ML20059M479
| ML20059M479 | |
| Person / Time | |
|---|---|
| Site: | University of Missouri-Columbia |
| Issue date: | 12/31/1993 |
| From: | Rhyne J MISSOURI, UNIV. OF, COLUMBIA, MO |
| To: | |
| Shared Package | |
| ML20059E930 | List: |
| References | |
| FRN-58FR50859, RULE-PR-171 NUDOCS 9311190111 | |
| Download: ML20059M479 (204) | |
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TABLE' OF CONTENTS I. The MURR Center Preface 1-2 Foreword 3-4 Organization 5 Staff Recognition 6 II. Research Groups and Activities 7-112 Biomedical Program . 9-20 Nuclear Analysis Program 21-50 Neutron Materials Science Program 51-94. Reactor Nuclear Engineering 95-108 University Reactor Sharing '109-112-III. Educational Activities 1131132 Research Experiences for Undergraduates 115-118 Courses, Lectures and Labs and Lectures Presented 119-123 Degrees Completed 124-125 Students Supported 126-129 Tours and Visitors 130-131 IV. MURR Operations Groups 133-141 Reactor Operations 135-138 Reactor Upgrade 139-141 V. MURR Support Groups 143-154 Facilities Operations 145-146 Health Physics 147-148 Computer Development 149 Instrument Development 151-154 ~ s I i VI. Service Applications 155-164 I Service Applications Urcup 157-159 Silicon Analysis Program 160-162 Radiopharmaceuticals Group 1sotope Service 163 Nuclear Analysis Program Radioisotope Production 164 VII. Appendices 165-199 i A. Publications 167-175 B. Patents 176 l C. Papers Presented 177-185 D. Grants and Contracts Awarded or Continuing 186-191 ) E. Professional Services Activities 192-194 i j (Appointments and Committee Participation) l L F. Outside Participants
- 1. MURR Research Collaborators .
195-198 ;
- 2. Recipients of MURR Produced Isotopes and Analyses 199 J l
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PREFACE October 13,1991 marked the twenty-fifth anniversary of operation of the University of Missouri Research Reactor Center (MURR), the highest power and most versatile research reactor located on a university campus m the United States. MURR was born in 1956 aut of the farsighted vision of a Reactor Study Committee commissioned by University President Elmer Ellis and chaired by - then MU Engineering Dean, Huber O. Croft. The members of this committee-Dean Croft, Dean Elmer Kiehl, Dean Vernon Wilson, and Physics Professor Newell Gingrich-recommended constructing a research reactor with a power in excess of one megawatt. In 1960 the committee selected Ardath Emmons as the first director. Dr. Emmons also led the design team that formalized the concept of building a light water moderated research reactor ofinnovative design including a central flux trap irradiation facility. Other irradiation positions for producing isotopes and other uses were provided for in the graphite rellector surroundingthe center beryllium neutron reflector elem ent. The reactor was planned initially to be five megawatts and to accommodate a later power upgrade to 10 megawatts. Six beamtubes were provided for neutron scattering and other types of research utilizing neutron beams. The design plan also called for an extensive laboratory building of 51,000 square feet associated with the reactor to contain radiological research laboratories and offices. Several of the laboratories were equipped with pneumatic tube remote irradiation facilities. Construction ofthe research reactor and associated laboratory building began ! in 1963 with funding from both the Federal Government and the State of Missouri. It was completed and commenced operation in 1966. Powerlevels and operating schedules were gradually increased, and in 1969 the reactor began operating a 100 hour / week schedule at 5 megawatts. In 1974 the reactor power was increased to 10 megawatts, and in 1977 operation of the reactor for 155 hours per week was initiated. This schedule has been maintained since and represents an enviable on-line record of more than 90 l per cent of available time over the past 15 years. I c d _ . _ _ _ _ _ _ _ _ _ _ _ _ _ _ . _ _ _ _ _ _ _ _ _ _ . _ _ _ _ _ _ _ _ _ _ _ _ _ . _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ . . _ _ . . . - -
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t L - Over the intervening twenty-five plus years of operation 'of MURR, the-number, quality, and breadth ofreactor-based research programs have grown -- enormously. Much ofthis expansion occurred under the 14 years ofleadership . by Dr. Robert Brugger, MURR Director from' 197411988. The number and : scope of research programs which utilize the MURR Center or isotopes produced by the Reactor are unequaled by any other facility. This an nual report for fiscal year (FY) 1992 presents research and operational ; accomplishments of the reactor and its associated users and collaborators. As - discussed later in this report, the year 1992 brought forth a number of new achievements as well a new organizational structure for the research groups. A MURR newsletter entitled From Out ofthe Blue was commissioned in May, - edited by Ms. Ronita Dinger. The format of this report consists of summary descriptions of the major programs, projects, and accomplishments in FY92. Publications, patents, talks, degrees awarded, and other information follow in tabular form. The intensive efforts ofMs. Christine Errante in editing and organizing this report and of Ms. Brenda Johnson for corapiling the monthly reports and generating '* the appendices are gratefully acknowledged. Note: Much of the above historicalinformation about MURR was obtained from notes graciouslyprovided by ProfessorNewell S. Gingrich, a member of the original Reactor Study Committee. James J. Rhyne Director, MU Research Reactor Center 2
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-FOREWORD The University of Missouri Research Reactor universities, and national. and industrial:
Center (MURR)is a multi-disciplinary research - laboratories. MURR takes its role very and education center operated by the seriously as one of the premier reactor facilities University of Missouri-Columbia (MU) and is providing educational opportunities for located in Columbia, MO, USA. The Center students interested in programs related to provides MU with opportunities for research neutron sciences and engineering. and graduate education in the neutron-related sciences and engineering that are unmatched The operation of the reactor is under the at any other US university. The central focus direction of the Reactor Operations Manager of this research Center is a 10 MW light water and operations group who also handle in-pool moderated reactor that is the highest power and flux-trap sample irradiation procedures. university research reactor in the United This group has close association with the - States. The reactor has been in operation for Facilities Operations Manager and group 25 years (commencing October 13,1966), and responsible for improvements and since 1976 has had a 156 hour per week maintenance of the reactor and associated operating schedule maintained more than 90% instrumentation facilities. Within Facilities of the available time MURR has a full-time Operations are engineering - design . and _3 stafT of 112 including 21 PhD scientists, and mechanical and electronics shops. The additionally supports 40-50 students many of Instrument Development group provides whom are engaged in graduate thesis research engineering of new electronic instrumentation. using the reactor or its isotope products. The Computer software and hardware support, reactor is a separate research Center, not part including the facility-wide computer network of any MU department, and reports to the Vice and central computer, are under the direction Provost for Research, Dr. J.D. Sheridan. of the Computer Deve.opment group. Health physics surveillance and su pport for the diverse MURR has a three-fold mission of promoting irradiation and laboratory facilities at MURR basic and applied research in neutron-related is provided by a Health Physics Manager and science and engineering, providing an group. educational opportunity for students in these fields, and providing radiation and isotope The Center has a Service Applications group,- _; production services for public and private headed by the Assistant Reactor Director for ! consumers. The breadth and quality of the Technical Applications (a new title this year), research programs, available facilities and that provides radiation services and produces equipment are comparable to those found in a wide range of radioisotopes for educational the US national laboratories. institutions, state and federal agencies, and ; industrial and commercial concerns. Income The scientific programs at MURR span a broad derived from this service work provides over ~ spectrum of research disciplines and 50% of the support for the education and techniques and include archeometry, neutron research programs within the MURR Center. and gamma-ray scattering, neutron interferometry, neutron activation analysis, The organization of the research groups at l human and anima nutritim, epidemiology MURR was restructured during this past year. -l and immunology, radiation effects, What had been five groups were reorganized radioisotope studies, health physics, and into four research program arcas encompassing nuclear engineering. The reactor research 10 research groups. As shown in the groups are made up of both MURR staff and organization chart on page 5, the programs researchers at the University of Missouri are Neutron Materials Science, Biomedical, System's (UM) four campuses. Most of the Nuclear Analysis, and Reactor Nuclear programs also have strong ties to other Engineering. The group narnes reflect the 1 3
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1 scientific focus of the researchers rather than The MURR Center is in the planning and the techniques or specificinstruments used by development stages for a major three-part - n the group members. In addition to delineating upgrade ofits facilities including a laboratory more clearly the scientific foci of the groups, and experimental building addition with a 201 f the reorganization provided: added x 30 m guide hall,;a newL fuel design, an O opportunities for outstanding scientists to . increase in its power level, and a cold neutron -
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l: assume leadership roles, which for the first source. A schematic'. design plan' for the . time includes as group leaders MU faculty expanded research building was completed: who have active reactor-based research, but during this ycar. When linished, this building 1 are not directly employed by MURRJ A list of will alleviate a critical space limitation that is j individuals in the groups is given at the - constraining further major program expansion Li begi n ning ofcach group's section of this report. in M URR's ed ucational and research functions. MURR scientific staff hold titles of Group As part of a continuing interim solution to theE Leader, Research Scientist, and Senior space shortage at MURR, a third temporary . Research Scientist. Active participants in office building was installed to create 11 new MURR research programs from other MU offices and a conference room. departments - other universities have titles (new this past year) of Research Investigator The MU Research Reactor Center wpresents and Senior Research Investigator. a major resce.ch and education resource for the University, the State of Missouri, and the The operation, oversight functions, and nation. Itis the goal ofMURRis to pmvide MU enhancements to MURR facilities and faculty, researchers, an d outside collaborators programs are reviewed and approved by a access to and opportunities for_ new types of Reactor Advisory Committee consisting of research activities and facilities not'readilyn members from M U departments, MURR, other available at other institutions. It is a facility UM campuses, and outside members. This to enhanee the international reputation of the committee, advisory to the MURR director, University, and to provide the catalyst for MU c has subcom mitt ees for Reactor Safety, I sotope to be the leader in the education 'of future Use, Reactor Service, Gemstone License, generations of neutron scientists' and Procedure Review, and Reactor Research. engineers.
..s . - . _ . . _ _ , . _ . _ .-,.i _ - , _ . _ . _ _4 DIRECTOR'S OFFICE
' James J. Rhyne, Director J. Charles McKibben Associate Director
- William F. Reilly, Assistant Director Christine M. Errante, Administrative Associate 11 Ronita A. Dinger, Information Specialist Rita E. Bonney, Administrative Assistant Brenda S. Johnson, Senior Secretary Dana A. Ward, Senior Receptionist 4
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STAFF RECOGNITION A reception was held in the MURR lobby on April 24 to honor the nine MURR staff members who reached or will reach University employment milestones during the calendar year 1992. These MURR Center employees were also formally recognized at a Campus-wide Staff Recognition ceremony held April 7 in Jesse Auditorium. p FIVE YEARS G. Lawrence Jesse Service Applications Brenda Johnson Directors OfTice l Leon'a rd Manson III Service Applications Paul Miller Service Applications Leslie Powell Health Physics William Reilly Directors Office TEN YEARS Anthony Schoone Reactor Operations FIFTEEN YEARS Charles Anderson Reactor Operations Ronald Berliner Instrument Development / Neutron Materials Sciences At the reception, Director Jim Rhyne expressed appreciation to all MURR staff for their valuable contributions to the MURR Center. h 6
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ji e RADIOPHARMACEUTICALS GROUP i PERSONNEL , Alan R. Ketring, Group Leader and Senior Research Scientist (Research Assistant Professor of Radiological Sciences) . . ;
~
GaryJ. Ehihardt, Senior Research Scientist (Research Assistant Professor of Radiological Sciences) , Wynn Volkert, Senior Research Investigator (MURR) and Professor of MU Radiological Sciences - Karl Kopicka, Visiting Professor (Nuclear Research Institute, Rez, Czechoslovakia) Lyrm M. Stringham, Senior Research Specialist 3 Renee J. Hammar, Senior Research Laboratory Technician Kavita K. Katti, Senior Research Laboratory Technician , Melissa Evans-Blumer, Research Laboratory Technician . { James P. Lanigan, Research Laboratory Technician (transferred to Service Applications August i 1991) Anita R. Maves Senior Secretary i FACULTY ASSOCIATES Robert M. Brugger, Professor of MU Nuclear Engineering :! Rodney Curtis, Resident of MU Surgery '[ Delbert E. Day, Professor of UMR Ceramic Engineering ; Richard A. Holmes, Professor of MU Radiological Sciences and Chief of Nudear Medicine, Harry S Truman Veterans Administration Hospital Silvia S. Jurisson, Assistant Professor of MU Chemistry Kattesh V. Katti, Research Assistant Professor of MU Radiological Sciences ' Jimmy C. Lattimer, Associate Professor of MU Veterinary Medicine Stanley E. Manahan, Professor of MU Cheraistry Jerome W. Olaughlin, Associate Professor of MU Chemistry Gilbert Ross Jr, Professor of MU Surgery Elmer O. Schlemper, Professor and Chair of MU Chemistry For the past decade the MURR Radio- and Chemistry has tesalted in the establishment
- pharmaceuticals group (formerly Radioisotope of the Center for Radiological Research in Applications) has been working with scientists facilities near the Ellis Fischel Cancer Center from the University of Missouri, other and a Radiopharmaceutical Chemistry Minor universities and private industry to develop the for MA and PhD Chemistry students. l usc ofreactor-prod uced radioisotopes for medical ,
therapy. This research has led to developments MICROSPHERES FOR THE TREATMENT OF in the areas oflabeled micmspheres, lone tumor. CANCER AND ARTHRITIS MURR and UM seeking agents, and high specific-activity scientists have been involved in the development isdopes for therapy using labeled monoclonal of glass, activatable microspheres for the - antibodnes. Nearly one thousand experimental treatment ofliver cancer since the early 1980s.. patient treatments have now been completed These microsphems are tiny glass beads slightiy ! using radioisotopes produced at MURR by the larger than the diameter of the smallest bkod Radiopharmaceuticals (RP) group. Our vessels or ca pillaries. When injected by catheter collaboration with the departments ofRadiology into the adery which carries blood to the iiver 11 n
Y .. tumor, the microspheres are trapped in'the develop agents for treating the intense pain' b associated with ' metastatic b(me cancer. We = capillary bed, where they deliver a high localized radiation dose to the cancerous tissue. have supplied and continue to produce Re-186 for the pain palliation agent- Re-186-HEDP (hydroxyethylene-diphosphonate), = first Early work in collaboration with Theragenics Corporation produced Y-90 TheraSphere*, now developed at the University of Cincinnati and approved for general use in Canada. More currently under evaluation as a potential drug mcent research focuses on developing Sm-153- product by Mallinckrodt Medical (see Re-186 AND glass miemspheres for the presurgical twat ment Re-188 HEDP CL:NICAL TRIALS OF A NEW BONE of kidney cancer and Re-188/Re-186 labelled CANCER AGENT). Trials are also underway using protein microspheres for the treatment of MURR-supplied Re-188 as Re-188-HEDP for rheumatoid arthritis (see PRACTICAL bone cancer patients at the University' of RADIOTHERAPY FOR RENAL CELL CANCER). In the Cincinnati. latter treatment, called radiation synovectomy, radiolabelled protein microspheres The RP group was also instrumental in appropriately sized for uptake by the inflamed developing Sm-153 EDTMP (ethylenediamine-synovial membrane are injected directly into tetramethylenephosphonate) at MU, in - the joint. collaboration with scientists in Chemistry, Radiology, Veterinary Medicine and School of In all of these treatments, it is important to Medicine with support from the Dow Chemical minimize or eliminate the leakage of the Company. Both Re-186-HEDP and Sm-153 radioisotopes fmm the target tissue to other EDTMP have demonstrated effectiveness in normal tissues until the radioisotope decays. relieving bone cancer pain and greatly mducing . This can be accomplished by the use of non- or removing the need for narcotic analgesics in biodegradable glass microspheres (as in the about 80% of the patients treated m clinical case of the liver and kidney cancer treatments) triais. These agents are currently in the final or by using short lived radioisotopes such as phases of clinical testing at numerous sites in Re-188 (tn = 17 hours) that will decay before the US, which are sponsored by Mallinckrodt any significant leakage occurs (as in the case of and Dow. biodegradeble protein microspheres for the treatment of arthritis). We are also studying During the course ofthis work, remote processing . glass compositions with other isot pes and facilities were designed and built at MURR for biodegradable glass formulas for the treatment the safe handling of Curie quantities of beta-
. of cancer, arthritis and other diseases. emitting radioisotopes. This facility and our extensi ve experience with Sm-153 have enabled BONE CANCER TREATMENTS Metastatic us to develop other rare-earth radioisotopes, j hone cancer afTects approximately 200,000 such as Ho-166 and Lu-177, for potential use in patients in the US each year, primarily by new therapeutic radiopharmaceuticals.
