviolet laser. The spectral and temporal olet and visible radiation. Because of properties of the subsequent fluores- the high transmissivity of optical fiber cence is used to identify specific in the near infrared, the diode pump chemicals. Chlorinated solvents, such can be located above ground while as carbon tetrachloride and TCE, will the UV-lasing crystals are incorporat- not absorb ultraviolet light in an easi- ed within the probe itself, thereby ly accessible wavelength region. avoiding fiber optic attenuation of These compounds are identified the UV radiation.

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Idaho National Engineering Laboratoty' 96 University Research Consortium Milestones Achieved Synthesis and Characterization of Vapochromic Materials for Environmental Sensors: Detection and Identification of Volatile • The synthesis and characteriza- Organic Compounds (V27) tion of two types of vapochromic platinum compounds and a com- Kent R. Mann, University of Minnesota pletely new class of vapochromic • compounds. Co PI and University: None • The production of samples for INEL testing. Graduate Students: Christopher Exstrom, Charles Daws, Marie Pomije, Daron Janzen, Carolyn Anderson, Jon Eyju • Mechanistic studies were reported in two manuscripts. Industrial Collaborators and Companies: John E. Trend, 3M; Alex Burns, Life Sciences, Inc.; Dennis Levens, 3M • A ccd based absorption/emission spectrometer is under construc- INEL Collaborators: Steven Hartenstein, Frederick E Stewart, Glenn tion for future studies. Moore Future Objectives Presenter: Kent R. Mann • Completion of additional mechanistic studies with the [Pt(phenanthroline) (p-CN- Goals The synthesis and characteriza- C6H4-CnH2n+1)2] [Pt(CN)4] A long-term goal is to develop tion of mixed salts of the form compounds. Substituted precur- and commercialize a hand-held fiber [Pt(bipyridine/phenanthroline) (p- sors will be synthesized. We optic based device that could identify CN-C6H4-CnH2n+1)2] [Pt(CN)4] expect all of these compounds to and quantify volatile organic com- (n= 6, 8, 12 for bipyridine; n= 6, 10, be vapochromic. pounds (VOCs) in air at regulatory 12, 14, 16 for phenanthroline). levels. Such a device would aid in These eight compounds offer out- • Develop an improved synthesis 2 pollution detection and monitoring standing stability improvements over of the [Ru(bpy)(CN)4] ' anion of waste sites. the previously studied vapochromic and related compounds. These compounds. The n = 6 compound is synthetic developments are Objectives exclusively a vapochromic alcohol straight forward and will produce To synthesize, characterize and detector; the n = 12 compound many new compounds. study new vapochromic compounds detects a broad range of organic func- • New mechanistic studies with the that undergo reversible color changes tional groups. The n = 12 compound diode array/CCD NIR fast time- when exposed to VOCs. The vapoc- could form the basis of an alcohol/ scale emission/absorption instru- hromes will be the chemically sensitive chlorinated hydrocarbon sensor. layer for the environmental sensor ment will allow sensitivity and that will use absorption or emission Mechanistic studies and an x-ray selectivity issues to be investigated. structure of [(n-C H ) N] [Pt(CN)4] spectroscopy for signal transduction. 4 9 4 2 • Continued development of neutral These compounds may also find were completed. [(n-C4Hc))4N]2 Pt compounds as vapochromes. application in air quality monitors, [Pt(CN)4] is vapochromic in the UV monitoring badges, alkane detectors, and IR regions of the spectrum. Proposed Milestones and ground water monitors. Mechanistic studies with this com- • Quarterly/Final reports of future pound answered a major question: Major Accomplishments studies. the CN groups of the anion are The synthesis, characterization important interaction sites for polar • Delivery (as per proposal) of at and Vis-NIR-IR vapochromic/ spec- or hydrogen bonding VOCs. least 100 mg of the three best troscopic studies were concluded for VOC sensitive materials available. isonitrile compounds of the form The synthesis and characterization of salts of 2,2'-bipyridine-tetra- These three will either be Pt salts, [Pt(arylisonitrile)4] [Pt(CN)4] (where neutral Pt or the pseudo-octahedral arylisonitrile = />-CN-CgH4-C H i; cyanoruthenate, [Ru^pyXCN)^". n 2n+ compounds. n = 6, 10, 12, 14). These compounds These compounds are prototypes of a represent a significant improvement new class of vapochromic compounds 3. Submit additional manuscript^) over the previous vapochromic com- that are not based on the Pt Pt or Pt for publication in a technical pounds available; we are applying for Pd stacking chromophore. journal. patent protection.