spreading from other common cancer sites such q as lung, breast and prostate. Since the early HIGH-SPECIFIC ACTIVITY RADIOlSOTOPES FOR j 1980s MURR scientists in the RP group have RADIOlMMUNOTHERAPY The ' development collaborated with University of Missouri of monoclonal antibodies has opened new scientists and others outside the University to horizons for guiding radioisotopes to tumors 12
a l' with remarkable specificity. The need for high enhble significant advances in the labelling of - l specific-activity radioisotopes to label these monoclonal antibodies for radioimmunotherapy ' antibodies has posed new challenges. MURR ofmalignancies. j and the NeeRx Corporation have combined their efforts to find new methods for producing Re- Due to the small size of some of the chelates, .! 186 and Re-188 for this application. Initially 'these labelingLtechniques are 'also being . :i centered on 17-hour Re-188 frcr.n a W-188/Re- examined for their potential to label' receptor-I88 gel generator invented at MURR (see NEW agents and small polypeptides which localize in ~', PEROXIDE PROCESS FOR PRODUCTION OF W-168/Re- cancer and other disease tissues. These agents' - 188 AND Mo-99/Tc-99m GEL GENERATORS),this work may be usefulin the diagnosis and treatment of has evolved to the use of 3-4 Ci/mg Re-186 disease. We are also ' developing magnetic producedatMURRhynewly developedtargetry resonance imaging (MRI) contrast agents by - and methods. This Re-186 is used at four sites using this technology to prepare paramagnetic - i in the US for attachment to monoclonal chemical compounds, antibodies and subsequent administration to patients with colon, small-cell lung, and ovarian RADIOPHARMACEUTICAL CHEMISTRY MINOR ' 'l cancers. Over 100 patient treatments have Adoption of a dedicated . minor 'in 'l been performed to date, with the best results Radiopharmaceutical Chemistry by the MU
'l observed in women with ovarian cancer. High- chemistry department has allowed seven ,
speciiic-activity isotopes with appropriate half- chemistry graduate students to base their work ; lives and emissions are vital for radioimmu- at the MURR Center with the RP group. RP notherapy and the reactors which can produce scientists and other researchers at the MURR ' ) them are few; the potential in this area provides are now involved in team teaching chemistry ! one of the majorjustifications for the planned classes in the areas.of radiochemistry and power upgrade of the MURR. radiopharmaceuticalchemistry. An RPscientist-' has also served as a co-advisor and co-project i CENTER FOR RAZOLOGIC RESEARCH (CRR) director for a medical physics studentin the MU , The potential significance for radioimmu- Nuclear Engineering Department doing~. notherapy using labeled monoclonal antibodies research in impmved brachytherapy seeds. RP. - could be enhanced by improved stability of the scientists are active on. graduate student ; label and by more rapid elenrance fmm nontarget committees and University committees, such as ! tissues. These challenges have led us to study the Central Radiation Safety Committee, the ; new labeling techniques for reactor-produced Isotone Use Subcommittee,the Reactor Advisory . radioisotopes. Limited space at MURR has Committee, and the Reactor Research Advisory forced us to obtain laboratory and office space Subcommittee. for tl is program in the Allton Building near the Ellis Fischel Cancer Center. The space (five laboratories and five offices) and the project are The trend toward greater integration of the ; shared by the RP group at MURR and MU MURR Center into the education and research Radiology. Several new ligand systems are efibrts of the MU campus has been clearly currently underinvestigation (see POTENTIAL OF evident in the RP group over the past twoyears, - NEW RADIOPHARMACEUTICALS FROM NOVEL setting the precedent for future interdisciplinary PHOSPHORUS-NITROGEN LIGANDS) that may achievements at the University of Missouri. , t 13
PRACTICAL RADIOTHERAPY FOR RENAL CELL (KIDNEY) CANCER Rodney Curtis, Gilbert Ross 01U Surgery), Jimmy Lattimer (MU Veterinary Medicine), Delbert
. Day (UMR Ceramic Engineering), Gary Ehrhardt, Jim Lanigan, Eric Volkert and Melissa Evans-Blumer(MURR) l Renal cell cancer of the kidney occurs in clinical radiation effect was seen at any about 3% of new cases of adult cancer and dose, while gross pathology changes were frequently results in distant and often fatal visible only in injected kidneys, primarily metastases. Surgeons feel that surgical visible in reduced size and evidence of removal of the diseased kidney and fibrosis. Histology showed abnormalities accompanying tumor, while always only in injected kidneys, being most necessary, often results in " shedding" of prominent in the renal cortex and malignant cells into the general circulation disappearing at the renal capsule. Severity due to disturbance of the tumor bed by the of the changes was dose-related, with no surgery. Thus it would be desirable to changes observed in surrounding tissues sterilize the tumor with radiation prior to such as bowel, liver, spleen, and surgery to minimize viability of shed cells contralateral kidney. These well-limited and also possibly reduce the tumor in size effects are due largely to the short-ranged and thus aid its surgical removal. beta and minimal gamma emission of Sm-Unfortunately, external beam teletherapy to 153 (which is still sullicient to permit the kidney is limited to 2,000-3,000 rads due evaluation of the " patient" by conventional ,
to the need to avoid over-dosing other gamma camera imaging). l tissues in the abdomen, and renal cell cancer is rarely responsive to such low Evaluation of the next experimental step doses. has led to the production of holmmm-doped glass microspheres, as the short halflife Intra-arterial, beta-emitting, chemically- (26.8 hr) and energetic beta emissions of Ho-durable microspheres offer a way to deliver 166 appear ideal for the larger kidneys in substantially higher radiation doses to these human renal cell cancer patients who will tumors while sparing normal tissue. In a subsequently undergo surgery. The near cooperative project between MURR, the MU one day halflife of Ho-166 results in School of Medicine (Division of Urology), complete decay of the isotope in about a UMR Ceramic Engineering, and the MU week, permitting prompt surgery without School of Veterinary Medicine, experiments radiation risk to the surgeon. The longer have been conducted in which samarium- maximum range (about I cm) of the beta doped glass microspheres 10-20 microns in particle from Ho-166 should scale diameter have been irradiated to produce appropriately to the larger size of human .1 Sm-153 and then injected via super-selective kidneys. catheter into the kidney in a set of 18 New Zealand white rabbits. The objective was to This therapy offers the hope of both aiding evaluate safety in ascending dose trials up surgical treatment of renal cell cancer and to -35,000 rads to the target kidney, with potentially increasing the survival rate of surgical removal of the kidney and these patients by lowering the occurence of evaluation of the animal for collateral distant metastases damage to adjacent normal tissues. Animals were sacrificed and necropsied at Progress in this project was reported at the intervals of from 4 to 14 months, with 1992 High Country Nuclear Medicine striking results. No clinical illness or Conference (Society of Nuclear Medicine). 14
)
,~ _ _ _ _ . _
NEW PEROXIDE PROCESS FOR PRODUCTION OF W-188/Re 188 AND Mo-99/Tc-99m GEL GENERATORS USING (n gamma) W-188 AND Mo-99 Gary J. Ehrhardt, Qixue Liang, Alan R. Ketring (MURR), Robert G. Wolfangel, David Pipes (Mallinckrodt Medical), Carl V. Hamby (New York Medical College) Several years ago MURR scientists also minimizing handling time and hand developed a new W-188/Re-188 radioisotope dosage. A patent has been applied for on generator which could use low specific this new technology. activity,69A-day W 188. [As W-188 must be made by double neutron capture on W- One of the exciting aspects of this peroxide 186, it is only available in relatively low process is that it has also been shown to be - specific activity.] The 17 hour Re-188 applicable to Mo-99ffc-99m generators - product was successfully evaluated as a produced using (n, gamma) Mo-99. With radioimmunotherapy agent in mice by the current severely restricted choice of 1 NeoRx Corporation, studied by researchers suppliers for fission product Mo-99, great ; at Harvard Medical School and at MURR as demand for this product, and ever- { a radiation synovectomy (rheumatoid increasing costs associated with fission- i arthritis) agent, and is being considered as a product waste disposal, the stage may be component of a bone cancer agent (see Re-186 set for a resurgence of(n. gamma) Mo-99 if - AND Re-188 HEDP CLINICAL TRIALS OF A NEW it can be made equivalePt to current .j BONE CANCER AGENT). Trials of this generators. Gel generator technology j generator as a radioimmunotherapy agent provides this equivalence by permitting the .l have also been conducted at New York loading of gram quanities of Mo onto small { Medical College and by researchers in Italy. cohtmns, using the fact that the column ' packing does not have to adsorb the 'j A new process has been developed for target, but rather is made from the target. i production of the zirconium tungstate gels which minimizes tedious handling and A new method of calibrating generator should produce a more consistent columns has also been devised and tested j stoichiometry. This process involves successfully. This method involves ' forming the peroxo complexes of W and Zr, counting of high energy gamma rays from - which enables mixing of the two components Re-188 from outside the generator at neutral pH without immediate precipi- shielding before and after elution. In this tation. Formation of the gel is achieved by method an efficiency calibration for the heating to decompose the peroxide column is not required, as only a relative 4 complexes. This is continued to dryness, measurement of column activity is needed. resulting in a free-flowing material which Combined with a dose calibrator assay of can be used to directly pack a generator the product Re-188, these data permit co!umn. This process also permits accurate assay of the W-188 content of the irradiation of W metal, avoiding problems column. It has also been found that more with formation ofinsoluble " blue oxides," highly enriched W-186 targets (99.7%) etc., encountered in irradiation of tungsten register accurately in dose calibrators, duc j trioxide and sodium tungstate targets. The to their much lower W-185 content (as resulting gel behaves the same as previous observed with ~98% enriched targets). [ W-188/Re-188 gel generators. Greatly - This should also increase the already high :! l improved apparatus for this process have specific activity of Re-188 product, as much : I been designed and found to cut the less stable product Re-185 should be L processing time from days to hours, while present from the decay of W-185. i I l 15 l L _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ . . - . . . . . .. . ./
TO q Re-186 AND Re-188 HEDP CLINICAL TRIALS OF A NEW BONE CANCER AGENT ' . Edward Deutsch (formerly at University of Cincinnati Chemistry, now at f Mallinckrodt Medical, Inc.), Harry Maxon (University of Cincinnati) and Gary Ehrhardt (MURR) ; For many years the MURR Center's Radiopharmaceutical group has. . supplied Re-186 radioisotope for collaborative chemical, animal, and then . t clinical studies of the nane cance pain palliation agent Re-186 ' hydroxyethylenediphosphonate sHEDP). Re-186, which has a gamma q ~ energy similar to that of Tc-99m and is therefore highly imageable, has a . therapeutic beta maximum energy of about 1 MeV and a halflife of about 90 hours. As the active component of Re-186 HEDP, Re-186 has proven about 80% effective in Phase I and II trials. With the advent of practical .i W-188/Re-188 generators (from ORNL and MURR), interest has arisen as ; to whether Re-188 might prove a better isotope of rhenium for this agent. Re-188 has a halflife of 17 hours, a Tc-99m-like gamma emission, a beta ,7 energy over twice that of Re-186 (about 2.1 MeV maximum), and convenient availability from a long-lived generator. As rhenium HEDP is - known to localize on the bone mineral spicules situated between microscopic sites of cancer cells, there is speculation that the greater - effective cross-fire range of the betas from Re-188 may exert a stronger therapeutic effect. Clincial trials to assess toxicity and efficacy in bone cancer patients are being continued at the University of Cincinnati using ! Re-188 obtained by irradiation of Re-187 target materials at MURR. f Significant improvements in rhenium targetry and glove box processing ! procedures made at MURR have made the routine supply of hundreds of mci of Re-188 for this purpose possible without large investments in remote handling equipment. Initial results have been promising, { exhibiting pain palliation in at least one patient at a much lower dose '! than expected. ; 6 A paper describing this work entitled Rhenium-186 (Sn)HEDPfor l
'"reatment ofPainful Osseous Metastases (JNM 32(10):1877-1881) and co- t authored by Gary Ehrhardt was awarded the 1991 Journal of Nuclear Medicine Award of Merit at the 1992 Society of Nuclear Medicine Meeting. It is of note that another MURR scientist (and MU Chemistry 1 alumnus), Alan R. Ketring, co-invented Re-186 (Sn)HEDP during
- postdoctoral studies at the University of Cincinnati. MURR Service 1 l
Applications currently produces Re-186 for Phase III studies of this agent .j sponsored by Mallinckrodt Medical, Inc. ! i 1 I 16 j i !
- i. i j k -
I
POTENTIAL OF NEW RADIOPHARMACEUTICALS FROM NOVEL PHOSPHORUS-NITROGEN LIGANDS Kattesh V. Katti, Hermogenes Jimenez, Alan R. Ketring, Kavita K. Katti(MURR), Prahlad R. - Singh and Wynn A. Volkert (MU RadiologyJ The research conducted at the Center for The phosphorus hydrazides showed trimodal Radiological Research (CRR) is focused on features of coordination with rhenium as three major aspects: shown below. However, a distinct
- 1. Development of new ligand systems regiosclectivity was observed in the g derived from novel phosphorus-nitrogen reactions of these ligands with Pd(II)
L frameworks"' centers. For example, alkoxy substituente
- 2. Understanding the fundamental on phosphorus favored the bidentate coordination chemistry with the early coordination of the terminal hydrazides with -
and late trareition metals in different the metal cemer (Scheme 2), whereas 7 oxidation states phenyl substituents showed chelation of the - l [. 3 Application of this chemistry t.: matallic l- radioisotopes to develop a new genre of g radiopharmaceuticals for therapeutic T 1" and diagnostic uses in nuclear medicine." utj%
,E Jf u,4 . sa, PdCl 4 .
l MULTIFUNCTIONAL PHOSPHORUS j
.i HYDRAZlDES or -l Three new classes ofligand systems ",l_ , , ,4, 8
developed at CRR are shown in Scheme 1. g,, l l l The synthetic strategies were aimed at the W 2 HN2 NH g Y s synthesis of all these new ligands in good 7'[, H C' #' C' C' yields and also to vary substituents at the phosphoms and nitrogen centers to afTord scheme 2 extensive ehemical flexibility. The phosphorus hydrazides, heterodifunctional metal center through the P=S and one phosphine-phosphinimines and the small terminal hydrazide unit. Therefore, a systematic tuning of substituents on the 1 E's phosphorus should allow the generation of "y "' ar-= specific regioselective features in this class a,e-[h.- e , a,a As f ofcompound. R' nr -
" *"** "**'*""** As part of our ongoing research, we have seeme 1 explored the reactions of *PdCl,8-( t g =
'13.5h; D = 1030 kev) with the phosphorus molecule phoephinimines as outlined in hydrazides. The phenyl and the ethyl Scheme 1 combine the ligating phosphorus hydrazides as outlined in characteristics of hard nitrogen centers, Scheme 2 produced *Pd chelates in high phosphorus chalcogenides and soft n-acid yields (85-90'1) and these complexes have phosphines to be used as versatile been found to be stable in aqueous media at '
L? coordinating systems for both the electron pH 7 for 48h. We foresee further poor (e.g., high-oxidation-state Re and Tc) developments in the use of"Pd based ' and electron rich (e.g., Pd(ID, Pt(ID, Rh(IID ) radiopharmaceuticals in r uclear medicine if metals and their radioactive isotopes. high specific activity "Pd can be produced. 17
The controlled Schiff base coupling reactions HETERO-DIFUNCTIONAL PN-UGANDS with the phosphorus hydrazides produce new bifunctional chelating agents (BFCA)in Recent studies in our laboratory with ligands which one of the terminal hydrazides is containing one phosphinimine group (or its - functionalized with a benzoic acid unit isoclectronic analogue, phosphine oxide) as
,,o cuo well as one phosphine group demonstrate g R their versatility in forming BFCs or UFCAs with *Tc, " rep"Re, "Pd and other
'Y** ,P 00H men I NMe transition meta! TadiGnuClideS. The presence -
uj [g, of both the P=N ahd phosphine functionalities on the same molecule provide a vehicle to complex metals (both early and y P late tranSiliOn metals) with a wider variety of men NMe men j}P NMe oxidation states than ligands containing only - N ys, N ug, one of these functionalities. Le versatility of using this general ligand design bas been d O dem nstrated by the fact that several variations in the backbone structure are:
*" tolerated without significant compromise in
-coan Scheme 3 complex stability. For example, we have recently shown that substitution of a (Scheme 3). The coordination chemistry of bridging N-atom for the bridging C-atom in these BFCA's have clearly given important PCPN results in stable **Tc and "Re insight into the metal-ligand bonding complexes.
features. The metal Me u, is bound to the P=S An important characteristic of these ligands N-P N unit and one of the is that they form complexes in a 1:1 hydrazine centen ligand: metal ratio with Re and Pd despite the
'flS l NH (Figure 1) leaving fact that they are only bidentate. In
\/M the -COOH group addition, the it rminal N-atom can be O Ln free for attachment g2 derivatized with a side :
to proteins, peptides g . chain and still COOH Figure 1 or other # RP PR . participate as a donor l biomolecules. 2 2 atom to form stable ll ' metal complexes. A The BFCA was shown to readily complex N- pa cula y re vant
*Tc and this ' preformed" bifunctional example of this was chelate (BFC) was conjugated to igg (70% demonstrated by.
yield). The stability of both the *Te-BFC results with an aryl and the labeled protein was showr to be isothiocyanate-PCPN excellent. These studies provide strong (Figure 2) ligand evidence for the potential utility of NCS Figure 2 system. multifunctional phosphorus hydrazide (BHP) based ligands to form BFCAs or Studies with this BFCA show that it forms a BFCs for labeling proteins (or other very stable '**Tc-chelate in 95129, yield. The biomolecules) with **Tc or "Rer'#Re. .
*Tc-PCPN BFC was conjugated to igg lM.
Studies with various BHP derivatives will No release of *Tc was measurable after beinitiated which may provide an incubating this *Tc-protein-conjugate at or important and unique method for producing near physiological pH for 24 hr. Clearly,
*Tc or *Ref"Re complexes with desirabic these typts ofligands hold immense potential biolocalization properties. for use in preparing stable radiolabeled 18
bioconjugates. Structure-activity this unique and exciting ligand system will relationships (SARs) with appropriate be performed, however, the requirement derivatives will be essential to identify the that these ligands must be labeled in non-specific structures that will produce polar solvents may limit, to some extent radiolabeled agents with optimal properties their use with macromolecules. On the for medical applications. other hand, they may be particularly ; effective for use in the design of new """Tc or PHOSPHINIMINES *Re/"*Re receptor agents that are comparatively small compounds. Simple phosphinimine ligands with the general structure shown in Figure 3, also NEW CHEMICAL APPROACHES FOR LABELING .i' exhibit the ability to form """Tc and *Re RECEPTORS complexes. . Ph3P=N 88'"TcO 3- The radiolabeling of receptors is an area of These ligands are considerable current interest with electronically significant clinicalimplications. Even Heat very versatile as though progress with radiolabeled receptors they can act as 1, has been made, the utility of these agents in Ph3P=NH2 . 99'"TcO42, or 4 electron humans has bec- limited for a variety of ' a donors to transi- reasons. For example, the chemical tion metals reactions employed to radiolabel a receptor 88'"TcO4" resulting in M-N frequently involve the incorporation of a multiple covalent ligating unit on the receptor backbone. bonds where M is Such chemicallinking processes may th metal Wng abnonnaUy mWy Mn&g amnity,in Ph3P=NSIMe3 Ph3P=N - SiMe y eieo uptake and specificity of the receptors. we have recently Therefore, ihr widespread applicability of demonstrated radiolabeled receptors, the complexities of ReO'4 that a compound ligating a receptor and its subsequent with Re(VII) in a radiolabeling techniques must be carefully i p 1:1 metahligand addressed. ratio can be Ph3P=NH2+ ReO 4 formed. i.e., In the last six months, staff at the Center l Ph3P=N-Re0 3, as for Radiological Research have developed an Heat determined by elegant synthetic strategy to incorporate a NMR, IR and X- new genre of multifunctionalligating units Ph3 P=N-ReO 3 ray crystallogra- on model recepter backbones as shown in , phy (Scheme 4L Scheme 5. The simple, straightforward and t e, n, , s-
- f. Studies with ""Tc scheme 5 } i 4ci and *Re indicate "Q ,-
that small,
- ci ,
'G%?. -4 g
I ,.N neutral-lipophilic .... i 7 icompounds with s ! V # y' - the same I am =,
/ w chromatographic c/chon %===f'w=us f Scheme 4 n. sw a. ist p,.o.wm tm formed which infers structural similarity of i the radiolabeled compound at tracerlevels g glM[
with the Re complex obtained at p + macroscopic levels. Further studies with W ) oW m j 19
. , , .~ ,, - - . . - - - .
A y 3 P one pot synthetic discovery we have made ' receptor agents with Tc-99m, with the . 1 (Scheme 5) is in sharp contrast to the multiple ultimate objective of developing new receptor :, and often difficult reaction steps that are agents that can selectively bind several types j
- being used by other workers in the US and of cancer cells (e.g., small cell lung Ca, o 4
across the world to incorporate ligating units : carcinoid, etc) that express somtostatin - onto the receptors, receptors. :
.l t We have investigated the fundamental' References /: . j coordination chemistry of the progesterone 1. K.V. Katti, PA Singh, WA Volkert, AA j Ketring and KK Katti,"A new neutral. j
~
and estrone functionalized phosphorous . hydrazides in order to understand the ligating lipophilic *aTc complex with a bishydrazine ' 4
. properties with the transition metals (Scheme phosphine (BIlp ligand),* Int J. Appl Rad and j d j
6). The complete H,82P and '3C NMR - 2 Isotopes 43,1151-1154 (1992) .. spectroscopic analysis and single crystal X-ray 2. M Corlija, K.V. Ltti, WA Volkert, T.J.( } structures of model compounds have clearly lioffman, C Higginbotham and RA Holmes, ; j revealed that Pd(II)is bound to the receptor
- Formation of a stable **Tc-trihydrazide - j functionalized phosphorus hydrazides in such phosphine oxide (*'Tc-THP)," Int J Nuct Biol j a way that the receptor is not in itselrinvolved Med (in press) j in direct bonding interactions with the metal. 3. KV.Katti, PA Singh and C.L. Ilarnes, j
" Transition metal chemistry of main group ' :;
,,,,J s M
- 1) J 4.
hydrazides," Inorg Chem 1 (in press) - . K.V.Katti and C.L. Barnes,"The heteroatomic l
~] mve, n,.