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Chemical Sensing Subsystem Components (V03) ing programs for wrist mounted chemical sensing systems, with Geo- Professor Joel Dubow, University of Utah centers on spin coatable solution stabilized vapochrome coatings, with Co-PIs and Universities: Ian Hunter, MIT; Lawrence Sadwick, University Attwood Technologies on parameter of Utah estimation and with the University of Minnesota on the effectiveness on Program Investigator: Douglas Chinn, University of Utah various vapochrome compounds. Graduate Students: John Madden, MIT; Luis Ortiz, MIT; Wenjia Zhang, The program has made signifi- University of Utah; Jeremy Riley, University of Utah cant progress in all areas. Prototype pump designs have been developed Industrial Collaborators and Companies: Bruce Nelson, Geocenters Inc., for polymer and silicon pumps West Newton, MA; Franco Consadori, Attwood-Technical Systems, Salt including lorentz force actuators Lake City, Utah (silicon and metal), peristaltic and INEL Collaborator: Steven Hartenstein, Chemical Systems Group membrane pumps (polymer) and polymeric bilayer gas flow modulation Presenter: Joel Dubow valves. Chemical field effect transis- tor wafers fabricated at MIT and coated with four types of vapochrome The objective of this project is to components of these modules on a and high qualitative sensitivities to develop modular, miniature chemical polymer substrate. This will include VOC's measured. Quantitative sensi- sensing system components for a a polymer battery and a conductive tivities will be determined before the wide range of applications. The com- polymer antenna for telemetry.This end of this contract period. A novel ponents include an inlet sampling will be ultimately more reliable since inkjet coating technique has been valve and gas flow modulator, chemical it will eliminate the need for coated developed to allow coating the fet field effect transistors, and nonlinear sensors. gates directly A wafer for evaluating parameter estimation software. The various polymer actuator concepts If successful, the project will hardware components are fabricated has been designed. Alternative poly- yield a family of wrist mountable and using silicon and polymer microma- meric detector compounds have been field deployable chemical sensing chining technology for the inlets, 1 studied. Volterra series parameter systems that are presendy unavailable micron CMOS fabrication technolo- estimation techniques have been and which will provide new capabilities gy for the chemical field effect tran- reviewed to improve selectivity and a for integrated chemical and biological sistors, and full 32 bit digital signal system designed to test these concepts. monitoring systems. Application of processing hardware for the parame- these systems include front end ter estimation. The initial effort has By die end of the next contract components for military and law focused on chemfets using coatings of period the system will be integrated enforcement chemical and biological the cyanoplatinate compounds devel- into a prototype miniaturized field detection and command and control oped by URC partners INEL and the testable sensing system will be deliv- systems, workplace monitoring, University of Minnesota, this effort ered to INEL for evaluation. Efforts worker protection for hazardous loca- will evolve into cyanoplatinate solu- will continue to develop a new line of tions, medical and home monitoring tions cofabricated into polymeric business based on this technology in for potentially hazardous substances. chemfets. The initial approach also partnership with INEL. Since detector arrays will be fabricated uses silicon technology, but the focus using VLSI techniques, these systems beginning next year, will be on mov- will provide an ultimately low cost, ing to all polymer inlet pumps and flexible means of adapting to a range transistors because of their inherent of sensing targets. advantages in compatibility with sensing chemical, performance and The program is tightly coupled adaptability. Our laboratory has the to INEL, to our industrial collabora- nations first polymer microfabrica- tors and to the University of Min- tion facility, and our extended project nesota INEL URC collaborator. We goal is the co-fabrication of all the are working with INEL on develop-

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Intelligent Fully Autonomous Micro-Robotic Control Systems be joindy defined with INEL and the for Hazardous Waste Site Characterization (G219) project commercialization partner, Caterpillar Inc. Robert ^W. Gunderson, Utah State University With numerous waste hazardous waste sites occurring in the surround- Co-PI and University: Nick Flann, Utah State University ing regions of Southeastern Idaho and Northern Utah, INEL has a Graduate Students: Steven Clarke, Brett Hancey, Eric Poulsen, John regional as well as national interest in Jacobs meeting the challenges of hazardous waste site characterization and reme- Industrial Collaborator and Company: Mel Greenhalgh, Caterpillar Inc. diation. The usefulness of this pro- INEL Collaborator: Robert Polk ject will be measured by the extent to which it contributes to the success of Presenter: Robert Gunderson INEL and the DOE in satisfying these demands, as well as by the extent to which it helps INEL to The principal research objective anticipated in integrating the vehicle identify and develop new roles in sat- of the project is to develop a fully hardware and path planning software isfying this nation's needs. autonomous micro-robotic vehicle systems on-schedule by the end of system for hazardous waste site char- August 1996. acterization, employing a new hybrid One of the major objectives of path planning technique for optimal this project has been to collaborate mission execution. This method is with INEL in identifying additional based on integrating off-line rein- uses for the results of the research forcement learning for rough plan- leading to the definition of new roles ning with a unique fuzzy logic and missions which satisfy national approach for obstacle detection and needs. It is becoming clear that the avoidance. T he idea is to greatly results obtained to-date, especially the reduce the need for detailed knowl- autonomous cooperative robotics edge of site environment by relying aspects, have interesting and poten- on the fuzzy logic system for local, tially significant applications for path execution, with the off-line rein- automating the effective, but highly forcement planner responsible only labor intensive, practices of prescrip- for global path supervision. The tion agriculture. A joint university- approach lends itself remarkably well INEL field demonstration of the dual to integration of fully autonomous (agricultural and hazardous waste cooperative robotic vehicle mission site) applications of this research is operations. currendy scheduled for the first week Significant progress has been of September 1996. made during the first seven months Two major milestones have been of the project. All of the milestones set for the end of month 6 and the set for this period have been met, end of month 12 next year. Develop- including readying a scaled up (by a ment of the sensor and software sys- factor of 1.7) ARC III vehicle for tem for dynamic obstacle detection assembly and system integration, on- and avoidance is to be complete by schedule the first week of June 1996. the end of the 6th month. By die The path planning software subsys- end of the 12th month, systems defi- tem was also completed on-schedule nition and specifications and prelimi- June 1, 1996, with its algorithms nary hardware and software develop- shown to be fully functional in arbi- ment of a 'black box' retrofit con- trary, partially unknown, simulated troller-path planner is to be complete. environments. No difficulties are Specifics of the latter milestone will

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Idaho National Engineering Laboratory 102 University Research Consortium

Idaho National Engineering Laboratoty University Research Consortium 103

Session 11. Materials Processing and Control

"Wednesday, 1:00 p.m. to 5:00 p.m.

T. Alan Hatton (MIT), chair James A. Seydel (INEL), co-chair E H. (Sam) Froes (Uof I), panelist Jim Key (INEL), panelist

1:00 a.m. N135 Jung-Hoon Chun A Real-Time Solidification Front Monitor for the MIT Continuous Casting of Metals

1:45 a.m. G22 Kevin L. Moore Advanced Welding Control Technology Idaho State University

2:45 a.m. — Break

3:15 a.m. G04 Merton C. Flemings Sensing in Advanced Solidification Processing Systems MIT

4:05 a.m. G12 Uday B. Pal Inclusion Free Refining of Molten Metals Using Short MIT Circuited Solid Electrolyte Cells

5:00 a.m. — Adjourn

Idaho National Engineering Laboratory 104 University Research Consortium

A Real-Time Solidification Front Monitor for the Continuous Casting of Metals (N135)

Jung-Hoon Chun, Massachusetts Institute of Technology

Co-PIs and University: Richard C. Lanza and Nannaji Saka, MIT Graduate Students: Mark M. Hytros, Imad Jureidini, Dongsik Kim

Industrial Collaborators and Companies: G. Hildeman and H. Yu, Alcoa; J. Gallenstein, US Steel; I. Saucedo and H. Pielet, Inland Steel; J. Dorri- cott, IPSCO Steel; E. Schonauer, AISI