~
e 4 [o dp. chelation of mixed phosphine for arsine) and i a,=.= "a phosphine oxide ligands with Re(V)," Inorg : , Chem 31,4231-4235(1992) j j ,y,I e 5. KV.Katti, PA Singh, K.K. Katti, K Kopicka, -
"l",, y d "'io o WA Volkert, AA Ketring,"First examples of A
h J m,,,,,,,
-~
odJ
..)_ a heteroatornic chelation of ReOf""ReOf*"TcOf and PdClf with a phosphine phosphineoxide (or a phosphinimine) bridged bifunctional .
system,"J Lobl Compd Radiopharm lawepted) ' sewne 6 6. WA Volkcrt, pA Singh, K.K Katti, AA ,j Ketring and KV.Katti, *A new and versitile , Recent studies in our laboratories have mu!tifunctional phospherus hydrazide ligand for , demonstrated that the sequence of reactions fonnulating neutral. lipophilic complexes of outlined in Scheme 2 can be extended to ""'Tc, "Re and '*Pd radionuclides," J Labl j
~
produce the '*Pd (t 1/2 = 13.5h; EB= 1030 - Compd Radiopharm (accepted) - i kev) analogues of the receptor functionalized 7. KV.Katti, PA Singh, C.I Barnes, K Kopicka, ;! phosphorus hydrazides. The 2*Pd complexes AA Ketring and WA Volkert, *The potential of ! of 2 and 3 are formed in high yields (>909) phosphinimines as building blocks for a new j and are stable in aqueous media (pH 7) for generation of radiopharmaceuticals,* ' . .j 24h. The '*Pd complexes of 2 and 3 are Phosphorus, Sulfur and Related Elements (in ^ 1 assumed to have structures similar to 4 and 5. press) . j
- 8. KV.Katti, PA Singh, AA Ketring and WA 'i The aforementioned studies have clearly Volkert,*Functionalized ph(,pborus hydrazides
; established the eflicacy of functionalizing- as novel chelating ligands to transition metals," [i model receptors on multifunctional Phosphorus, Sulfur and Related Elements (in N phosphorus hydrazides and have also proven press). .. . !
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l NUCLEAR ANALYSIS PROGRAM J. Steven Morris, Coordinator ' Charles A. Fairfax, Senior Research Specialist Ginger L. Koziatek, Research/ Laboratory Technician -r Lynn R. Smith, Senior Secretary Groups in the Nuclear Analysis Program Nuclear Archacometry and Geochemistry
)
Analytic Epidemiology, Nutrition and Immunology Actinide Chemistry i During its 25 years of operation, the MURR universities access to neutron applications in Center has evolved with I. gh quality, diverse, their research programs. nuclear anal sis programs which reflect the stmngths of the MU campus and support the The NAP research programs heavily emphasize j operation, revenue generation and academic the unique capabilities of the MURR Center. mission of the MURR Center. This has been For example, the NAP biochemistry program , accomplished by a MURR-based scientific stafT maintains several isotope production networks ! in collaboration with MU faculty and a very featuring radionuclides that are not routinely extensive set ofscientists from otheruniversities, available elsewhere i.e.,Se-75(~1000Ci/g),Cu-government agencies and industry. All three 64 (-250,000 Cilg) and Ca-47. These networks , components are critical to the success of the provide isotopes forNAP research, a mechanism ' Nuckar Analysis Program (NAP). forcollaboration with otherhigh-qualityreseamh - programs, a service to the MU campus, and MURR's Nuclear Analysis Program is a funding opporttmities. In today's competitive comprehensive one which includes integrated rescamh environment thereis an everincreasing components of research, teaching and service. need to develop interdisciplinary approaches to
- The central focus is the utilization of neutron attract and sustain adequate funding. l activation combined with gamma-ray spectro- Recognition of this need is evident in the NAP scopy to provide users the full range ofneutron research programs. Each individual research ;
activation analysis (NAA) techniques (i.e., area defined here has evolved beyond just the prompt gamma-ray NAA, epithermal .NAA, exclusive use of nuclear methodologies. ' For l instrumental NAA and radiochemical NAA) as example, the Actinide Chemistry group has well as fate of tracer studies utilizing tissue developed an excellentinert atmosphere facility culture and animal models. MURIrs NAP has and routinely utilizes sophisticated high j a well qualified staff, limited-but highquality temperature, non-aqueous electrochemistry laboratories-and state-of-the art instrumenta- methodologies to study thermodynamic tion. These Pmgram components am summarized properties of the actinides. The archaeology in Table L research uses microscopytechniques and applies cutting-edge principal components analyses to The range of NAP research efforts reflects the statistically test its extensive element strengths of the MU Campus including its composition database which containsboth source Eminence Programs such as Food for the 21st materials and artifacts. The epidcmiology area : Century (FF21C) and Molecular Biology. In develops and applies nuclear and atomic addition, in this and previous fiscal years, NAP spectroscopy techniques to study chronic trace- - research projects have been the largest element and mineraliimbalance. The- ' component of the DOE funded reactor sharing biochemistry, nutrition and immunology-program. Reactor sharing allows other US collaborations utilize state-of-the-art tissue I 23 J
j ' 1' I a culture. and small: animal laboratories and The biochemistry and nutrition amas utilizeH d instrumentation at MURR to advance the use of . unique isotope pmduction capabilities at the -
- nuclear methodologies in these disciplines. MURR Center, with' nuclear and atomie: i spectmscopy,in combination with biochemistry i The primary teaching responsibility.of the methodologies. . These techniques examine .
NAP is training students in 20 or more macro- and trace-element' requirements, z n academic departments using the Program's interactionsandbindingbyproteinsusingboth - 5 substantial resources. In addition, NAP staff tissue culture and whole animal models._ Thisi l members routinely assist in teaching a wide research emphasizes the combination of the. 1 variety of courses. utilization of high specific activity radiotracers ~ , (someofwhichareuniquelypmducedatMURR), . 1 Service is the third leg ofthe mission triad. Here cell culture and small animal models, with ; the Nuclear Analysis Pmgram is also very active innovative application of gamma #ay spectro-in supporting reactor operations, in pmviding scopy to quantify and image radiotracers of the ; the quality assurance programs required by trace elements under considerationi. j exempt licenses, and in making NAA services :i available to other universities, government The nutrition program supports MU's Graduate . d agencies and industry. Nutrition Area Program and the FF210 - , Nutrition Emphasis Area. Faculty, studentsL .I Funding for the Nuclear Analysis Pmgram is and staff fmm MU departments of Agronomy, I derived from grants (55%), MURR grant Animal . Science, Biochemistry, Child Health, incentive fund (127), service contracts (119) 'd: Food Science and Human Nutrition' utilize and MURR general operating support (22%), MUlUt's neutron activation analysis, isotope - - totaling $1,014,321 in FY 92. production, gamma-ray spectroscopy and small > animal facilities to. study a wide range of. Ii NAP RESEARCH In the Life Sciences, the nutritional interests such 'as trace-element - '! NAP has programs in analytic epidemiology, interactions, calcium metabolism and endophyte 1 biochemistry, immunology and nutrition. These mfestation ofMissouri fescues. programs actively collaborate with MU departments such as Agmnomy, Animal Science, The radio-immunology research studies the
. j a Biochemistry, Biology, Chemistry, Child Health, production of monoclonal antibodies, their-Food Science 'and- Human Nutrition, labelling with radionuclides while mtaining Immunology, Microbiology, Obstetrics & immunological activity, and their use as
- Gynecology and Veterinary Medicine, as well as radinimmunodiagnostic and radioimmuno ' y many outside research universities and agencies therapy agents in the diagnosis and treatment j such as Harvard, Johns Hopkins, Washington of human diseases < The curmnt focus is the - 3 University, USDA and NIH-NCI. development of a human r.mnoclonal antibody capable of the sensitive diagnosis of ovarian j Nutritional epidemiology research uses NAA cancerin ritm through the reaction with ovaria n . 1 and flame and furnace atomic absorption in cancer antigens pmsent on the cell membrane. !
collaboration with the major US centers for There is. closeL collaboration with the'MU ' i epidemiological research to. study the relationships between chronic deficiency of Departments of immunology, Microbiology, Obstetrics and Gyrecology, Biochemistry and - j trace-element nutrients and elevated intak'es
~
Food Science and Human Nutrition. 1 of toxic trace elements and human disease outcomes such as cancer, cardiavascular In the An thropological and Geological Sciences, - i disease and adult onset diabetes. The MURR the NAP has programs in nuclear archaeology H component focuses on the linkage between and geochemistry, which,in addition to the MU H
' dietary intake ofminerals and tracc elements "
departments of Anthropology . Art andi and the resulting concentration of these Archaeology and Geology, also interact with* nutrients in tissue monitors. major US universities and agencies with 24 i
, . < ' .- . . , . - ,- . - -, ~- , , , .
I' emphases in amhaeometry thmugh an NSF NAP SERVICE In addition to its research funded center for nuclear archaeology. The activities, the NAP provides services to other Archaeometry Laboratory at MURR combines MURR groups, MU faculty, studat. a and staff, t NAA and microscopy techniques in and to outside universities,;apncies and ' archaeological rcsearch . requiring industries-especially Missouri industry. NAP determination of the sourtes of raw materials - service programs can be characterized by three utilized by prehistoric peoples. Collaborations distinct groups / techniques / facilities; the Co-60 include projects with Harvard, Tulane, Irradiation Facility, neutron activation aualysis Dartmouth, Arizona, Arizona State and the (NAA) services, and the Quality Assurance -! Smithsonian Institution. Program. : The objective of the nuclear archaeology The Co-60 Irradiation Facility pmvides gamma-program is to determine the geographical ray irradiation services in support of academic > origins and ages of artifacts from various and industrial research in the following ways: cultures. Heavy emphasis is placed on the a impairing the immune system to provide sourcing capability of multi-element neutron a baseline forimmunology research , activation analysis. The extensive " Missouri a TLD dating of archaeological artifacts Collection" of Mesoamerican obsidian is one a biochemical inactivation of biological 4 example of the comprehensive collections of tissues and receptors - j' source matetials that are under investigation = sterilizing a wide variety of biological at MURR. samplen >
- development of vaccines The objective of the geochemistry program is to
- eradicatingendophytefrominfected fescue..
develop petrogenetic models to study the seed chemistryand thennodynamics associated with
- inducing chromosomal damage in maize -
the formation of the earth's oldest geological
- inducing ESR in calcite; to study >
formations. Neutron activation analysis is irradiation sterilized foods . utilized as a means of studying rare earth a generating fruit fly mutations; to generate .l' anomalies. free radicals in Sm-153
- testing and calibrating avalanche detectors r Actinide chemistry research was initiated at = creating defects in semiconductor .
MURR in January 1990, in addition to MU materials ^! departments of Chemical Engineering,
- testing MOSS devices in a high gamma Nuclear Engineering and Chemistry, the radiation field Actinide Chemistry group also collaborates
- inducing polymerization of acrylics. ;
with Rockwell International, DOE, the 'r Central Research Institute of the Electric NAA services to industry are primarily in ! Power Industry (CRIEPI) of Japan and response to the domestic need for analysis of l Kawasaki Heavy Industries (KHI) ofJapan. high-puri y materials. Materials routinely ; The Actinide Chemistry group uses analyzed include silicon (starting, refined and electrochemical measurements to determine finished materials), graphite, quartz and Imron. the thermochemical and thermodynamic properties of the actinide metals (specifically The NAP Quality Assurance Program provides
- U.Np, Pu and Am) and the metal chlorides in the quality assurance expertise necessary to i fused eutectic salt mixtures and cad nium obtain and sustain licensed activities such as that exist in nuclear fuel wastes and spent the MURR exempt materials license which is !
nuclear fuels. A specific aim is to determine critical to the MURR's revenue generation. [ the theoretical and practical feasibility of The QA program includes gamma-ray , using an electrochemical process that would spectroscopy and othernuclearanalysis support i be carried out in molten salt solutions to for the exempt release of byproduct materials .; ' separate the actinide elements from the to the unlicensed general public, such as complex radiological and chemical mixtures neutron color-enhanced gemstones and neutron : in which they exist. transmutation doped silicon. 25 ,
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.! Table 1 - The Nuclear Analysis Program at the MURR Center I
1 DESCRIPTION
- 1. COMPONENT 4
I
! Staff 14 fullsime staff members including 5 research scientists,4 . ! research specialists,4 research laboratory technicians and a i
secretary ;
?
approximately 50 faculty, students and outside scientists
! collaborators
! 1
')
f Laboratories 2 counting labs,4 radiation labs with pneumatic-tube irradiation facilities,3 sample preparation / project labs, an actinide chemistry j l lab, a small-animal research area, a tissue culture lab and a Co-60
! irradiation facility "l Major Equipment Canberra / Nuclear Data-bssed gamma-ray spectroscopy system -
- operating through acquisition-interface modules (AIM) attached - ; 1 i
; via Ethernet to a multi-node Microvax computer network including l :
l six low-background spectrometers, four shielded spectrometers l with sample changers, two shielded spectrometers in pneumatic-l tube labs, one x,y-energy spectrometer and one PGNAA , spectrometer l , ; I
-t l Other major equipment:
- atomic spectroscopy equipment
; including flame, furnace and ICP systems e sample preparation equipment including analytical balances, a micro-balance, static :
f i and centrifugal freeze-driers, microwave wet-acid digestion system, i i muffle furnaces and binocular and petrographic microscopes * .; biochemistry equipment including a UV-visible spectrophotometer, o l electrophoresis systems, column chromatography equipment with fraction collectors and a refrigerated centrifuge a tissue culture j equipment including a biological safety cabinet, incubators,
-]
microsmpes (inverted and fluorescence), autoclave and an ELISA .I reader
- small animal surgery equipment, housing and metabolic -l units
- actinide chemistry glove box with an argon inert -
atmosphere and equipped with Ni-train and Dri-train argon l purification systems, computer controlled electrochemistry j instrumentation and a high-temperature thermowell
}
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NUCLEAR ARCHAEOLOGY AND GEOCHEMISTRY GR.OUP a PERSONNEL Michael Glascock, Group Leader (Adjunct Assistant Professor of Nuclear Engineering) Hector Neff, Research Scientist (Adjunct Assistant Professor of Anthropology) Robert Benfer, Senior Research Investigator (MURR) and Professor of Anthropology-Michael O'Brien, Senior Research Investigator (MURR), Professor of Anthropology and Associate Dean of Arts & Sciences Kathleen Slane, Senior Research Investigator GIURR) and Professor and Chair of Art History & Archaeology Marcus Rautman, Senior Research Investigator (MURR) and Associate Professor of Art History
& Archaeology Peter Nabelek, Research Investigator (MURR) and Associate Professor of Geological Sciences -
JefTrey Denison, Senior Research Laboratory Technician Sindy Hays, Research Laboratory Technician The Nuclear Archaeology and Geochemistry Group, or"the Archaeometry Group" t as we are frequently called, uses neutron activation analysis (NAA) to characterize thirty or more trace elements in artifacts and geological specimens. These data are used by archaeologists to determine the origins of artifacts and by geochemists to investigate the natural processes that created different types ofigneous, sedimentary, and metamorphic rocks. The Archaeometry Group has an extensive network of student and faculty collaborators from MU and other universities. Major accomplishments during the past year include:
- obtaining a three-year renewal of a obtaining a unique collection of our NSF Archaeometry grant, obsidian artifacts from the Valley enabling continued support for of Oaxaca in southern Mexico ,
five or six students
- sponsoring a visiting doctoral
- analyzing over 3,000 new candidate student from the samples from 25 research University of Michigan who used projects, further enhancing the NAA to study ceramic materials _ ;
utility of our archaeological from Peru databank
- beginning a long-term study of- :
- developing an abbreviated-NAA pottery and ceramic raw procedure that reduces the cost materials from Mississippian and effort of sourcing obsidian occupations in SE Missouri.
artifacts from Mesoamerica In addition, Dr. Neff published an !
- beginning the incorporation of the edited volume entitled' Chemical hydration dating technique to Characterization ofCeramic Pastes in supplement our NAA sourcing Archaeology that reports data from method on obsidian MURR and other universities.
27
MESOAMERICAN STUDIES Hector Neff, Michael D. Glascock, J. Michael Elam (MURR), Frederick J. Bove (University of California-Santa Barbara), Mary Thieme (Vanderbilt) and Ernesto Gonzalez-Licon (Instituto ; Nacional de Antropologia e Historia-Mexico) One long-term research focus ofMURR's Current Archaeometry Group research - Archaeometry Group under the direction of activities in Mesoamerica center on the ; Michael D. Glascock is the archaeology of Valley of Oaxaca, Mexico and Pacific coastal the region known as Mesoamerica, a Guatemala. NAA combined with obsidian designation which refers to northern hydration rim dating are providing fresh , Central America and the southern half of perspectives on the prehistory of both Mexico (Figure 1). The Archaeometry regions. Group's first large-scale project, initiated in the early 1930s, was an effort to In the Valley of Oaxaca, J. Michael Elam, characterize by neutron activation analysis PhD candidate in Anthropology at MU, is - (NAA) all of the major Mesoamerican exploring how acquisition of obsidian (which obsidian sources. The resulting source was unavailable locally) changed at several ; database permits identification of the sites during the period 500 BC - 1520 AD. geographic origin of obsidian cutting tools Interestingly, Elam has found that the found on archaeological sites throughout histories of source utilization differ between Mesoamerica. sites in different parts of the Valley. The I 5 m, ,, S *
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i 500 or so obsidian dates to be generated by Guatemalan and US collaborators since the project will also provide evidence 1987 to amass both the required source pertaining to a controversial hypothesis that sample database and a database of the entire region was nearly abandoned analyzed pottery. Here, as in the Oaxaca between about 700 and 1100 AD. study, there are two general research goalsm The first is to learn how humans exploited Another project, now in the planning stages, certain natural resources such as ceramic - will combine NAA of modern and prehistoric. raw materials. The second is to determine pottery from the Valley of Oaxaca in an how humans interacted with each other investigation of ceramic resource use and over the past 3,500 years or so.- pottery consumption from 500 BC to the present. The modern pottery comes from Of course, the goals just mentioned require four villages whose ceramic traditions can be precise control over the chronology, and traced to their pre-Columbian roots. . this is where obsidian comes in. Next to - Prehistoric pottery will come from the great pottery, obsidian is the most abundant Zapotec capital ofMonte Alban, whose artifact category in Pacific coastal - _; inhabitants consumed vast quantities of Guatemala. Thus, using obsidian - j pottery from all over the Valley of Oaxaca hydration rim dating,it is possible to over a period of about 2,000 years. The obtain many calendrical dates from prehistoric pottery will be sourced to archaeological excavations in this region. different Valley subregions by comparison Taking the number of dates per unit of time with the analyzed modern pottery. A major as a rough index ofintensity of occupation, goal of the project is to trace the waxing and extremely detailed information on the , waning of Monte Alban's ties with various population history of particular sites can be parts ofits hinterland. generated. For example, the stair-step pattern of dates at the important coastal In Pacific coastal Gue.temala, whem there site of Balberta (Figure 2) suggests several are no modern potters, sourcing prehistoric periods ofintense occupation, the last one pottery requires systematic survey and around 300 AD. The importance of the sampling of clay and temper sources. obsidian dating evidence is highlighted by Temper is any non-plastic material mixed the fact that the few existing radiocarbon , into the clay. Hector Neff, a research and archaeomagnetic dates from Balberta scientist at MURR, has been working with only document the period from 0 - 500 AD. 2000 1500 1000 500 .... g g O . ....,,.. ;
-500 g...""