INEL Collaborators: Dennis C. Kunerth, Timothy Roney

Presenters: Jung-Hoon Chun, Richard C. Lanza

We are developing an industrial- ried out at MIT's Bates Linear Accel- scale high-energy computed tomogra- erator Laboratory, where a shielded phy (CT) sensor to monitor the facility is being built. The x-ray solidification of metals during the source is a 6-MeV, 300 rad/min linear continuous casting process in real- accelerator. A controlled solidifica- time. The shape and location of the tion platform will create steady-state solidification front play a significant solidification profiles in a laboratory role in affecting the productivity of environment. The solidification plat- casting operations. By monitoring form consists of a furnace capable of the solidification front, one can opti- melting aluminum and its alloys, an mize the quality of the casting by air-cooling system, and a thermocou- reducing such defects as inclusions, ple-based data acquisition unit to cracks, and macrosegregation, in monitor the location of the liquid/ addition to optimizing the process by solid interface. An array of cadmi- increasing production rate and elimi- um-tungstate scintillation detectors nating breakout accidents. will measure the transmitted x-rays.

The technique behind the sensor The project milestones for the is based on the principles of CT and coming year are to have all the com- the attenuation of high-energy x-rays ponents of the laboratory system through a solidifying strand. The assembled and operating properly, to densities of liquid and solid metals conduct CT scans on phantom differ by as much as 4 to 12%. Thus, objects to determine baseline opera- it is possible to measure the intensity tion, and to begin detailed testing of transmitted photons through a sec- and analysis of sensor performance on tion of strand to determine the relative the solidification front profile of alu- proportions of the solid and liquid minum alloys. phases. With the application of CT, two- or three-dimensional images of the density distribution within the strand, and thus the solidification front, can be generated. At present, the project is in its first phase of development: laboratory-scale development and testing of a prototype system. This will be car-

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Idaho National Engineering Laboratory 106 University Research Consortium

Advanced Welding Control Technology (G22)

Kevin L. Moore, Idaho State University

Co-PI and University: D. Subbaram Naidu, Idaho State University

Post-Doctoral Fellow: Lyndon Brown (six months FY-96 only)

Graduate Students: Robert Yender, Justin Tyler

Industrial Collaborator: H. Redding, V.P., Eagle Rock Manufacturing

INEL Collaborator: John A. Johnson

Presenter: Kevin L. Moore

The Advanced Welding Control INEL. Current activities are focused Technology project is a University/ on characterizing, both theoretically INEL/Industry collaboration working and experimentally, the capabilities of to develop methods for controlling the constant-power control scheme; gas-metal arc welding (GMAW) completing the experimental facility processes, with an emphasis on the at ISU; and studying alternate control control of the mass and heat properties strategies for the GMAW system, of the process. Project activities to including artificial intelligence date have included: building the methodologies and advanced control personnel and equipment infrastruc- of weld pool thermal properties. ture needed to support project activi- Planned activities for the final phase ties, including an automated welding of the project include continued con- laboratory at ISU; carrying out basic troller design and validation; proto- research, in collaboration with INEL, type development in collaboration aimed at modelling the GMAW with an industrial partner; and plan- process for controller design; and ning for turn-key software/hardware. development of a novel constant- implementation of the controllers power GMAW controller, which has that have been developed. been validated experimentally at *

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Idaho National F.ngiin^ng Laboratory 108 University Research Consortium

Sensing in Advanced Solidification Processing Systems (G04)

Merton C. Flemings, Massachusetts Institute of Technology

Co-PI and University: Anacleto Figueredo, MIT

Graduate Student: Yusuf Sumartha

Industrial Collaborators and Companies: Paul Mikkola, GM Powertrain; Keith Thompson, Dynacast Inc.; William Eisen, Crucible Research;

Jere Brophy, Brush Wellman

INEL Collaborator: None

Presenter: Prof. Merton C. Flemings

The aim of diis research is to have been made using aluminum and develop advanced sensing methods aluminum alloys, and 6 runs using for studying the flow and rilling of copper alloys. The video camera is die castings, using prototype labora- seen to be an excellent method of tory equipment to simulate the die measuring flow velocities through the casting process. A second, longer gate, and of determining the charac- term, aim is to study die deteriora- ter of the flow front as it emerges tion under severe thermal conditions. from the gate. Thermocouple Die casting, including semi-solid response times of less than a second forming are processes of central have been achieved thus far, and importance to production of modern, work will be undertaken in the com- reliable, economic, fuel efficient ing months on optical pyrometry. automobiles. This program seeks to Emphasis of current work is on contribute to process reliability and commercial aluminum Alloy 413 economics in a significant way. (Al-Si of approximately eutectic composition). Copper alloy being Laboratory equipment has been ' studied is Cu 37.8% Zn. Tests show developed for the study which com- that for higher melt temperatures and prises (a) a melting and holding fur- long flow times, accelerated die ero- nace, (b) a channel with test mold sion is readily obtained under highly material comprising the "ingate" controlled conditions of melt temper- portion and a transparent material ature and flow. comprising die "die cavity, and (c) apparatus to apply a controlled vacuum During the coming year we to draw the metal into the die cavity anticipate meeting the milestones at controlled rates. Advanced instru- originally laid out for the program, mentation being tested or employed including die life testing and initia- in our experiments are (a) a state-of- tion of tests on metal matrix compos- the-art video camera capable of a ite slurries and semi-solid slurries. frame speed of 40,500 frames per second and a spatial resolution of 64 X 64 pixels, (b) high speed optical pyrometry, and (c) fast response thermocouple pyrometry.

To date, approximately 50 runs

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Idaho National Engineering Laboratoiy 110 University Research Consortium

Inclusion Free Refining of Molten Metals Using Short Circuited Solid Electrolyte Cells (G12)

Uday Pal, Massachusetts Institute of Technology

Co-PI and University: Harold R. Larson, MIT

Graduate Student: Prashant Soral

Industrial Collaborator and Company: Brad Schroeder, Reading Tube Corporation

INEL Collaborator: Ronald Mizia

Presenter: Harold R. Larson

The objective of this project is to and applied voltage doesn't help and scale up die concept of deoxidizing can be destructive to die electrolyte. metals by means of solid electrolyte Thermal shock problems have been cells to a unit diat can be demon- resolved, and we believe we have a strated on copper deoxidation in a cell design diat will withstand the plant environment. Technical diffi- plant environment. Copper has been culties limiting die industrial applica- successfully deoxidized to levels below tion of the approach will be identified 10 ppm. The solid electrolyte tubes and resolved. Data will be acquired must be coated with cermet on die to permit a detailed analysis of the inside surface to provide current col- economic viability of the process. lection and minimize contact resis- The project involves bodi laboratory tances. The cermet coating protocol (MIT) and plant testing (Reading and assembly procedure is being opti- Tube Corporation). Copper is tradi- mized based on laboratory tests. tionally deoxidized by reaction widi Progress has been significant. The copper-phosphorus additions. This plant test fixture will have 55 cells results in phosphate slag inclusions in and a total exposed surface area of die final product, and undesirable about 625 square inches. We are amounts of phosphorus in solution in evaluating die applicability to odier copper, bodi of which are detrimental metal systems. In die next program to the properties of copper. Earlier year we will complete plant trials on laboratory tests have shown that elec- copper, and design a second genera- trolytic cells can deoxidize copper tion pilot test apparatus. Cell life in widiout introducing any foreign ele- die industrial environment will be ments at rates that could be of indus- determined, and process economics trial interest. A pilot test fixture has will be quantified. Testing on a sec- been designed and fabricated, and die ond, industrially important, applica- plant test site is being prepared. tion will be proposed.

In die laboratory, we have found * diat at dissolved oxygen contents above about 300 ppm die deoxidation kinetics can be enhanced by a factor of two or three by applying external voltage. Below diis concentration oxygen diffusion in die metal becomes important (rate limiting),

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Session 12. Membrane and Adsorption Separation

Wednesday, 1:00 p.m. to 4:30 a.m.