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l 29 l
EXAMINING GEOGRAPHIC VARIATIONS IN OBSIDIAN SOURCE COMPOSITION AT SAN ' MARTIN JILOTEPEQUE, GUATEMALA Michael D. Glascock, Hector NefT G1URR) and GeotTrey E. Braswell (Tulane) Although the vast majority of obsidian from the large volcanic source near the city ; sources are highly homogeneous in chemical of San Martin Jilotepeque h>cated in the i composition, a few sources are known that highlands of Guatemala. Braswell collected ~ ! exhibit compositional variation according to 75 3ource specimens from geographically ! location around the source. Provided recorded locations that were distributed enough information concerning the around the city of San Martin Jilotepeque. geographic variation in composition is A map showing many of the collection sites obtained, archaeologists have hypothesized is shown in Figure 1. The source specimens , that it might be possible to trace artifacts to were analyzed by MURR to determine a 28- j the specific subregions of the sources from element chemical fingerprint. To facilitate . ' which they were quarried. This knowledge examination cf the data, principal { might assist archaeologists in obtaining components analysis was applied to the information concerning chronological matrix of trace-element concentrations. A ' i changes in obsidian acquisition for specific scatt.erplot of the first and second principal l sources. components is shown in Figure 2. The - source data are shown as individual samples - .y This collaboration between MURR's and are compared to a 95 percent confidence Archnecmetry Laboratory and Tulane ellipse generated from artifacts previously g University has sought to examine obsidian sourced to San Martin.. The interpretation of this scatterplot is that only certain areas .; N i around the source at San Martin were being ,
* ~
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CHEMICAL CHARACTERIZATION OF MISSISSIPPIAN PO1TERY AND CLAYS FROM THE SOUTHEAST MISSOURI LOWLANDS AND ADJACENT OZARK UPLANDS Hector Neff, Michael D. Glascock, James W. Cogswell (MURIO, James E. Price, Michael J. O'Brien (MU Division of American Archaeology) and Mark J. Lynott (National Park Service) . An ongoing project funded by the National Several tantalizing results have emerged . , Park Service is assessing the feasibility of from the pilot study. First, both clays and using chemical characterization of pottery raw materials manifest two distinct and raw clays to study prehistoric ceramic compositional profiles, one associated with - production and exchange in southeast the Ozark uplands and one associated with - Missouri. The first 100 specimens analyzed the Mississippi Valley lowlands. Therefore, by neutron activation analysis at MURR ceramic resources do manifest suflicient' came from locations indicated on the geographic patterning to permit sourcing of accompanying map (Figure 1), prehistoric pottery, at least on the broad ~
~
_ __ level of uplands vs. lowlands. Related to the upland vs1 : I lowland dichotomy, pottery } L from the lowland sites of l' Powers Fort and Turner / i g Snodgrass pertained - exclusively to the lowlands, i
. while pottery from the q~
upland site of Gooseneck d pertained to_both uplands
~
g and lowlands. This evidence suggests a difference in 1L, , geographic scope of economic y~
. activities between the f- 2 l upland and lowland
- g ' 1 { inhabitants.
- On a finer scale of
,,',,, geographical resolution, I ,,
muou,, P4 y compositional distinctions are also recognizable with,n i thelowlands. Forinstance, i Turner /Snodgrass pottery i y analyzed in the pilot study was found to be composition-aUcE[g1sn. ally distinct from the pottery
. of Powers Fort, which is ;
'5"*'
. locat4d only 6 km fmm l Turner /Snodgrass._ Thus,' !
lowland ceramic production ' Ag.1 The study region in southeast Missouri showing and consumption was even archaeological sites and clay sampling locations. The Ozark more restricted in geographic
, escarpment indicates the separation between the Ozark i I ' uplands and the Mississippi Valley lowlands. Scope than suggested by the [
l upland vs. lowland contrast L__ _ . _ _ - __ a mentioned above. i l 31 ;j
-t
l SOURCING OBSIDIAN ARTIFACTS BY AN ACBREVIATED-NAA PROCEDURE Michael D. Glascock and Hector Neff(MURR),in collabora* ion with more two dozen archaeologists working in Mesoamerica Obsidian is a naturally occurring volcanic archaeological sites. Unfortunately, the glass similar in composition to granite but cost of generating a full 28-element lacking in crystalline structure. When fingerprint is far higher than most struck by a skilled craftsman, the glass archaeologists are able to afford. In yields conchoidal-shaped fractures and response, the Archaeometry Laboratory produces some of the sharpest edges of all recently developed an abbreviated NAA lithic materials. As a result, obsidian was a procedure, one relying on the highly-prized natural resource for measurement of short-lived elements, prehistoric peoples who used it to that succeeds in sourcing about 90 manufacture sharp-edged tools, weapons percent of the artifacts from this region. and ornaments. A scatterplot of Mn vs. Na is shown in Figure I where more than 500 artifacts Although the glass occurs naturally in only from Guatemala, Belize, El Salvador a few regions, there is much evidence for the and Honduras are compared to the 95 existence of exchange networks during percent probability ellipses for the three prehistoric times. In particular, the pre- main obsidian sources in Guatemala. Columbian inhabitants of Mesoamerica The ten percent of artifacts not sourced mined and traded obsidian from source by the abbreviated NAA procedure can areas to numerous sites that archaeologists still be submitted to the full 28-element have discovered more recently. analytical procedure such that we retain the ability to source nearly 100 - Since the early 1980s, the Archaeometry percent of the artifacts from Laboratory at MURR has been involved in Mesoamerica. Thus, we have developed an effort to characterize by NAA all known a method that increases sample Mesoamerican obsidian sources. The NAA throughput, provides the same rate of database consists of a 28-element success in determining source, and compositional fingerprint for every source greatly reduces the cost of NAA for specimen analyzed. Currently the source archaeologists. database includes fingerprints for p , , more than 800 . source specimens E ' El Chayal
~
from approxi' . _ txtepequa _ mately 40 sources 4 , located throughout o m
. San Martin Jilotepoque
+
Mesoamerica. c- ', f -
; w . .. .- -
Z
- Applying the same procedures to artifacts as to 0 -
+
+
([i
+
source specimens + l permits near 100 .".
~
_ . , .' l percent success in det.crmining the geographic origins g* * * * * * * *
- M"IPP"I ofobsidian Fig 1 Scatterplot of Mn versus Na for obsidian artifacts from archaeological Sites in artifacts found at Guatemala, Belize. El Salvador, and Honduras.
32
F t ANALYTIC EPIDEMIOLOGY, . NUTRITION AND IMMUNOLOGY GROUP PERSONNEL J. Steven Morris, Group Leader and Adjunct Professor of Chemistry Kurt Zinn, Research Scientist ' Tandra Chaudhuri, Research Scientist ; Harold Anderson, Senior Research Investigator (MURR) and Professor of Science, - } Stephens College - ' Dennis T. Gordon, Senior Research Investigator (MURR) and Professor of MU - Food Science and Nutrition Laura S. Hillman, Senior Research Investigator (MURR) and Professor of MU a Child Health - Ronald F. Sprouse, Senior Research Investigator (MURR) and Professor of MU - , Pathology Roger A. Sunde, Senior Research Investigator (MURIt) and Professor of MU Food Science and Nutrition Connie Baskett, Senior Research Specialist Vickie Spate, Senior Research Specialist ! Dan Trokey, Senior Research Specialist , Charles Fairfax, Senior Research Specialist _l Maddie Mason, Research Specialist : Ginger Koziatek, Senior Laboratory Technician Cheryl Reams, Research Laooratory Technician > FACULTY ASSOCIATES Gretchen M. Hill, Associate Professor of MU Food Science and Nutrition i S.R. Koirtyohann, Professor of MU Chemistry Alfred S. Llorens, Professor Emeritus of MU Gynecology Oncology ; Gregory A. Mcdonald., Assistant Professor of MU Microbiology Boyd O' Dell, Professor Emeritus of MU Biochemistry The Analtyic Epidemiology, Nutrition and Immunology group is a part of the Nuclear-Analysis Program and is involved in research, teaching and service. The research _; function of the group has been described elsewhere in this report (see NUCLEAR ANALYSIS l PROGRAM also) and Is summarized in Table L
. i The Analytical gmup is also responsible for operation and utilization of the MURR1 Cobalt-60 Irradiation Facility and supports the regulatory requirements of the exempt license under which irradiated gemstones are released.
I 33 j
r l i i r ,- ! I Table 1 Research Summary of the Analytic Epidemiology, Nutrition and immunology Group METHODS MODELS EXAMPLES i Radioisotope Production Small Animal Selenium-an essential ; trace element - *
^
Gamma-Ray Spectroscopy Cell Culture i Neutron Activation Analysis lluman Radioimmunodiagnosis of
-l hospital-based ovarian cancer Atomic Spectroscopy Human Fluoride and osteoporosis ; population-based l '
Biochemical Analyses .r t 6 k
.. I I
i i _. j i 34
'i
~
NUTRITIONAL STUDIES INVOLVING TRACE ELEMENTS Kurt Zinn, Tandra Chaudhuri, Daniel Trokey (MURR) and Dennis Gordon (MU Food Science and Nutrition) - - For the past two years MU and MURR Cu utilization, although it was not clear researchers have used MURR's unique in vivo whether the interaction might change with rat whole body counter and scanner. This gamma- age, or with time that rats were fed Fe-ray spectroscopy instrument includes a . supplemented diets. germanium detector and is therefore capable of , high resolution and simultaneous measurement To investigate this interaction further,24 of several gamma-ray emitting radionuclides. male weanling (21 d) Sprague-Dawley rates MURR scientists and MU collaborators have were divided into three gmups and fed test relied on this instrument to investigate diets identical in Cu and Zn levels but with , nutritional questions, particularly those related different Fe concentrations. The test diets to trace element metabolism. were the same basal diet recommended by the American Institute of Nutrition supplemented . Typically the rat model has been used, with with either 25 pg,125 pg or 250 pg of Fe. The , varying test diets to determine their effect on the radionuclides CCu,"Zn and 5'Fe were retention of the radionuclides.' Several administemd by gavage at three dosing - radionuclides are administemd to the animal, intervals (6 hours,10 days,20 days) after the and the gamma rays are detected with the rats were started on their respective test diets. ' instrument. Each gamma ray is associated with TheCCu and "Zn were available at MURR ~ a specific radionuclide and has a measumd count - since a regular production schedule is rate. The count rates are normalized to the rate maintained for research programs. Following following dosing and are reported as percent desing, the in vivo retentions of the ; - retention. Because all measurements are radionuclides were measured at six time performed simultaneously, the scanner has intervals. , mduced the numbers of animals needed to . conduct meaningful studies. There was a significant effect of high dietary Fe on percentage of CCu retention (p<0.05) The following two collaborative research projects over time for all three dosings (Figure 1). In , were conducted in FY92 using these techniques. ' contrast, the "Zn was not significantly : afTected by dietary Fe level (Figure 2). As ; Fe-Cu-Zn Interaction Previous collaborations expected, high dietary Fe decreased the between Professor Gordon and MURR pementage of"Fe retention (Figure 3). . researchers investigated dietary copper (Cu), l iron (Fe) and zine (Zn) interactions. That work Consistent with previous studies, our suggested a negative interaction of excess Fe on - investigations this year reproduced a negative l 5 * ; inn po ) i i 50 - u- 30 - I .. i g ,. E o n.nw 7 MN ._.4 I ~ ^
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8 58 W no MD N O 50 100 150 200 250 0 50 i00' 150 200 250 I Time FoBowbg Dose 00 Time Following Dose (h) Time Following Dose (h) s
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Fig.1 Percent retention of Feg. 2 Percent retention Fig. 3 Percent retention of j
Cu over time. of $52n over time. "Fe over time. l f
r 35 ;
r [p 7g d L interaction of Fe on CCu retention in the rat! The Rats were fed their respective test diets interaction did not change with rat age, and was ad libitum for 11 days and were dosed ' not minimized as rats wem fed the diets for longer with radionuclides by stomach gavage. periods of time. The results indicate that "Zn The mixture contained "Ca, "Mn, "Fe, retention is not adversely affected by high Fe level, "Zn and Se. The retentions of all but that high Fe significantly decreases 5"Fe radionuclides was measured over the . retention. Future work will focus on the next 10 days. All radionuclides could be mechanism of the interaction, particularly at the - measurext simultaneously because of the level of the intestine. high-energy resolution of the detector system. Figure 4 demonstrates the Dietary Fiber and Trace Element Metabolism gamma-ray spectra plotted with log of Dietary fiber (DF) is a topic of keen interest in counts versus gamma-ray energy. The nutrition. While NIII guidelines suggest that right inset clearly shows the resolution . Americans should increase their daily consumption of two gamma-ray peaks that differ in - ofdietary fiber, there have been reports that DF energy by only 5 kev (5*Fe and Ca). has a negative effect on mineral absorption. MU/ The gamma rays for determining . MURR collaborative research has set out to miention are shown in Table 1. measum the effect of fiber on mineral bioavailability by studying the effect of DF on the mientions of trace element radionuclidesc Seven Table 1 Gamma Rays For groups of male weanling rats, six per gmup, were Determining Dietary Fiber fed dieta containing calcium (Ca), phosphorus (P), Retention magnesium (Mg), iron, zinc, manganese (Mn) and copper at threshold levels adequate to sustain "Cu 1297 kev gmwth. An additional contml gmup was fed a diet "Zn 1115 kev with no DF but with mineral concentrations "Fe 1099 ~ kev recommended by the American Institute of "Mn 835 kev Nutrition as a control diet. Diets with threshold "Se 264 kev mineral concentrations were prepared to contain 0, 5,10 and 15% total dietary fiber (TDF) from soy hull cellulose and 5 or 10% 'IT)F from wheat bran. Percent retention of the radionuclides aller 10 days for rats fed the diets with threshold mineral concentrations s supplemented with either cellulose or r,-upM r ,-s, c._,, WR'- r wheat bran averaged: "Ca,78%;"Mn, l lp , 5G;"Fe,70%;"Zn,60% and 75Sg 40%s 3 I l These values were not significantly different from retention values in rats -
"1 fed a DF-free diet. The results of this 3, investigation strongly indicate that gi ,,f l q ,
neither celluk>se nor wheat brim -
,u q il ; impaired mineral absorption or j hk t
L ,_] i! ! .h. i wtention. Furthermore, the utility of o is age N l 'l multi L es
% l s~ple ~~ radionuclides a-~ for evaluating i FS 4 Gamma-ray spectra from a rat that was dos,ed with the five radionuchdes, on so 245 400 su tio een 102 tire issi Each peak is associated with the Energy (kev) decay of one of the radionuckdes.
36
RADIOIMMUNODETECTION AND THERAPY OF OVARIAN CANCER ; Tandra Chaudhuri, Kurt Zinn, Steven Morris (MURR), Gregory McDouald (MU Microbiology), i Alfred Llomns (MU Obstetrics and Gynecology) and T.K. Chaudhuri (University of Texas, Nuclear Medicine) Ovarian cancer, also known as silent developed at 150 kDa. The radiolabeled l killer,is one of the leading causes of death antibody was incubated with rabbit blood at nmong American women. Owing to the 370 for 2 hours to test the stability. Only { lack of quality control, purity and specific one sharp radioactive peak was obtained in . ; binding nature of existing antibodies, false a second chromatography purification, and ; diagnoses have been all too common, with this peak was subjected to native PAGE. j inaccurate therapy a further result. Autoradiography showed one distinct band 't Without a reliable method for early at 150 kDa, with other silver-stained [ diagnosis of ovarian cancer, dedicated proteins from rabbit blood not radiolabeled; ' research is crucial for improving methods However, the immunoreactisity of the for both diagnosis and therapy. One of our labeled antibody was not preserved. major areas ofinterest is the radioimmu- , nodetection (RATD) and radioimmuno- We developed a niethod to radiolabel ! I therapy GLAIT) of cancer. monoclonal antibodies, developed against human ovarian cancer cell surface antigens, , Radiolabeled monoclonal antibodies have with Au-198 and to retain immunoreactivity. , been used by numerous investigators in This was accomplished by protecting antigen nuclear medicine as well as in other areas binding sites with' affinity chromatography , oflife science mscarch. Murine monoclonal techniques using Sepharose 4B column. Sixty ; antibodies are increasingly used for percent of the total radioactivity bound to the t immunoscintigraphy and RAIT. However, antilxxiles was recovered by this method.- ] these agents are foreign proteins to humans and produce undesirable side Immunoreactivity of the radiolabeled . .; effects, such as Human Anti-Murine antibodies was first tested in a slot blot Antibodies GIAMA). In order to overcome experiment, where various types of antiger.s j the effects of HAMA, we have developed were bound to the nitmeellulose blot. Au-198 human monoclonal antibodies to purified labeled antibodies were reacted to these ; ovarian cancer cell surface antigens. antigens followed by autoradiography. -t Or e human monocknal antibody, TC5, Au-198 labeled antibodies reacted only to
- was found to be specific for ovarian cancer the extracts of ovarian cancer and a breast -(
as indicated by Western blot, immunodiffu- cancer but not to any normal cell extracts.' ' sion and fluorescent antibody assays. TC5 Binding studies using Au-198 labeled 't did not react with any normal cells of the antibody were furtLer conducted with ' ovary, uterus, cervix or fallopian tube, nor human biopsy specimens (Figure 1). In a l did it react with normal lung, heart or blind experiment, Au-198. labeled TC5 breast tissue. This monoclonal antibody reacted strongly with six out of six . was directly labeled with Au-198 and specimens pathclogically diagnosed as purified by column chromatography. The metastatic ovarian cancer (scrous and : purified Au-198 labeled antibody was endometrioid). One" normal" ovary tissue analyzed by using native polyacrylamide reacted strongly by our method; four months ; i gel electrophoresis (PAGE) followed by later metastatic ovarian cancer was ' autoradiography. A distinct band was diagnosed in this patient. Au-198-labeled j i l lc 37 ; l i
,-v-
100 TC5 did not bind with different types ao of normal tissue (ovary, uterus, j co . p fallopian tube, endometrium and ; 43 M W ! normal breast), but did bind to a breast gg cancer specimen. Our method offers g
;, o "
higher sens.'tiv:ty to detect ovarian ;o,oo cancer at its early stage compared to sk 5 ' existing metheds. We hope to use this l' highly specific human monoclonal
' % ==10 antibody and Au-198 labeling "- %
ser.n raa,, M,fs.n.t u ,..i l techniques, for early diagnosis (and q ['(",d'"a a$tj$undto y possibly treatment) of ovarian cancer. tiiopsy specimens , i PRODUCTION OF NO-CARRIER-ADDED Cu-64 Kurt Zinn, Tandra Chaudhuri, Steven Morris, Ting-Pang Cheng. Daniel Trokey and Walter Meyer ' (MURR) During the past year MURR staff developed a conducting the fluxtrap irradiations under new technique for the pmduction and purifi- bomn shielding. MUPJrs machine shop staff cation of very high specific activity of"Cu. The produced a special boron-nitride-lined can for development was sparked by collaborations with these irradiations. Under the guidance of the Dr. Michael Welch (Washington University), MURR ReactorManager, the can was tested who wished to use this radionuclide for imaging under a variety of conditions, and this year , with positron emission tomography (PETA In the can was approved for running in the flux this application of PET, a monoclonal antibody trap. Results indicate a 15-20 fold reduction directed against colorectal cancer was labeled in unwanted zine radioin. purities. The uith copper using a bifimetional chelate. A benefits of this special bomn-nitride-lined can relatively high percentage of the copper atoms go beyond producing a high specific activity attached to the antibody needed to be radio- "Cu: reduction of radioimpurities reduces the active to allow imaging in animal models. The radiation exposure to the individual purpose of these imaging studies was to processing the "Cu: and the reduced demonstrate that the radiolabeled antibody radioimpurities result in less radioactive ; could detect tumors in the animal model and to waste that must be packaged and shipped. ' establish the basic research required for human ' testing. Hence, a very high specific activity "Cu The key to prodacing very high specific
- was required. This was accomplished at MURR activity "Cu is the chemical separation ,
with the nuclear reaction "Zn(n p)"Cu. method. Our method employs a three-step Following the pmduction of"Cu, the zine target procedure to remove the zine target from the had to be removed in such a manner that all "Cu. First the "Cu and zine are dissolved in metal impurities were minimized. concentrated hcl and taken to dryness. The chloride salts are dissolved in 1 M acetic acid The fast neutron reaction pmducing the "Cu is and passed through a chelex column (4 ml); , ~) only one type of reaction that can occur with the the "Cu remains sekstively bound to the )
- high purity zine metal target. Thermal column, while the zine impurities pass l
) neutrons produce unwanted zine radioim- through. Following a rinse, the "Cu is cluted ! purities, mainly **Zn and "Zn. These reactions with 1 M hcl, and passed through an ion l were minimized in our production method by exchange column for final purification. As a i 38 !