Kenneth A. Smith (MIT), chair David L. Miller (INEL), co-chair Edwin W. House (ISU), panelist Jim Delmore, Lloyd McClure (INEL), panelists

1:00 a.m. VI9 Mark M. Benjamin Waste Component Separation and Volume Reduction University of Washington of an Acidic, Heavy-Metal Bearing, Low Level Liquid Radioactive Waste

1:55 a.m. N163 John D. Lamb Novel Separation Systems for Waste Processing and Brigham Young University Resource Recovery Based on Macrocyclic Ligand Complexation

2:35 a.m. — Break

3:05 a.m. V101 F. P. McCandless Membrane Processes for the Recovery of Radioactive Montana State University Species from Acidic Solutions

3:45 a.m. V250 Christopher W.Allen Improved Phosphazine Polymers for Membrane University of Vermont Technology

4:30 a.m. Adjourn

Idaho National Engineering Laboratory 114 University Research Consortium

Waste Component Separation and Volume Reduction step to remove the residual dissolved of an Acidic, Heavy-Metal Bearing, hazardous metals from the water and Low Level Liquid Radioactive Waste (VI9) non-hazardous salts. Solid/liquid separation after the precipitation and adsorption steps could be accom- Mark M. Benjamin, University of Washington plished by crossflow microfiltration.

Co-PI and University: None The heavy metal precipitation/ adsorption portion of the treatment Graduate Student: Lloyd E. Voges process and the membrane microfiltration step have been investigated Industrial Collaborator and Company: Andro Wipplinger, The Boeing using two forms of iron oxide (amor- Company, Environmental Affairs Department phous ferrihydrite and crystalline INEL Collaborator: Tom P. O'Holleran goethite) as adsorbents and filtration aids. Both simulated and real waste Presenter: Mark M. Benjamin streams from an electroplating facility were investigated. Using either iron oxide, the permeate concentrations from the microfiltration process were Low-level liquid radioactive metal/salt residue. The LLLW also consistendy below 50 mg/L for each wastes (LLLW) are currendy stored or contains non-acidic nitrates that can- metal. Ferrihydrite had a higher will be generated from future process- not be evaporated from the unmodi- capacity for metals than an equivalent es at ICPP. Treatment options for the fied waste. Although nitrates remain- mass of goethite, but goethite caused LLLW include waste component sep- ing after evaporation do not con- less resistance to permeate flux. Each aration, volume reduction, immobi- tribute acidity to the residue, they are was capable of releasing concentrated lization and disposal. undesirable because they interfere metals to an acidic regeneration solution. with the ultimate immobilization of The objective of diis project is to the residue in a grout. To our knowl- develop methods of separating the Additional testing is planned to edge, sulfate ions do not have this waste components while minimizing study nitric acid evaporation from drawback. Therefore, one manage- the volume of each component, and concentrated metal and salt solutions ment option is to replace the residual especially of the hazardous compo- and treatment of the metal/salt nitrates with sulfates. In tests per- nents. The components of the LLLW residue. The latter component will formed to date using simple mixtures are metals (0.5 M), acid (1 to 2 M), include a study of the regeneration of nitric acid and sodium nitrate to sodium (1 M), nitrates (2 to 3 M) and reuse of the iron oxide adsor- simulate the nitrate-containing com- and other salts (<0.2 M). Separation bents. Achievement of the research ponents of the LLLW, we have suc- of metals is conventionally performed objective will allow volume reduction ceeded in removing almost all the using hydroxide precipitation. Pre- of the disposed hazardous wastes and nitrate from solution and recovering cipitation requires that the acidity of segregated disposal of the nonhazardous it as nitric acid. the LLLW be neutralized or removed. components. S uccessful results of the iron oxide treatment stage studies Whereas conventional neutralization Treatment of the residual metals can also be applied to improve waste of the acid with a base would increase and salts might involve dissolution in treatment operations at electroplating the salt concentration in the system water followed by precipitation of facilities. considerably, separation of the acid metals, solid/liquid separation, and from the aqueous phase would not. adsorption as a polishing step. The Furthermore, since acids are required most concentrated metals in the in parts of the process, separation of residual are aluminum and iron. the acid presents the potential to reuse With proper pH control, these two it, rather than purchasing additional non-hazardous metals can be precipi- acid and generating even more salt- tated as hydroxides while leaving the containing wastes. hazardous metals in solution. The hazardous metals can then be precipi- The dominant and most volatile tated to generate a small volume of acid in the LLLW is nitric acid. Evap- solid hazardous waste, in conjunction oration of the nitric acid and water with or followed by an adsorption from the LLLW would leave a

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Idaho National Engineeiing Laboratory 116 University Research Consortium

Novel Separation Systems for Waste Processing and Resource Recovery Based on Macrocyclic Iigand Complexation (N163)

John D. Lamb, Brigham Young University

Co-PI and University: None

Visiting Researcher: Alexander Y. Nazarenko, D.Sc.

Graduate Student: Tatiana Levitskaya

Industrial Collaborator and Company: IBC Advanced Technologies, Inc

INEL Collaborator: Robert Lash

Presenter: J. D. Lamb

A novel polymer material com- tial use in coalescence extraction. posed of cellulose triacetate as support, Extraction experiments were per- different octyl ethers as plasticizers formed to compare measured extrac- (solvents) and crown ediers as carriers, tion constants values to those was investigated as solid extractant for obtained using traditional solvent sys- metal ion sorption and as a membrane tems. Extraction constants values for material for ion transport. Selective dinitrile solvents were ten to twenty sorption and transport of Sr(II), times higher than those for tradition- Pb(II), U(VI), Ga(III) and Fe(III) al solvents. was investigated. A difrusion-limited Commercial polyethylene oxides transport model has been found to and crown ethers form a second accurately describe metal ion trans- phase when trichloroacetic acid is port by crown ethers in diese systems. added to an aqueous solution. This The influence of counter- ion on liquid phase is stable at high concen- sorption and transport processes was trations of HNO3 and NaNO3, investigated. The membranes are being convenient for selective metal easy to prepare in the laboratory, ion extraction. Experiments show highly stable, and they may be useful complete extraction of lead in this in different separation and concentra- system. tion procedures.

A number of new solve'nt extraction systems were studied for poten-

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Membrane Processes for the Recovery of posal because a graduate student was Radioactive Species from Acidic Solutions (VlOl) not available for the project because of die timing of release of funds for the project. F. P. McCandless, Montana StateUniversity If this project is continued, Co-PI and University: None emphasis should be on the develop- Graduate Students: None ment of a membrane diat has a greater selectivity than for those Industrial Collaborator and Company: Randi Wright Wytcherley, Glitsch observed for the ordinary diffusion Technology Corporation process investigated to date. This might be accomplished by facilitated INEL Collaborator: R. Scott Herbst transport and/or other means of Presenter: F. P. McCandless selectively complexing specific ions in the feed or strip solutions.

This research addresses Cs and Sr tion containing XQJ = 0.001 by a fac- removal from acidic solutions of dis- tor of 1000, while increasing the Cs solved Idaho Chemical Processing concentrattion in the heads product Plant high level waste calcines and aby factors of 10 and 100. The liquid sodium bearing waste. Effec- results of the modelling indicates diat tive methods for the separation of Cs the countercurrent recycle cascade are not well established. Selective configurations are required to make separation of radioactive constituents the desired separations, and that sys- would significandy reduce die tems with higher selectivities are amount of HLW diat must be sent to probably required if die process is to a repository for permanent disposal, be attractive for the intended use. A and die resulting low level waste may large number of stages and corre- be stored at gready reduced cost. sponding large total interstage solvent removal rates would be required for Parallel experimental and theoret- cascades designed for the experimen- ical (modelling) studies were carried tal systems investigated to date. For out to meet the goals of the project. example, for a binary system with. CC Experimental permeabilities for ordi- = pCs/pCa 2.75, an ideal cascade nary (passive) diffusion of dissociated = containing 22 ideal stages would be salts in solution through several required to make the desired separa- immobilized liquid membrane phases tion (yP - 0.01). Since only dissoci- have been determined in a batch test ated salts are transported through the cell for Cs, K, Na, Ca, and Sr membrane, and since the driving (nitrates). The ratio of permeabilities force for diffusion is a concentration are pC*/pCa _. pCs/pSr 2.75, = difference, stagewise re-concentration pCs/pNa 44 pCs/pK . . = 1# f = 1-05 of the permeated strip and unperme- These ratios were essentially die same ated feed solutions is necessary. For for all membrane phases tested which the above cascade, about 145 liters of include n-octanol, 2-octanol, 2- solvent (water) per liter of feed solu- octanane, and cyclohexylamine. Sin- tion would have to be removed by gle permeation stages, simple cas- evaporation (or possibly reverse cades, and countercurrent cycle cas- osmosis) if the stage feed and strip cade configurations containing solutions were maintained at 2 and perect-mix stages have been modelled 0.1 Molar respectively. to determine what membrane process configuration would be required to The experimental investigation reduce the tails product Cs concen- was carried out at a level much lower tration in a hypothetical binary solu- than anticipated in the original pro-

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Idaho National Engineering Laboratory 120 University Research Consortium

Improved Phosphazene Polymers for Membrane Technology (V250)

Christopher W. Allen, University of Vermont

Co-PI and University: None

Post-doctoral: Azzam Hneihen

Graduate Student: Michael Calichman

Industrial Collaborator and Company: Debra Saez, Technically, Inc.