.]
P'
?
1 1 measure of the separation method, a zine In summary, our method to produce "Cu has purification facter has been calculated. This - resulted in a very pure radionuclide with high !
. facter is the ratio of"Zn in the final "Cu measured specific activity. The boron-nitride- _ ;
solution divided by the total "Zn produced, ; lined can has reduced undesired thermal : and gives a measure of the fraction of zine neutmn reactions as well as radioactive waste. ! which makes it thmugh the purification - The separation method for purification of the E scheme. The zine separation factor for the "Cu was ten times better than literature . 3 current technique averaged 1.3 x 103, and mports, and could be accomplished in just 1.5 , with the best separation method reported in hours. The "Cu has been used in evaluating a the literature at 1.1 x 108, the MURR method 5 monoclonal antibody against colorectal cancer,8 offers a ten-fold improvement. and is currently being used in human clinical trials. Our group has also been actively , A second assessment of the "Cu radionuclide involved in using this unique radionuclide to._ j is the measurement of"Cu specific activity. investigate copper metabolism and evaluate This ratio is the "Cu correntration divided by copper-binding proteins in animals. the copper concentrationJ Copper concentrations were measured using graphite References j furnace atomic absorption. Early runs L A.K. Dasgupta. L.F. Mausner and S.C. averaged 282 mci /pg Cu, with 7.3rIr of the Cu Srivastava, *A new separation procedure for.
Cu from pmton irradiated Zn " Appl Radiat. a
. atoms being radioactive. We anticipate future runs will improve. For comparison, Mausner Isot., Int. J Radiat. Appt Instrum. Part A42, et aP reported 5 mci /pg Cu for"Cu 371-376(1991).
- 2. C.J. Anderson, J.M. Connett, S.W. Schwarz, .
production, which is 0.66% of the Cu atoms P.A. Rocque, L.W. Cuo, G.W. Philpott, K.R. radioactive. Another comparison is high inn, CMeares and M.J. Welch,
- Copper.64s
- specific activity "Re (3 mci /pg), with 1.6% of 8 labeled antibodies for PET imaging l'J. NucL the atoms radioactive- Med. 33,1685-1691 (1992). 1 DETERMINATION OF FLUORIDE IN HUMAN NAILS VIA CYCLIC INSTRUMENTAL NEUTRON ACTIVATION ANALYSIS d J.S. Morris, V.L Spate, C.K. Baskett, M.M. Mason and C.L. Reams (MURR) The role of fluorine in human health has are essentially pmtein that contain a large , become somewhat controversial. It is widely perrentage of n-keratin. We know of no accepted as pmtective against dental caries, reason to believe that fluoride actively - may be protective against osteoporosis, and participates in nail gmwth; however, it may has been very conservatively implicated with be passively captuwd pmportional to its level , osteosarcoma in male rats. We have found ~ofintake. To evaluate this possibility, we that toenails collected in population-based developed an NAA method using "F(n,fF epidemiology studies apparently reflect and applied it to toenails obtained from fluoride intake. To our knowledge none of ~ subjects consuming different levels of the geographical osteoporosis studies or drinking water fluoride. .. fluoride therapy studies, or any osteosarcoma " study known to us, have attempted to DETERMINATION OF FLUORIDE VIA NAA ' measure the individual fluoride status. Fluorine has one stable isotope, F-19, which:- llence,it was in this context that we began ' can participate in several nuclear reactions experiments in our labomtory to' determine if ' that are summarized in Table 1.- In the case neutron activation analysis could be used to of prospectively collected nail specimens, such ' measure fluorine in human nails, and if that as would be the situation in population based - measurement reflects fluoride intake Nails epidemiology studies, the total . sample 39:
Table 1 Fluorine Nuclear Data 0,,(RI) Target Nuclear or a, rRay (Abund %) Reaction ch Product t ,, E,(kev) Abund % -
"F, n,y 9.5(39) "F, 11.03 s if,33.6 100 (100) n.p 1.35 50, 26.91 s '97.1 95.9 n.a 7.85 "N, 7.13 s 6130 69 n,2n 0.0073 "F, 109.8 m 511 194
~ - - .
quantity is quite variable and small, ranging ! from 10 to 100 milligrams for most subjects. NAA Methods I r the Determination of Fluoride These small samples and poor F-19 thermal #sennot and epusennal neutmn mptum.* n,y . neutmn cross-section (9.5 mb) combine to make the determination of fluoride by NAA in % + 'n, -, F, + 7(pmmpt) these specimens quite challenging. Neverthe-less, we have managed to develop an adequate 2"F* w ("Ne'"T + *B4 + u , l method by summing the spectra from ("Ne'"r -, "Ne + 7 (delayed) , repeated cycles, each consisting of a 7-second
- irradiation,10-second decay and 18-second count. The nuclear mactions and experimental conditions are shown in Figures 1 and 2.
for "F*: t = 11.3 seconds and E'= 1633 Fig.1 Nuclear reactions for fluonne Fifty milligram samples,if available, are weighed into small (~ 0.5 m'.) high-density NAA Methods for the Determination of Fluoride polyethylene vials (UDPE) which are placed thermal and epithermal neutrun capture: n,y in HDPE rabbits for irradiation. The rabbits are transferred, with a four second one-way irrad. time = 7 see transit time, to the irradiation position $,, = 8x10 Sn.cnr2 .sec i immediately adjacent to the beryllium $g = 2x10"n.cm.2,3eca reflector, and reactor core, thmugh a decay time = 10 sec pneumatic tube. The thermal and epithermal count time = 18 sec neutron fluxes are shown m Figure 2. ; Following irradiation and return of the rabbit sample vial in contact with detector end cap. i to the laboratory, the sample vial is quickly 3 to 6 cycles, > 60 minutes between cycles removed and centered on the end cap in contact with a 30% HpGe detector. The _
+
samples are real-time counted for 18 seconds p g. 2 Experimental condmons used for the analysis of following a 10 second decay which is under fluorine at the MURR , the control of the data acquisition system. '!; The 1633.6 kev gamma-ray from the decay of Nucicar Data Interactive Peak Searth F-20 (t,, = 11.03 seconds)is measured using a program.- Data reduction is accomplished by [ Microvax-based spectrometer with a Tennelee standard comparison. ' 244 spectroscopy amplifier, Nuclear Data 599 .; loss-free counting module and a Nuclear Data FLOOR'DE STANDARDS - Twenty micro-
- 581 ADC. This analysis cycle is repeated for gram standards, giving 600 counts /pgicycle, .
cach sample 3 to 6 times at intervals of were prepared from a .100 ppm standard . appmximately 60 minutes or more. The (RICCA, Chemical Co., Arlingt4m, TX) by . spectral data are summed and the area of the pipetting onto a small quantity of filter paper 1633.6 kev peak is extracted using the pulp substrate (Schleicher & Schuell Inc., 1 40
~!
- Keene, NH) which had been placed in the Health Study submitted a set of toenail HDPE vials. The F standards were then frozen clippings for use in nested case-control studies and freeze-dried. relating diet and disease. A second set of clippings was obtained 8 years later from 70 STUDY SAMPLES All toenail specimens were of the subjects; and both sets were analyzed ' collected at various times as part of the for F in this study. We found that fluoride Harvard based Nurses' Health Study. The levels remained highly correinted (Spearman specimens were cleaned in DI water using a r = 0.60) over the eight-year period suggesting sonicator and allowed to air dry. When that toenails are a useful monitor of available, sample masses of approximately 50 individual fluoride status. mg were prepared. For approximately 207c of the samples, it was pessible to prepare a EXPERIMENT THREE Twenty-four of the duplicate. NHS participants that provided nail specimens in 1983 reside in Lynn, MA, which RESULTS AND DISCUSSION at that time had an unfluoridated water
- supply. In the ensuingyears, fluoridation EXPERIMENT ONE Nail specimens from 13 was implemented and a second set of nails women living in Holden, MA, a low fluoride was collected from the 24 participants eight '
area with a drinking water fluoride level of 0.09 years after the first, and several years after ppm, and specimens from 12 Boston area fluoridation began. Based on the 24 before residents, where the drinking water is fluoridated to a level of Table 2 Comparison of nail fluoride levels in subjects from 1 ppm, were analyzed municipalities with fluoridated and unfluoridated water using the above supplies described NAA method. The results F in Water F in nails (ppm) are given in Table 2. Locale (ppm) range mean* ' The Holden and - Boston means,4.2 and Holden, MA 0.09 2.4 - 9.7 4.2 6.4 , respectively, are Boston, MA 1.0 2.7 -10.1 6.4 significantly different (p < 0.05). However,
- means are signifcantly differont, p < 0.05 the ranges overlap (Table 2L One Hol%n subject had a toenail F level of 9.7 which was reproducible on a second and after samples, we observed a significant set of clippings. This value is significantly increase in toenail F levels due to higher than the means for both areas indicating fluoridation. The mean change was 2.1 ppm that while the toenail levels generally reflect F (p = 0.04) which coincidentally is practically drinking water levels, there are individuals that the same difference as observed in the toenail are misclassified. F levels from residents of Holden, MA (a low F area) compared to Boston, MA (a This could account for some of the _
fluoridated area)(Table 2). , inconsistencies and inccmclusione reported in * - the geographic-based epidemiology studies CONCLUSIONS where drinking water F concentrations have - been used as a surrogate for tissue levels in Geographical epidemiological studies relating- . predicting the incidence of osteoporosis. F drinking water levels to the incidence of osteoporosis are for the most part EXPERIMENTTWO Thelong-term inconclusive. In cases where a low F area (~ reproducibility of F in nails was evaluated. In 0.1 ppm or less) was included, the studies 19S3, over 60,000 participants in the Nurses' tend to show a relative protective efTect due to 41
, 4
- y
.r fluoride. In at least one study comparing 4 - While there is no dimet evidence that -
. ppm to 1 ppm areas, a greater incidence of fluoridation of drinking water increases the fractures occut red in the higher F area. As we risk of osteosarcoma in humans, the Delaney
- have shown in this study, the level of F in nails clause has prompted a call for further study is genemlly correlated with drinking water based on the development of a small number levels; however, there is an overlap that can of osteosarcomas in male rats consuming result in misclassi.fication and may explain highly fluoridated water, some of the inconclusive findings.
We have shown that neutron activation Fluoride therapy is controversial. Well analysis can be used successfully to measure designed and carefully conducted studies have, fluoride in human nails collectedin in one case found a significant protective effect, population-based studies, and that nails and the conclusive absence of such an effect in apparently do reflectintake. The NAA another. In both studies,incmases in certain method is based on cyclic NAA and could be , types of bone mass were reported. In the latter, substantially improved by reducing the 10 j cortical bone loss was also observed; and in second decay time through development of an ; both, there were non-trivial side effects due to automated process. The method will be j fluoride therapy. Again, no attempt was made applied to a population-based fracture study j to individualize F status. in the near future : DETERMINATION OF TOTAL AND BOUND SE IN SERA BY INAA ' V.L Spate, M.M. Mason C.L Reams, C.K. Baskett, J.S. Morris, and D.S. Mills (MURR) ; The role of dietary selenium as a protective paper as " bound Se " The development of -. agent against cancer and heart disease has high-purity germanium detectors and ! been studied in our laboratory in collaboration improvements in both the hardware and with epidemiology groups for many years software used for pulse pile-up correction and ' , using difTerent monitors of selenium status peak extraction now allow for the accurate ! such as blood, red blood cells, sera, plasma, determination of Se in fmeze-dried serum hair and nails. Since 1973, MURR Center that has not been otherwise altered by . staff members have been developing metheds dialysis or ashing. We refer to the Se ' for the analysis of selenium in biological concentration determined by this method as i sampho using the standard comparator " total Se " The difference between " total Se" method. This method is based on and " bound Sc"is timt small fraction of instrumental neutron activation analysis selenium that is either not bound to large - (INAA) using the Se-77m isotope, which has a molecules, or is fme to dissociate from them - :' half-life of 17.4 seconds and a gamma-ray during dialysis; We refer to that component energy of 161.9 kev. as the " free Se." l The analysis of bk>od serum using the dialysis We also make use of the samples prepamd for ] method at MURR has proven to be an _
" total Se" to determine the sodium . Z accurate and long-term reproducible method. concentration. This allows for the : . . =!
The Se component quantifled using the - identification, and normalization if desired, of dialysis method will be referred to in this those samples that have been mncentrated as - 1 42 j 1 s r
e a e a msult of freezer-burn or the efTects of QC sera (SK9-90)is uconstituted to a volume of , repeated thawing, aliquoting and re-freezing 3 ml using DI water. Replicates kr the deter-mination of" bound Se",
- total Se ' and sodium that sometimes occurs with these unique sera banks, prospectively collected, and limited in are prepamd as described for the study samples.
amount. .
. d Each dialysis rack is loaded with duplicate samples fmm four subjects and one QC serum This paper will discuss the standafdization and quality control approaches used to sample. The racks are placed in DI water at .
identify the relatively small" free Se" pool,' 35 C for one hour. The volume ratio of DI describe the two sample preparation methods water to sera is .approximately 500:1. After , and report on a comparison between " bound dialysis ofone hour, the samples are removed Se " " total Se" and " free Se" concentrations in and the outside of the dialysis membranes are - l' 977 case-control samples. rinsed with D1 water. The samples are : . frozen, then freeze-dried for approximately 12 E .; ' SAMPLE PREPARATION hours, removed, and folded in the shape of a -
"Z", then placed in t. numbered HDPE vial, t The study sera were retrieved from multi-year secured with a polyethylene plug, and capped. ]
storage and shipped frozen to MURR. The replicates prepared for ' total Se" and ' Samples were stored frozen until sample sodium are frozen, freeze-dried for 12 hours, : , preparation was done in sets with 20 subjects plugged and capped. Typically, the replicates'. , per set. Four one milliliter vials, each vial and QC specimens for approximately 40 containing approximately 0.5 ml, were subjects are prv: pared per day. shipped for each subject. The contents of the ; four vials were mixed to produce a composite RESULTS AND DISCUSSION , sample having a volume of approximately two . . milliliters. One hundred and ten " bound Se" and " total Se" selenium standards wem analyzed on the Duplicate samples for both the " total Se" and same day to quantify the difTerence (net --
" bound Se" configurations were prepared from counts per pg) due to the slight difTerences in 'j '
the two ml composite sample. Typically, the geometry and gamma-ray absorption. These - duplicates for the determination of" bound Se" results rav shown in Table 1. SRM-1577 l were prepared first followed immediately by bovine .iver samples, prepared in the two i those for the determination of" total Se" and difremnt configurations, were also analyzed . sodium. The composite sampleis thoroughly using the above mentioned standard data. l vortexed immediately prior to pipetting each The bovine liver results are given in Table 2. j aliquot. Dialysis membranes 7.5 cm in length . . _ . _ are freshly prepared, labeled with the The data in Tables I and 2 were taken from ; assigned sample number and placed in the stimdards and SRMs which were analyzed on ' ; specially designed plexiglass dialysis racks the same day over a continuous 6 hour periodi ; with a ten-membrane capacity. In turn, each There is a small but significant (p < 0.001F , membrane is individually plawd on a holder difTerence (~4%) between the " bound Se" vs i on an analytical balance and samples of " total Se" counting geometries (Table 1), approximately 0.5 ml are carefully pipeted However, the standardization approach used 1 into the dialysis membrane and the mass is accurately compensates for this difTerence in ~! determined by difTerence. After the
- bound actual samples (Table 2L 7 Se" duplicates am prepared for each sample, .
j the duplicates for the " total Se" and sodium Results for the MURR QC serum (SK9-90) .. determinations are prepared by pipetting previously described are given in Tables 3 and - 1 approximately 0.3 ml of the composite serum 4. The data in Table 3 were taken in a l into pre-numbered 1.5.ml HDPE vials preliminary expciiment to demonstrate the - l positioned on the analytical balance. Again low variability due to sample preparation over . j the mass is determined by difference. a 10 day period. The data in Table 4 resulted - l l 3 o 43 [ c; r
g F from the analysis of the MURR QC
' Table 1 ~ Comparison of seleniura standards used in the determination of serum selenium sera over the 9 months during which concentrations the case-control analyses were done.