INEL Collaborator: Eric Peterson

Presenter: C.W.Allen

Work at INEL has led to the mance in current applications. The identification and utilization of a approaches employed involved chem- class of hybrid organic-inorganic ical synthesis and physiochemical polymers, poly(phosphazenes), as investigations of materials. In this membranes for selective removal or early stage of die project effort has separation of various harmful compo- focused in two areas (beyond recruit- nents form harsh chemical systems ment of personnel and outfitting a thus representing a promising technol- new laboratory and equipment for ogy for environmental improvement. die project). The first study involves optimization of the preparation of The project involves a systematic [NP(OPh) ] from (NPCl ] . The approach to the design and synthesis 2 n 2 n role of the metal cation (M+OPh"; of improved poly(phosphazenes) for M+ = Li, Na, Tl) as well as that of a membrane applications. A three-fold catalyst, (QjHj^N+Br, has been strategy involving preparation of explored. The NaOPh/(C H ) N+Br- polymers without die chemical 4 9 4 mixture is the superior system. Work defects which may exist in the current on [NP(OPh) ]n preparation is con- systems, chemically modified poly- 2 tinuing widi exploration of alternate mers to improve water transport and routes to (NPCl ) and polymeriza- consideration of die membrane 2 n tion of monomers containing the potential of a related class of poly- phenoxy substituent. The synthesis mers is being explored. of carbon-chain polymers of the The ultimate goal of the project, methylmediacrylate class with if successful, is two-fold. The first. cyclophosphazene substituents has goal is the improvement of properties been explored. Derivatization with and preparation routes of the system die phenoxide ion gives a polymer currendy under investigation, (poly- with side groups, radier than the diphenoxyphosphazene) [NP(OPh)2]n. back-bone, containing the NP(OPh)2 The value of this part of die study moiety. The introduction of die phe- would be development of membranes noxide results in a significant increase better able to withstand the demands in the thermal stability of the poly- of severe environmental stress. The mer. After scale up procedures are second goal is die development of developed, this material will be exam- new materials with new properties ined as a potential membrane. dius providing membranes for new applications or improved perfor-

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Index of Principal Investigators and Presenters

Allen, C. W. 120 Lidsky, L. M. 48 Apostolakis, G. 30 Lienhard, J. H. 80 Benjamin, M. M. 114 Lowe, G. A. 64 Brannon, £. L. 8 Mann, K. R. % Carleson, T. E. 64 Mayes, A. M. 22 Chun,J.-H. 104 McCandless, F. P. 118 Crawford, R. L. 10 McMurtrey, R. D. 58 Davis, L. L. 62 Miley, G. H. 46 Downar, T. 78 Moore, K. L. 106 Dubow, J. 98 Murty, K. L. 28 Empie, H. J. 60 Newbury, N. 94 Flemings, M. C. 56, 108 Pal,U. 110 Froes, F. H. 18 Petersen, J. N. 6 Golay, M. W. 32 Reinhold, T. A. 38 Griffiths, P. R. 86 Rosentreter, J. J. 70 Gunderson, R. W. 100 Sarofim, A. F. 56 Harmon, F. 52 Sato, C. 68 Hatton, T. A. 74 Taylor, P. R. 20 Hemond, H. F. 94 Tester, J. W. 56 Herman, H. 16 Todreas, N. E. 26 Hoff, W. A. 88 Toksoz, M. N. 40 Hughes, S. S. 62 Turpening, R. 90 Ishii, M. 82 Wai, C. M. 58 Kunze, J. F. 44 Watwood, M. E. 12 Lamb, J. D. 116 Yanch, J. C. 50 Larson, H. R. 110 YingJ.Y. 72 Leung, C. K. Y. 36

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Idaho National Engineering Laboratory