In both cases the MURR QC sera, once mp s ug* % C.V. reconstituted to 3 ml, were aliquoted to - Geometry prepare three 0.5 ml replicates for the
' Bound Se* 110 '72061 123 0.2 " bound Se" determination and two 0.3
" Total Se' 110 75081 69 0.1 ml replicates for the
- total Sc" determinations. In the preliminary difference between geometre conhgurations is signifcant u# ment onh MW NM at p <0.001 scrum was used whereas a random
,_ selection pmcess including all Table 2 Comparison of the Se concentration in SRM- concentrations of SK9-90 were used 1577 Bovine Liver analyzed using " bound with the case-control analyses. All ?
r Se" and " total Se" standards concent. rations w;ere normalized to the : ' Number of Mean Stan63rd undiluted sera. Geometry samples . PPM e.wr *4 C.V. The 7% difference between the " bound -
" Bound Se" 6 1.139 0.035 35 Se" and " total Se" concentrations
" Total Se* 9 1.129 0.034 3.0 I which remains after the geometric -
correction is made is statistically Table 3 Se concentration in "MURR" quality control significant (p < 0.03). We have defined sera SK9-90 sample preparation variability trial this as the " free Se" component which is either alow molecular weight Se Mean Standard compound present in sera or a - Treatment Number PPM
- error % C.V.
fragment that dissociates during
" Bound Se* 30 0.108 0.0007 0.6 dialysis.
" Total Se* 20 0.116 0.0030 2.4 Significant difTerences between " total
- difference is signsfcant at p < 0.05 geaand
- bound Se"in this study were observed in both the MURR QC and Table 4 MURR quality control sera (SK9-90) analyzed study sera sets. consequently, we over a 9 month period have defined the ' free Se" component .
Mean Standard to be the difference between these two . Treatment Number PPM
- error *A C.V. pools. Hence,the" free Se"poolis generally that small fraction of the
" Bound Se" 174 0.106 0.0008 S.5 serum Se thatis either not bound to
" Total Se" 116 0.113 0.0023 14 protein, or some other high MW -
I
- difference is signmcant at p <0 00 8PUCiC8' or is free to dissociate from
! such compounds. _ Of the 977 case-
' control samples,651 had_" free Se" Table 5 Comparison of " Bound Se" and " Total Se" components, i.e., the " total Se" was concentrations in 977 sera samples from a case control study over a 9 month period greater than the " bound Se " Twenty _ q w
three percent were greater by ono Mean Standard standard deviation or more. We Treatment PPM
- Deviaton Low PPM High PPM Separately tested the correlatiou >!
" Bound Se* 0.109 0.0174 0.060 0.185 een b b e M w M h W !
" Total Se" 0.115 0.0273 0.060 0 657 Se" and " bound Se" pools. Thi.re is no j Total Na 3214 182 2tB9 4053 significant correlation betwetn the
" free Se" and " bound Se"(r = 0.06);
- bound Se vs " total Se" concentration means are however, the " free Se" and
- total Sc" signifcantry different, p < 0.001 pools are highly correlated (r = 07/8). -;
I
'I i
q
~ . . . . .
,_ y e - .
'a.
,- p Q , CONCLUSIONS -
There is a small difference between the A correlation (r = 0.59) between the %und Se" ~ :
%und Se" and %tal Se" counting a ,al 't<.tal Se"_was observed in this study. '
geometries which was accurately however, a stmnger cormlation (r = 0.78) exists . compensated by the standardization between %tal Se" and " free Se" concentrations appmach used. The MURR quality control with no correlation (r = 0.06)between %und - , sera had 6% diffemnce between the mean Se" and "fme Se" concentrations ofselenium in sera.
%und Se" and " total Se" concentrations.
It has been shown that there is also a We would recommend the continued analysis of significant difference (5.2%) between both %und Se" and " total Se* to test ,
%und Se" and " total Se' concentrations hypotheses mlating %und Se,"
- total Se," and in study sera samples. A small, but real, " free Se" serum selenium concentraticns to fraction of the selenium in human serum disease end points. Additionally, the' .
is either not beund to high MW (12,000 D) determination of sodium is useful to determine if species or is free to dissociate from them the serum has been concentrated duringlong-during dialysis against DI water. term storage. THE DETERMINATION OF SELENIUM IN URINE C.K. Baskett, V.L. Spate, V.M. Mason, C.L. Reams, J.S. Morris Selenium is an essential trace element in selenium as monitomd by the urine.' The + human nutMon. It is present at the active second objective of this study was to apply the site of gluti .ione pemridase, an enzyme method to a dietary trial whic> was designed that catalyzes the breakdown of to evaluate and correlate vanaus dietary , hydroperoxides, maintairdng the monitors, such as, urine, blood, sera, and ; appmpriately low levels c,ithese oxidants in toenails. This method would then extend the the cell. The status of selenium in humans is selenium methodologies that are already used .' : assessed by estimating dietary selenium in our laboratory for blood, sera, plasma, and intakes, by measuring selenium in tissues or nails to include urine. The procedure for excreta, or by determining glutathione sMenium analysis discussed in this paper was perexidase activity in blood components. applied to urine samples from a selenium Dietary selenium intate causes urinary supplementation study conducted in ' ; concentration of selenium to change rapidly. collaboration with Harvard Medical School. 1 It was determined that the urine selenium concentration may be a sensitive indicator of The selenium feeding study conducted at I selenium intake. Harvard Medical School consisted of12 healthy, adult male subjects who were , This study had two major objectives. The randomly assigned into three groups. Whole first was to develop a method for the NAA of wheat bread was chosen as the medium for , urine which could be applied to the large the selenium because grain is a major source quantity of samples required in of dietary relenium. The study bread epidemiological studies. Udne samples contained three different doses of selenium cannot be analyzed byINAA due to the determined by the fraction of high-Se wheat ' interference fmm the sodiurr contained in flour that was used. Subjects were requested the urine. The method developed focused on to eat two slices of the study bread daily for ~ , minimizing the required chemical steps to a one year. The contml who?e wheat bread ; manageab!c level, while still pmducing useful contained 32.410.2 pg relenium per two epidemiological data regarding dietary slices, the medium dose bread contained 206
..} l 1 '45 - i r
q . i i 17 pg selenium per two slices, and the high prepared. Deionized water was used for the dose bread contained 388 22 pg selenium analytical blank. The SRM urine and the - per two slices. Toenails, whole bknod, sera, blank were pmpared in the same manner as and urine were collected at regular intervals the urine samples. The NIST urine was during the feeding year and the following lyophilized and had to be reconst.ituted before year. pipetting. Blanks were prepared with each group of samples which went through the The urine samples must be chemically separation procedure. separated prior to the irradiation due primarily to the large amount of sodium The Se-75 standards, the urine samples and contained in the urine. The separation duplicates, the SRM urine, and the blanks procedure used for urine is based on a co- were counted on a Nal detector, attached to a pmeipitation of the selenium with arsenic. multichannel analyzer, to determine the Five ml of urine was pipetted into Erlenmeyer percent yields of the Se-75 fmm the flasks and the sample mass was determined. separation procedure. The application of the All urine samples were prepared in duplicate. arsenic-copmeipitation separation to Approximately 1 x 108 pCi ofquantified Se-75 undigested urine specimens produced tracer solution, diluted fmm high specific consistent yields ranging from 65 to 87%. The activity Se-75 produced at MURR, was added yields between duplicate samples were very to each flask. The flasks were heated on a hot similar. plate to just under boiling, fbr approximately five minutes. Carrier solution containing 5 Fifly-eight urine samples from the fbeding mg As was added to each of the flasks. The study, along with duplicates, SInf urine, and samples were heated for an additional five to blanks, were analyzed according to the So ten minutes. Three ml of hypophosphorus 77m analysis metimd used in our laboratories, acid (50% ) was added as a mducing agent and Se-77m is useful for the measurement of samples were heated another five to ten selenium because ofits favorable production minutes. A second three ml aliquot of and decay parameters. Se-77m, the isotope of hypophosphorus acid was added and samples interest, has a gamma-ray energy of 161.9 were heated for an additional 20 minutes. A kev and a halflife of17.4 seconds. Each dark, almost black, arsenic pmeipitate formed sample was placed in a shuttle rabbit and . during the heating. Selenium was also irradiated for five seconds via the MURR reduced and co-precipitated with the arsenic. pneumatic tube system. The thermal neutron The precipitate was filtemd onto a 0.8 micron flux in this irradiation position is Nuclepore fiher membrane. The flask was approximately 8 x 10" n cm-2.sec2 . The rinsed with deionized water and acetane to shuttle rabbit was returned to the laboratory remove any residual precipitate. The and the sample vial was quickly removed and Nuclepore filter membrane was folded, using transferred to the appropriate counting plastic forceps, and placed inside a high geometry. The decay time for each sample density polyethylene MURR vial. A was 15 seconds and the real time count was polyethylene spacer was placed on top of the 25 seconds on a high resolution gamma-ray filter membrane to maintain the same spectrometer. The spectrometry system geometry in all samples and a lid was placed included a Tennelec 244 amplifier coupled to , on the vial. a Nuclear Data 599 loss-free counting module _ .; and a Nuclear Data 581 ADC. Data { Se-75 tracer standards were prepared to acquisition and peak extraction were done i check the percent yields of the separation. using a VAXstation 3100, nodel 38. National Institute of Standards and Technology Urine (NBS SIB 12670)was The Se-77m concentrations were then prepared as a qtmlity enntml chek of the determined using the standard comparator separation procedure. Both normal level and method. National Institute of Standards and elevated level of the NIST urine were Tecimology Bovine Liver (NBS SRM 1577) 4ti
,y
was analyzed with each batch of samples as - The urine samples were analyzed in L .. an additional analytical quality contml check. duplicate. All duplicates had a coeSicient of.
. The bovine liver SRM was not subjected to variance ofless than 51 The concentration -
the pre-irradiation separation. It was ofselenium in the urine samples ranged from'. primarily utilized to ensure that the Se 0.0168 to 0.7071 ppm. The mean - compar: son standards are accurate.-- concentration of selenium in the 58 urine samples fmm the feeding study was 0.0904 ' The certified concentrations of selenium in ppm. The urine msults are shown in Table 2. the normal level and elevated level NIST urine are 0.03010.008 and 0.46 0.03 ppm, In conclusion, the pre-arradiation separation - respectively. Our determined concentration which was used appears to be a useful of 0.027 ppm selenium for the normal level appmach for the analysis ofurine for - i urine is within the acceptable range. selenium using NAA. This method is useful for the analysis ofi F - selenium in urine as a - [ reDectionofdiet. Useful' L Table 1 Quality Control Samples and Blank epidemiological data can [:. l Certified Se be obtained by using - Quality Mean Se urine as a dietary l PPM ( Control PPM Std. Dev. % C.V. monitor for selem,um. i i L Normallevel 0.027 0.010 - 37 0.030 10.008 Thelevel of the selenium ~! unne supplement could be (NBS 2670) detectedin the Elevated level 0.56 0.03 5.6 0.4610.03 -l unne concentration. The 1 (NBS 2670) separation procedure can be applied as a screening - Bovine liver- 1.16 0.03 2.3 1.110.1 method for the large-(NBS 1577) sample sets requiredin Blank O.0029 0.00076 26 epidemiological studies. This method gives useful
- Bov'ne e hver SRM used as analytical QC, did not go through separaton procedure. - results for selenium with a limited degme of ~
u chemical processing. However, the vefficient of variance was F Tam 2 wne specirnens rather high. Our determined concentration of 0.56 ppm selenium for the elevated urine is n 1.ow Se High Mean Mean % C.V. . above the acceptable range, but the coeflicient Duplicates . PPM SePPML Se PPM for Dupts.' of variance was 5.6% The SRM's had been lyophilized and consequently required 58 0.0168 0.7071 0.0904 2.364 reconstitution prior to analysis.- The study specimens had been stored frozen. Perhaps the freeze-drying process afR cts the pre-irradiation separation. The certified There was a dose-response relation observed concentration for selenium in NIST bovine between the selenium intake'and the urine liver is 1.110.1 ppm. Our determined selenium concentrations in the samples from concentration of selenium in NBS 1577 bovine the selenium supplementation study liver was 1.1610.03 ppm selenium for all . conducted at Harvard Medical School. Urine '. analytical runs The results of the quality samples were compared with sera and whole . control analyses am shown in Table 1. blood samples fmm individuals in the 47
0.5 , selem,um , supplementation s
- study. The selenium g 04 -
~~,,..
concentrations in o , the urine were Q , a
- 4; .. ~~~,,..
~ '
highly correlated a 03 - with both the
* * ' - i~~*...
selenium concentrations in J b 02
^
-kY. ,* o o sera (r = 0.70) and S ed
- 4 whole blood (r = d sce'% #o
~
0.72). These E 0 to relationships are shown in Figure 1. ,, , , , 0 00 0.10 0.20 030 0.40
""" 7"' "'" ? T.
- URINE PPM Fig.1 Unne vs, sera and whole blood 48
ACTINIDE CHEMISTRY - GROUP PERSONNEL , Truman Storvick, Group Leader, Professor of Chemical Engineering' C. Leon Krueger, Research Scientist Paul Sharp, Senior Research Investigator (MURR) and Associate Professor of-Chemistry FACULTY ASSOCIATES AND VISmNG SCIENTISTS LeRoy Grantham, Senior Chemist, Rockwell International David Grimmett, Chemist, Rockwell International Jeff Roy, Chemist, Rockwell International Hajime Miyashiro, Senior Research Engineer, CRIEPI David Retzloff, Associate Professor of MU Chemical Engineering i Yoshiharu Sakamura, Research Engineer, CRIEPI , The Actinide Chemistry Group was spent nuclear fuel from the boiling formed to do experimental work on water reactors used to generate - uranium and the higher actinides electricity. In the PUREX process, the under contract with Rockwell metal oxides in the spent fuel elements International, Rocketdyne Division, are dissolved in acid and the uranium , Conoga Park, CA. Funding comes to and plutonium are recovered by a Rockwell International from Japan's combination of liquid extraction-electric power industry through ch emical complexingbetween aqueous = contract with Kawasaki Heavy and organic phases. The PUREX. Industries (KHI) and the Central residue (about 3-4% of the total metal Research Institute of Electric Power content of the spent fuel) contains all Industries (CRIEPI), both of Tokyo, of the fission products, some uranium - Japan. The Department of Energy, and plutonium, and the minor USA, has provided the pure uranium, actinides: neptunium, americium and neptunium, plutonium and americium curium. These actinides have long ! metals that are used in the half lives and present .long-term , experimental program. radiological hazards (tens ofthousands _l of years) which must be managed if .; TheJapanese plan touse theTRUMP- placed in a repository. '"he TRUMP-S - q
~
S (IRansuranic Management by process is designed to remove the Eyropartitioning-Separation) process actinides from the PUREX residue. ; to remove the transuranic metals from Removal and fissioning or transmuting the liquid extraction residues from the the minor actinides produces a smaller . PUREX process used to reprocess the residue stream that should require . l r 6 I 49 l
management for 200-300 years. The for the TRUMP-S process. Instruments
, : TRUMP-S process can also be used for have been developed: to measure the- (
- "on site" repmcessing of the metal fuel standard potential of the actinide metal that is proposed for the next generation chloride in equilibrium with the-pure -
ofliquid metal cooled nuclear reactors for metal. The electrochemical experiments' - ~ 1 production ofelectricity. useless than 10 mgofactinide chloride to ! conservetheavailablepureactinidemetal - The proposed pyropartitioning- and to reduce radiation levels so that the .! separation process is dry. The aqueous work can be done.in a glove box. The ; 3, PUREX residue streaal is dried and experiment can be modified to measure l j denitrated, the metals are chlorinated the activity coeflicient of the actinide :; and dissolved in fused salt. Processing metals dissolved in cadmium. must be done in an inert atmosphere . because all of the metals are chemically Thisyearhasbeen spent on the properties : active and readily form oxides, nitrides - of americium chloride and ' americium ! and hydrides which areinsolublein fused metalin cadmium. The measurements 3 salt. Molten lithium chloride-potassium suggest that americium chloride.is chloride eutectic salt provides a solvent present in both the +2 and +3 oxidation l for the metal chlorides at 400-500 C. The state in the fused. salt when it is in1 1 actinide metalchlorides canbe chemically equilibrium with pure metal. This i reduced to metal and alloyedinto a liquid complicates the ~ electrochemical - i cadmium phase placed in contact with - measurements and the interpretation of '
- the fused salt mixture. The chemical the experiments.1 The potential of the .
reduction leaves the more chemically americium chlorides is closer to the activelanthanidemetalsin the saltphase lanthanide chlorides and this will make il i with a small fraction of actinide metals. it the most difficult actinide to remove - l Thelasttraces ofactinide willbe mmoved from the salt without removing the; ; from the fused salt by electrolytic lanthanide metals. It is important.to f j- reduction to an inert ehrtrode. know this potential accuratel1 l l Interpretation of the 'americi..- . { The experimental program at MURRis measurements continues as the ! 4- designed to provide laboratory measurements. of the equilibrium ' [ l measurements to determine the separation coefficients the pure actinides ; I thermodynamic and rate data required fmm the lanthanides begin. !
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NEUTRON MATERIALS SCIENCE PROGRAM James J. Rhyne, Coordinator (acting) G. David Peeler, Senior Research Engineering Technician Mary B. Seewoster, Senior Secretary Grcups in the Neutrrm Materials Science Program: Electmnic and Mechanical Pmperties Magnetic and CrystalStructures Neutron Optics Nanostructures and Excitations Gamma Ray Scattering The new Neutron Materials Science Program detector array, a small angle scattering includes groups who primarily use elastic and spectrometer in vertical geometry, and two inelastic neutron scattering, gamma-ray neutron interferometers. scattering, and neutron radiation damage in their research work. The groups are Electronic Significant instrumentation funding was and Mechanical Properties; Magnetic and awarded last year from the National Science Crystal Structures; Nanostructures and Foundation (NSF), supplemented by university > Excitations; Neutron Optics; and Gamma-Ray resources, to provide for the construction of an Scattering, and include members from MURR entirely new 15 m high-resolution horizontal and from MU Physics, Chemistry, and geometry SANS, and the initiation of a joint Mechanical and Aerospace Engineering program with the Ames Laboratory of Iowa departments. Major collaborative programs State University for the upgrading and are maintained with scientists from MU modernization of the Ames triple-axis departments, and a number of outside spectrometer which was moved to MURR from universities, national laboratories, and the de-activated ORR. In addition to these industrial research organizations. new instruments, extensive modifications are being made in an existing diffractometer to The scattering research makes use of the six provide a neutron reflectometer facility. Work radial beam tubes at MURR of either 4* or 6" is also underway on a new residual stress - diameter which view the core at three closely- facility. It is anticipated that all of these spaced vertical positions. Because of the light instruments will be fully operational during water moderation, extensive use is made of the coming year, and will provide state of the cooled and room-temperature silicon and art diffraction and scattering capabilities for sapphire filtering in the beams before the research at MURR. A schematic drawing of instruments. Of the six beam tubes, five are the existing, new and upgraded instruments devoted to neutron scattering facilities, and on the beamport floor is shown in Figure L the sixth is a filtered neutron beam used by , nuclear engineering. The MURR-MU Physics neutron , interferrometry program, funded by NSF, is The present beamport facilities include a high the only such facility in the US. The recent resolution powder diffractometer, a triple axis obr,ervation of the Aharonov-Casher effect for spectrometer,two single crystal diffractometers, neutrons which has attracted wide attention a long wavelength diffractometer with a five was made at this facility. ; 53 l i
~j- - i In addition to neutron scattering, MURR ; An extensive elTortis underwayin the Electmnic 1
- alsohas a program in gamma-ray scattering . . and Mechanical Properties group to' study the -
' which utilizes high intensitygamma sources - effects of high energy neutron irradiation on produced by irradiation in the MURR flux - the new ceramic . superconductors and- on :
+ rap. The facilities include a gamma-ray semiconductor materials. A crystal growth a diffractometer MUGS, and a photon analog effort on the YBa,Cu,Oi has.' been highly; j of a triple-axis spectrometer, QUEGS, successful, and the neutronirradiation produces l employing the Mussbauer effect and used significant enhancements in the critical current ;l for quasi-elastic gamma spectroscopy. Tlus density achieved in these materials. j latter instrument is currently being significantly upgraded, the result of a DOE Summaries of the major mscarch projects in . j instrumentation development grant, to the neutron and gamma ray scattering group) include fourindependent gamma-ray beams and descriptions of the instrumentation and a new detector system. upgrades are in the following pages.
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Pg.1 Neutron scatronng instruments on the beam-port floor at MURR. Instruments shown dotted are under development. l c i
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54 ,
l ; ELECTRONIC AND MECHANICAL PROPERTIES GROUP l PERSONNEL John Farmer, Group Le 3 der (Adjunct Associate Professor of Physics and Adjunct j Associate Professor of Electrical and Computer Engineering) Aaron Krawitz, Senior Research Scientist (MURR) and Professor of Mechanical - ; and Aerospace Engineering i Andrew Winholtz, Research Scientist (MURR) and Assistant Professor of ' s Mechanical and Aerospace Engineering , FACULTY ASSOCIATES I David Cowan, Professor of Physics Jon M. Meese, Professor and Chair of Electrical and Computer Engineering > t The Electronic and Mechanical role of defects in the enhancement of Properites Group at MURR has a these very exciting new super-commonality based in materials conductors. science, but the research has a n atural , [. division between electrical and The M echanical Properties component mechanical properties. The efforts in of the group formally began with the the Electronic Properties area have addition of R.A. Winholtz in August had a strong basis in the 1991 and the change in status of characterization of radiation' damage Professor Krawitz after his return from in semiconductors. More recently, the a research leave in January 1992. Both focus of research has shifted to the are now half-time in the MAE study of defects in high temperature department and MURR Center. This supercond uctors. The inability of these component is primarily concerned with matelials to carry a useful current has neutron diffraction measurements of been a hindrance to many of the residual and applied stress. The exciting applications that were current research program is focussed originally envisioned. Itis known that on the construction ofa new, dedicat ed ; the introduction ofirradiation defects instrument for residual stress can increase the current carrying measurement, the establishment of a capacity of these materials. Neutron ca pability to measure residual stresses irradiation, in particular, appears to forindustrial customers, and continued i enhance greatly the usefulness ofthese scientific research concerned with new superconductors. The Electronic residual stress methodology and Properties group is investigating the problems. i I 55 l
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i HIGH TEMPERATURE SUPERCONDUCTORS d John W. Farmer GIURR), Paul Chu (University of Houston), Marcus Kirk (Argonne National Laboratory) and Matt Kramer (Ames National Laboratory) , The Radiation EfTects program at MURR efficient method of all for increasing the has been studying the role of neutron critical current the high temperature irradiation induced defects on the ability of superconductors. , high temperature superconductors to carry current. The inahility of the new materials Mo> e recent results indicate that the to carry useful current has been a hindrance enhancement mechanism is more complicated , to the development of many of the exciting than expected. The neutron irradiation , applications that high temperature produces a large amount oflattice expansion. superconductors promise. It is generally More important, the expansion exhibits an , undarstood that the cause of the limited non linear dependence on fluence (Figure 1), current capacity of the new superconductors The unusual expansion suggests that oxygen is due to the movement of magnetic flux vacancies play a dominant role and that it (fluxoids) within the sample, and recently it may be possible that more simple point has been shown that neutron and other defects can contribute the flux pinning. We forms ofirradiation greatly enhance the have observed that the final value of the current capacity of these new materials. It enhanced current is strongly sample is believed that the defects introduced by dependent as well as a function of fluence. irradiation act as pinning centers which The sample dependence indicates that the prevent or impede the motion of the fluxoids irradiation induced defects are interacting and thus lead to enhanced current capacity. with existing defects and that this interaction 3 MURR-based research and collaborations can play an important role in the pinning have focused on understanding the process. Further work is ongoing to
- mechanism that produces the beneficial understand this interaction and to find the efTects of neutron irradiation in order to optimum process for enhancing the critical :
optimize their beneficial efTects. current. Estly MURR results indicate that um neutrons are much more effective than most other forms ofirradiation. It was postulated that the small displacement "" [' cascades (10 to 30 A) unique to neutron irradiation are responsible for the u,% . ; superior efTectiveness of neutron ? irradiation. These clusters are heavily 2 damaged regions which act as very 6 m effective pinning centers for magnetic flux due to their near optimum size (approximately the magnetic coherence
- R length). Materials irradiated at MURR have shown current denaities among the highest in the world, currents that are ,S ow r okn we me.. e adequate for most of the applications of j high temperature superconductors. Fluence W cm m MURR research has also shown that R91 The change h sample volume as a function of fast -
neutron irradiation is far more efTective r.eutr n fluence; the rate f change increases with , '! nuence. ms sumnsing msutonay be due to ennect than eitbar Proton or electron of orygen vacancies and implies that a large number of irradiation and may in fact be the most point defects are pmduced in neutron irradiation. i I 56
1 NEUTRON LINE BROADENING STUDIES RESIDUAL STRESSES IN ADVANCED SOLID ROCKET MOTOR CASING , Aaron D. Krawitz and R. Andrew Winholtz (MU Mechanical and Aerospace Engineering Aaron D. Krawitz and R. Andrew Winholtz and MURR) (MU Mechanical and Aerospace Engineering and MURR) For many years studies of the broadening of x-ray diffraction peaks due to plastic The Advanced Solid Rocket Motor (ASRM) deformation have been conducted using is the next generation solid rocket booster Fourier methods. The physical origins of such for the NASA Space Shuttle program. A - broadening, which correlate with a variety of project has been funded to characterize the physical properties, can be separated into two residual stress state associated with the quantities, particle size and strain variance, welding procedure in the vicinity of the < In engineering alloys, particle size usually weld at representative locations, , refers to the average size of dislocation cell particularly in the steady state weld region, networks (mosaic), and strain variance refers The actual sample to be investigated is a - i to the local variation in interplanar spacing, sub-scale model of an'ASRM cylindrical-also due to dislocations. The object of the section. The ASRM is assembled from a study is to apply the method to neutron series of circumferentially welded sections g diffraction patterns. This involves adapting of a high strength (HP9430) steel. i an exis. ting x-ray analysis program, < determining minimum breadths and Residual stresses associated with the intensities suitable for analysis, and steady state weld will be determined in the comparing results with simpler integral peak weld and unafTected base metal regions of a breadth methods previously used in our work. subscale cylinder of approximately 36 in. Such an application has only become possible diameter by 0.59 in. wall thickness, a with the construction of high resolution Regions of specific interest include the weld neutron powder diffractometers, such as the center line, first pass heat affected zone, instrument on beamport D. just outside the cap pass heat affected zone, and the base metal. About five positions - A series of rolled copper plate samples (22,40, through the wall will be investigated. Data 59 and 72% reductions in cross-sectional area) collection will provide information have been measured, with matching concerning: j standards recrystallized to remove cold work. Her ults indicate that the percent difTerential 1. The sign and magnitude of the broadening (%DB) measured for the lower residual stress state. I angle peaks, ~45*2q, is not suflicient without 2. The directions of the principal extended data collection time, due to the stress axes. 1 instrument resolution function. The rule of 3. The effect on the stresses of a post thumb for x-rays is that a minimum of ~ weld heat treatment on the as-20% DB is needed for good results. Neutrons welded stress state. may require a higher minimum because the 4. The effect of a hydroproof test on ' run times needed for statistically sufficient the post weld heat treated cylinder. intensities become impractical at the lower percentages. Experiments will be also be This workis supported by a research ' performed on cemented carbide composites. contract with Babcock and Wilcox. i 57 .;
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, m 3
RESIDUAL STRESS IN METAL MATRIX COMPOSITES - Aaron D. Krawitz and R. Andrew Winholtz (MU Mechanical and Aerospace Engineering and ,, MURR) and R.J. Arsenault (University of Maryland)
' Modern composite materials are typically spheres (diameter- 0l5 mm). Results combinations of two mechanically combined indicate that the average stresses in the Al . ,
i phases for the purpose of obtaining enhanced matrix for whisker and spherical sic physical properties, most commonly strength. A reinforcement are close in value and greater .l major class of composites consists of a metal than for platelets (Table 1). These results -! matrix reinforced with a high strength ceramic di&r from finite element model predictions component. They are mixed, bonded at elevated and indicate that particle spacing, as well as temperature, then cooled. Because of the shape, determine the magnitude of thermal i di& rent properties of the constituent phases, residual stresses. It is also noted that the i the rates ofcontraction upon cooling are general stress level is quite low, indicating typically very different, creating what are the sensitivity of the method. known as residual microstresses. Neutron diffraction is particularly useful for the , , measumment of such stresses because of their extreme depth of penetration relative to more _. conventional x-rays. This enables good volume averages to be obtained, even on actual parts,
" { ~
and avoids surface preparation problems. ~
" 1 i
-se-I -
The nature and role of such residual stresses in metal matrix composites has been the subject of M33 " - [ two studies conducted at MURR in collabora. (MPa) , j _ tion with Prof. R.J. Arsenault at the University , ofMaryland. The first studyinvolved measurements of microstresses in silicon _1g _ carbide (sic) reinforced 1100 aluminum (Al) x FEM Tenst!e Defortnation a
+ FEM Compressive Deformation alloy. Measurements were made on samples a Exp. Tensile Deformation containing 20 volume percent (V%) sic in the -2ea a Ee conwsyn Deonna form of whiskers (length-to-diameter ratio - 2, e e.et e.e2 e.e3 diameter = 0.5 mm), platelets (major diameter- Iei i to-thickness ratio - 3, diameter - 70 mm) and Fig.1 Deformation-induced changes of a' verage matrix residual stresses in the longitudinal direction in sic /Al as a function of applied tensile and
- compressive strain.
Table 1 Thermal residual stress in the Al phase of 20 V% sic /Al composites The second study monitored changes in sic sic Transverse Stress Longitudinal stress whisker (20 V%) reinforted 6061 Al-Morphology (MPa) (MPa) composites subjected to deformation.
,l Measurements were made using the actual ! ! Whiskers 58120 110119 mechanical test samples. The changes were .l Spheres 94120 100t19 found L be asymmetric in response to )
Platelets 32116 43116 uniaxial external tensile or compressive loads -l _ . _ . _ . . _ . _ _.._ applied along the longitudinal whisker axis. l 1 58 i I
The changes in the longitudinal direction References are shown in Figure 1. The initial residual ' 1. L.F. Smith, A.D. Krawitz, P. Clarke, S. stwss in the undeformed samples is about Saimoto, N. Shi and R.J. Arsenault, 150 MPa, i.e. the changes due to tensile " Residual Stresses in Discontinuous? ~ deformation are substantial. Finite 1 Metal Matrix Composites," Mater. Sci. element and analytical models were Eng.,in press. developed to predict the behavior, which 2. N. Shi, R.J. Arsenault, A.D. Krawitz and , was found to arise due to a gradient of L.F. Smith," Deformation-Induced t plastic flow in the matrix. Le relation of Residual Stress Changes in sic Whisker , such an asymmetry to residual stresses has Reinforced 6061 Al Composites "Metall. H been a subject ofcontroversy. Tinns. A,in press. 6 RESIDUAL STRESS AND STRESS DISTRIBUTION IN TUNGSTEN CARBIDE-NICKEL - COMPOSITES Aaron D. Krawitz and R. Andrew Winholtz (MU Mechanical and Aerospace Engineering and . MURR) v Tungsten carbide (WC) particle reinforced diffraction data and a new set of samples composites are the basic class of materials has been produced and measured. As a used for high performan-e cutting tool and result of this work, the stress magnitude rock drilling applications. While the most and distribution is understood to be - common grade is WC-cobalt (09), in our related to particle shape and size, mean present work, the metallurgically simpler free metal binder spacing, local variations , metal nickel (Ni)is used. These materials in rietal binder spacing, and the in situ l are produced from powders sintered at yie'.d strength of the metal, which is high temperature (- 1400 C). Due to large afrated by dissolved tungsten content as difTerences in their coefficients of thermal wa i as particle spacing. expansion,large thermal residual micro-stresses levelop upon cooling and have Thermal residual strains in WC-Ni - been characterized using neutron composites of 11,20,40 and 60 V% WC diffraction. In addition, diffraction peaks were measured using neutron diffraction ' are observed to be significantly broadened techniques. Cell parameters and volume due to a range of residual stress around an fractions of the phases were determined average value. The origin of this using the Reitveld profile refinement broadening is not clear but has potential method. Gaussian fits to Ni(111,200,311 ; implications for failure of the material in and 222) and WC (101,110,002,102,201 service. The purpose of this project is to and 112) peaks were also made. The + investigate the nature of this broadening strains for the a- and e-directions in WC using neutron diffraction and finite were compressive for each sample, as - element modeling (FEM) methods. expected considering the relative thermal . expansion coeflicients of WC and Ni. _ l Preliminary FEM results indicate that the Within experimental error, the magnitude , angularity of the WC particles and their of the compressive strain in each direction' distribution and interaction have a strong decreased as the WC volume fraction effect on the stress distribution and increased. The a-strain exceeded the c-magnitude. FEM models are being strain in each sample as predicted by i developed to match previous neutron analytical and FEM models. 59 1 o
The lattice parameters for Ni increased with -distribution increases with strain ;
. increasing WC. They are influenced by both magnitude, and there is also an increase in -
the stress in the Ni phase and W in solid . WC peak breadth for the 11,20,' and 40 V% - solution. Preliminary calculations indicate - sampics.- Micrographs show an increase in - that for 8 atomic percent dissolved W, the - particle interaction as V% increa~ses. FEM ~! volume-averaged strains in the Ni phase of models ofisolated WC particles show the l all composites are tensile and increase with particles to only be in compression, , WC. These results are consistent with whereas WC-Ni models involving _ analytical and FEM models, and previous interacting WC particles reveal substantiar ] neutron diffraction measurements. The stress distribution in this phase, reaching volume fractions of WC and Ni calculated by into the tensile region. Such a distribut on j i GSAS for each sample were in good - would contribute to the peak breadths. agreement (differing by a maximum of 0.32 The mean free paths of the Ni of the 40 '! V%) with those determined from density and 60 V% samples are clo'se, suggesting i measurements. that the trend ofincreasing strain distribution with increasing strain ! Ni peak breadth increased with increasing magnitude dominates the influence of 'l
.WC content,in agreement with FEM particle interaction for composites of calculations which show that binder strain higher WC content. i r
9 e i I t h l
-?
d t b 60 ;
MAGNETIC AND ' CRYSTAL STRUCTURES GROUP William B. Yelon, Group Leader (Adjunct Professor of Physics) J Ronald R..-Berliner, Senior Research Scientist (Adjunct Associate Professor of Physics and Adjunct Associate Professor of Electrical Engineering) Fred K. Ross, Senior Research Scientist (Adjunct Professor, Chemistry) Elmer O. Schlemper, Senior Research Investigator (MURR) and Chair and Professor of MU Chemistry Mihai Popovici, Visiting Research Scientist (since September 1991) Olivier Isnard, (Visiting) Research Specialist (since June 1992) During the past year, this group has a double crystal monochromator in 3 concentrated on research with and antiparallel configuration can give about the position sensitive detector large intensity gains while preserving (PSD) diffractometer, and with the resolution. A proposal to DOE to eingle crystal diffractometer on develop these methods has been ~ beamport E. In addition, design work prepared. on the new single crystal diffractometer ' (sharingbeamport A with TRIAX)has Research with the -PSD has continued. concentrated in three areas: hard , magnet materials, including nitrided , The most exciting results have involved phases; hydrogen (deuterium) in . the development ofbent perfect crystal Nd2Fe14B and Ti based alloys and techniques. In place of a conventional high Tc superconductora. Research in mosaic monochromator, an elastically the first area produced ine Physical bent perfect Si crystal has been put Review Letter and an in rited talk at , into use at the PSD diffractometer. the Intermag Conferenc i (St. L,ouis, _ Although the effective mosaic of this April 13-16,1992), whih the second crystal is about a factor of 10 smaller area featured the exch inge visit of than for the Cu crystal perviously in Olivier Isnard from .1: CNRS e use, it is used without collimation and Grenoble, to carry out measurements i thus receives a much higher indicent previously scheduled for the ILL and i flux. This factor, plus the use of an no longer possible there due to the asymmetric geometry, leads to a net outage ofthe reactor. The high Tc area gain in flux on sample. The choice of hasseenworkonboth 1-2-3 compounds - radius ofcurvature leads to phase space and BISCO related phases. focussing effects and to better resolution than with mosaic crystals Single crystal diffraction studies and collimation. This success has led included cis [Co(en),(NO,),1NO 2, to the consideration of these methods MgHPO3 16H2 0, NaH 3(PO 3)2 and t to other facilities including the new YBa2 Cu3 )u. The analyses on all of single crystal diffractometer, for which these are in progress. l 61 i i
d i. m BENT PERFECT CRYSTAL MONOCHROMATORS ON THE PSD !! HIGH RESOLUTION NEUTRON DIFFRACTOMETER M. Popovici, W.B. Yelon and R Berliner (MURR) Two bent perfect crystal monochromators and computed linewidths for two cases, the were succesively implemented at MURR on 1/8" diameter Ni specimen and a large plate the high resolution powder diffractometer . Al specimen 1/8" thick, oriented to optimize with position sensitive detection. Large- the resolution at high angle. diameter silicon plates were bent in pneumatic devices in which vacuum or air . A second Si monochromator was pressure was used to produce spherical subsequently installed in this instrument. curvatures by pressing the crystals against The crystal plate was cut obliquely from a 0-ring surfaces. The curvature was 1100] ingot to give a'more pronounced beam controlled either by the pressure differential condensation efTect for the (511) planes.' The or by a spherical mechanical limit. crystal was 6 mm thick and curved by a 90 - psi pressure to a radius of14 m. The The old configuration of the instrument used resolution at high angle was preserved and a 15'in-pile collimation and a Cu (331) there was a notable improvement in both monochromator. The in-pile collimation was resolution and background at low angle, as removed and the Cu monochromator was well as a further gain of 2.5 in peak replaced by an elastically bent Si plate 3 intensities. This configuration is close to the mm thick, set in reflection best achievable with clastic bending and is from (511) planes. The plate had a 1100] orientation and m ' ' ' ' ' ' ' ' ' thus the reflection geometry Monochromator: curved (6 m) 3 mm SI (511) at 90' take-off was asymmetric. Data for No Sollers _ two specimens were 7 compared in detaih an annealed Ni sample,1/8" {
- Al plate sample 2x4".1/8" thkA eom . 44' inclination _
diameter and 2" high, and a i standard A1,0, specimen 1/4" [
- diameter and 2" high, which goso- -
we use for instrument g o calibration. With the Cu 5 Standard Ni sample (1/8" dia) monochromator the reso- om lution was reasonably good, but a noticeable 1/2 ao contamination was present. o.o A A A
- Detbor ankie 2dta, degrees With the sdicon monochro-Fig.1 Bent perfect monochromator on MURR PSD, plate vs, cylineirical sample mator, an improvement in resolution, despite the somewhat shorter wavelength, was expected to be our normal one for the apparent for both samples, with no 1/2 immediate future. At the present time, peaks. Normalized for equivalent counting however, the monochromator is used with a times, the Ni peaks at high angle were 50% (331) reflection for residual stress higher with the silicon monochromator than measurements and for structure with the copper. determinations of magnetic materials. The larger wavelength puts close to 90 the The computations were found to give a fairly diffraction line (211) convenient for stress good description of the measurements. As determinations in steels, and allows better an example, Figure 1 shows experimental separation of the crowded lines with 62
o significant magnetic information in the This would give an additional intensity gain materials unda study. Thia illustrates a of almost two on the existing diffractometer, useful option available, that of choosing The mechanics of such a system are, _. from more than one plane of a given crystal. however, more compler and development of ideas are underway. Thicker crystals could A relatively straightforward extension of be used, with an intensity gain proportional this case would use elastic bending in the to thickness and little resolution loss, if they horizontal plane and pseudo-bending in the could be bent to the necessary radii. Thick vertical plane to create a polygonal - silicon, however, cannot clastically support approximation to a curvature for strong such radii and the current system is close to' , ' vertical focusing (radius of 1.25 m needed). the breaking limit. NEUTRON POWDER DIFFRACTION STUDIES OF MAGNETICALLY HARD PHASES f W.B. Yelon, H. Xie (MURR), G.J. Long, O.A. Pringle, W.J. James (UMR Physics), KH.J. Buschow (Philips, Eindhoven), F. Grandjean (University of Liege, Belgium), G.C. Hadjipanayis (University of Delaware), D.J. Sellmyer, S. Jaswal (University of Nebraska), O. Isnard, D. Fruchart (CNRS, Grenoble), F. Pourarian (Cent ral Methodist University) The largest use of the high resolution The substitutional systems R, Fey,T, powder diffractometer has been for (T=Al,Si) have been studied. Both systems research in magnetism. This has been show enhanced Curie points compared to the an interest area at MURR for the past pure Fe compound and our research has 16 years and our excellent facility and ,,,, ; expertise has led to a growing circle of interactia s. There is a continuing =< interest in new Fe based compounds E with Curie points comparable to j ~~ Nd,FeuB. These include nitrides of rare g- g j;",ll;' a =' ~ ~ earth (R) compounds R,Fe,, and RFe,,,T, , a (T= transition metal), substituted R,Fe n } ~~ compounds and others. ,,,.. 7 Reasearch on the nitrides has revealed ... ,;. ,;. ,;. ,;, .. the h> cation of the 1,itrogen atoms in the cuiu rosin m crystal structures.u In all cases the N Fig.1 Curie point versus average Fe-Fe bond atoms are found only in the single length in Fe nch Nd based compounds largest interstitial site, and the occupancy can be varied from 0 to about 907c full. The lattice expansion depends focussed on the origin of this effect. It is upon the occupancy as do the magnetic found that the Al compounds show strong properties. Band structure calculations latuce expansion while the Al shows a carried outin relation to the NPD d'.minished preference for the c-site, the one measurements suggests that the most strongly connected with good magnetic dominant effect is the change in band properties (Figure 2). These two effects structure with Fe-Fe distance and not overcome the cir ect of Fe dilution. On the
- any effect of electron transfer with the N other hand, the efTect of Si is more I' atoms. For a given rare earth (e.g., Nd), mysterious; the lettice does not expand and ,
it is found that the Curie point increases the site preferenet effcets do not clearly (perhaps linearly) with average Fe-Fe provide an explana'. ion for the enhancement. bond length (Figure 1). Furt.her studies of substitutional compounds 63 i-
are underway and may provide insight into ' ' ' ' ' ' ' ' ' ' - this problem and lead to the development of y" " better materials. o o,g _ _ The effect of D in Nd,FenB has been y 0.6 -
, a studied as well. Samples prepared in _
.* 8,' ,
f
- ish -
{04 */'-
~
France with D content varying from 0-4/f.u.
~
are being studied between 10K and room ] temperature in order to determine both the 50.2 o I l D site occupancy, thermal motion and the ' oo _
'e ; ; ; ;u .
changes in magnetic moments with ' ' ' ' ' ' ' ' ' < > ' concentration and temperature. These o 2 4 6 a 10 12
]
sample are unique in being well Aluminum Content, x ! crystallized, single phase specimens and Fig. 2 Frachonal occupancy of Al on the four Fe sites the final results of the study should be in Nd,Fe,3Al, quite intoresting and definitive. The analysis of these data are being performed I. S.S. Jaswal, W.B. Yelon, G.C. using a Rietveld code brought from the ILL Hadjipanayis, Y.Z. Wang and D.J. which allows magnetic refine ment of Sellmyer, Phys. Rev. Letters 67,644 multiphase samples. While less user (1991).
- friendly than the GSAS program,it should 2. W.B. Yelon and G.C. Iladjipanayis,IEE be a useful addition to our library. Trans on M rgn. (in press).
References i NEUTRON MICROFOCUSING BY DOUBLE REFLECTION ON CURVED PERFECT CRYSTALS M. Popovici and W.B. Yelon (MURR) Double crystal monochromators with two returned to the neutron case in a recent identical flat crystals in parallel (+,-) setting paper' for an examination similar to that are quite common, both for neutrons and presented for SR.3 synchrotron radiation (SR). The parallel setting is known to be non-dispersive: all For a neutron double monochromator radiation diffracted by the first crystal, required to image the source at the sample regardless of wavelength, automatically has position, the design relations were derived the right conditions to be diffracted by the by accounting for the condition of efficient second one. An equivalent of this setting double difTraction in the facusing equations. exists too for diffraction from two bent The configuration with the strongest crystals. The neutron results on the optics demagnification appears indeed to be that of diffraction by two bent crystals' were with crystals in antiparallel (+,+) setting. particularized to the point-source SR case.28 The instrument resolution can be adjusted Computations for the SR case have shown to put the minimum of the difTraction that for curved crystals, the distinction linewidths at a desired position. The small between parallel (.+,-) and antiparallel (+,+) radii of curvature necessary for ; configurations is no longer relevant from the microfocusing can be achieved with plastic intensity point of view. An essential bending techniques only. The peak , di!Terence, however, is that the full beam reflectivity decrease on bending then intensity can be easily condensed into a becomes importzmt. This restrirts the choice narrow fbeus in the antiparallel setting. We of useful planes to strongly reflecting ones. ; G4
- 3
, 1 . , _ _ _ . h J
.' l
.i As an example, a microfocusing double - curvature should be set quite accurately,- ;
monochromator for stress scanning has been 'with a precision of about 21 The considered. In such measurements the dependence of the powder diffraction . - strain is probed by recording a diffraction . linewidths on the detector angle is shown in j line in the vicinity of 90* for a sample. Figure 2 both for the single Si(511) a volume limited (by beam-defining slits) to monochromator and the double Ge (400). In' . 1
- several cubic millimeters. Computed data the microfocusing case the lines broaden -'
on a configuration meeting the requirement considerably on going away from 90*. At [ of narrow diffraction lines in the vicinity of minimum, the linewidths are still worse- 1 90* are shown in Figures 1 and 2. The than in the single monochromator case. j distances from source to first crystal and - However,in a limited range around 90*, between crystals were fixed to the actual there is a large intensity gain from spatial , values for a MURR beamport where a stress focusing (factor of about 15) that more than ! instrument is to be installed. The instru- compensates for the broader linewidths. ment is being designed to have a single, The lin'ewidths in Figure 2 were computed i clastically bent, Si (511) monochromator in for no sample broadening. When the sample. '[
- breadeningis important, as sometimes _ .,
happens, the intensity gain may approach . .j
- 3. " %. i o. m e - c c airr.
-u- t .u t u aur that of the intensity through sample.
n ,.w .am,,.o. a.,.us . { "' ' " " ' " ~ " ' ' '
$ References 8 "- 1. M. Popovici, A.D. Stoica, B. Chalupa and j P. Mikula, J. Appl. Cryst. 21,258-265 f n-
# ,, . (1988).
l 2. M. Popovici and W.B. Yelon, J. Appl. , o "' Cryst. 25,471-476 (1992). .
- o. 3. M. Popovici and W.B. Yelon, Nucl. Instr. l Meth. A319,141-148(1992). .
"a =
= ,*ll;,, gag,%,44 = = =
- 4. M. Popovici and W.B. Yelon, Proc. Int. !
Symp. " Neutron Optical Devices and j Fig.1 Intensity through sample (3x3 rnm area) vs. second crystal curvature for a double APPlicatione," San Diego, July 1992, j rnonochromator with plasticaHy bent Go (400) SPIE,in press. - crystals in antiparallel setting (thermal source
'?
flux 10" niem'/sec). strongly asymmetric reflection. For the double monochromator, plastically bent Ge '"~
**7 ["_* r i
(400) crystals in symmetric reflection were considered. Vertically, the first crystal was fg*' . M ca m'=' m=*=a**
-[
l taken to be flat and the second crystal 4 l optimally curved. ( "- k i The computed minimal beam widths are f"- j below 6 mm in the diffraction plane and I ! t cm in the vertical plane. The neutron a- s ,.sq3m ...a. a . , miensity through a 3x3 mm sample (source l flux 10" n/cm 2/s)is shown in Figure 1 as a ", 4 & 4 ,;, 4 4 4 5 . D=**'*******'*") function of the second crystal horizontal '! curvature.' At maximum,it is 34 times Fig. 2 Neutron powder diffraction knewidths vs. detector ' hrger than that computed for the elastically angie for the configuration considered in rigure 1 and " bent Si (511) monochromator. The radii of - for an etasucesy bent singie si (511) monochromator. i A. .j 65 - t I
DETERMINATION OF REFLECTIVITY CURVES OF MULTILAYER NEUTRON ' MONOCHROMATORS M. Popovici, B.J. Heuser, W.B. Yelon (MURR) and J.E. Keem (Ovonic Synthetic Materials Co.) i To anticipate the performance of a syr.thetic curvature of several tens of meters and i multilayer monochromatorin a SANS lateral variations in layer spacing of the j instrument under construction at MURR, order of I'ncm 8 were found in all cases. i four Ovonics Ni-Ti multilayers deposited on Consideration of their effects turned out to a Si 1100] thin wafers were investigated. Two be essential in understanding observed ! of the multilayers had 60 Ni-Ti bilayers with rocking curves. I 10 nm nominal spacing; the other two had -i 30 bilayers with 9 nm spacing. The Figure I shows the results of diagnostic measurements were made on the MURR 3- measurements for a 30-layer along one of ' axis neutron spectrometer by rocking the the 1110] directions of the support wafer. multile.yers against the Si (Ill) The changing slopes of the variation of the - monochromator. transmission rocking curve position on ' translating the multilayer give correspond-The initial results were confusing; ing changes in the rocking curve peak and . ' conventional rocking curves appeared to width values. Minimal widths and best depend on whether the face (deposition side) peak values were expected to ccrrespond to.. or the back of the multilayer was measured some optimal slopes (shown in Figure 1) and and on the port. ion ofits surface that was this did indeed happen, as seen in Figure 2. exposed to the beam. The multilayers turned out to be curved (convex), due to deposition-induced stresses. Further checks
"~
indicated that the layer spacing was also ;[ non-uniform over the surface. It became - 1 i-- %, clear that the conventional technique of I measuring and interpreting double crystal 8+ ,. rocking curves should be adapted to the E ,, peculiarities of synthetic crystals: due to f o.; # the shallow Bragg angles the separation of 3 the incident and reflected beams is small; the multilayers may be curved and, unlike j' ,_ %% "" _
~
__ j g;;;L natural crystals, may have d-spacing non-' .. uniformity. " ' A Ja A
- The most convenient measurement Fig.1 Variation of the Bragg angle scale dip position of the transtrussion rocking curve on translating configuration was found 1.o be that with a 30-tayer parallot to its large flat (L.F).
tight collimation in front of a narrow detector and with meaauring the neutrons transmitted through the multilayer. The measured rocking curves showed some Formulae for the interpretation of such structure between the total reflection range rocking curves were derived, multilayer and the outer dips due to Bragg reflection i curvature and lateral gradient oflayer for the nominal d-spacing, indicating that - spacing accounted for. The radii of the Fourier transform of the multilayer curvature R and the lateral gradients g were contrast distribution is difTerent from zero determined by scanning the multilayer not only in the proper Bragg range. Data , surfaces. By measuring the reflection fmm obtained under difTerent conditions showed 'l
- the face and back of the multilayers, R and g that the correction procedures were could be determined separately. Radii of adequate and gave consistent reflectivity
?
66 # f
parameters. The observed peak reflectivities w were 80% for 30-layers and 94% for 60- smmuw = , layers. No real discrepancies were noticed I anwm mam ' between measured and theoretical widths l "' w ww _ (~0.8 mrad).- t , I u- - A detailed account of this work will be - presented at the International Symposium
- Neutron Optical Devices and Applications," ,
[ s San Diego, July 1992. i u- Face sadi d Fig. 2 Vanation of the depth of the rocking curve dip ", , , , , p , on translation H to LF (same multilayer). Pava.kugmage aM DESIGN COMPUTATIONS FOR SYNCHROTRON RADIATION CURVED TWO-CRYSTAL l MONOCHROMATORS M. Popovici and W.B. Yelon (MURR) The design of curved two-crystal An automatic generation of those monochromators for synchrotron radiation parameters will have to be implemented to , (SR) has been considered in two papers'2 make the program suitable for general use starting from earlier neutron optics in SR computations. results.aBoth for neutrons and SR, one can . ensure that all the radiation difTracted by The heat load problem _ In flat SR double the first crystal automatically have the right monochromators, there is a loss of intensity , conditions to be diffracted by the second one. as the flat second crystal nolonger For this to happen, one has to choose the efliciently diffracts the beam given by the right curvature for the second crystal in the thermally distorted first crystal. Our SR case, and the right curvature and the . computations referred to the monochro-right reticular spacing in the neutron case. mator on the A, beamline at the Cornell-The difTerence is due to the fact that in the High Energy Synchrotron Source (CHESS) diffraction plane an SR source is sharp while for which the heat load e(Tects are well'
- a neutron source is usually wide. documented. Figure 1 shows the rocking :
curve width and peak intensity vs. the , The first paper discussed the problem of second crystal curvature R, for two radii of_ , overcoming the heat load problem in SR curvature of the first crystal, It is san that double monochromators by suitably curving by curving the second crystal to the right the second crystal to accommodate the radius, the rocking curve width is curvature of the thermally distorted first practically restored to its flat-crystal value. ' crystal. The second paper discussed also the The peak intensities are slightly higher possibilities of achieving large demagni- than two flat crystals, due to the reflectivity : fications. Results of computations with a increase on curving. For a heat load ten neutron optics program adapted to the SR times higher, computations showed that the , specifics were presented in both papers. The . lattice spacing gradient in curved crystals j adaptation consisted merely of working with no longer allows the rocking curve widths to .j appropriate perfect crystal reflectivity be restored to their flat-crystal values, but parameters and with effective crystal the residual broadening is accompanied by thicknesses given by the absorbtion depths. a marked intensity increase. This effect is
.iJ 67
f
> related to the large absorbtion depth of. It is seen that the setting of crystal ;
silicon (about 100 microns at 20 kev) and for. curvatures should be very precise and the j
- germanium it is virtually absent. This' focus is expected to be very sharp (5'pm). In . ;
makes silicon double monochromators . contrast to the situation for flat crystals, in -i superior to' germanium ones at high the (+,+) configuration the full beam energies and high heat loads. intensity is higher than for two crystals in - , u parallel (+,-) 7;osition The beam flux - i
. c. # 2-crystat si(111) . (number of quanta per unit area) at focus is " l 3 expected to be larger than in the present s -
E = 20 kev 8 tC 4 configuration by a factor of about 1000J A h further enhancement by a factor of 100 is ' 1 "' possible through saggital focusmg. N 02-
- j. , = .233 m R, = -113 m gg j8'd N 1. M. Popovici and W.B. Yelon, J. Appl.' ;
it u._ . Cryst. 25,471 (1992). ;
- 2. M. Popovici and W.B. Yelon, Nucl.
,j l z instrum. Meth. Phys. Res. A319,141 j / (1992).
j 25 - 2-crystai si o t1) 3. M. Popovici, A.D. Stoica, B. Chalupa and , P. Mikula, J. Appl. Cryst. 21,258(1988). g j E = 20 kov . E' '" [ 1 % so. w-35 l L, = 1450 cm. L - 37 cm. L, = 14.3 cm
-233 m . .
, --113 m m 00 O.C 0.002 0 004 0.036 0 008
. d ** '
0 010 0 012 r (+,+). E = 20 kev Second crystal curvature 1/R,(1/m) g x, First Si, R, = 1.83 m - E po, Fig.1 Computed dependence of the rocking curve I 8' m'
- widths and peak intensit;es on the second crystal curvature R, for the geometry of the oo , _ . _ ,
CHESS A,beamhne. The radii of curvature of .W7
^
the firt.t crystal correspond rer.pectively to the galbumtooled (-233 m) and water-cooled (-113 h .(+,+). E = 20 kev f tro' First si, R.1 = 1.83 m m) Si (111) doubie monochromators set to 20 - kev at a power load of about 0 4 W/mme f, Second Ge - . q o.7s ~ 4
' Microfocusing With identical crystals in j ' '
- antiparallel symmetric reflection, large [ "' ,
demagnifications can be obtained just by E
' *' ' ' 7 ""# " ' ' # '*
correctly choosing the distance between the two crystals. Computational results are
- l " 8
'; ~
u . .
- shown in Figure 2 referring to a possible ""**'d' cod' M g ,'fjdd*p$ "" "*' _
{ optimal configuration for microfocusing on , the same CHESS A, beamline with a mixed Fig. 2 Computed beam intensity and width at focus for . l[ Si+Ge monochromator (the smaller a possible configuration with strong image . . 5 demagnification on the same geometry. using a l absorptw.n depth ofgermanium gives a first Si and a second Go (111) curved crystals of ' lower aberration due to beam penetration). optimal curvatures. . r !- f t 68 i 1 ,
J NANOSTRUCTURES. ANDl EXCITATIONS GROUP' l James J. Rhyne, Group Leader (Professor of Physics) - Brent J. Heuser, Research Scientist i Kenneth W. Herwig, Research Associate 1 Haskell Taub, Senior Research Investigator (MURR) and Professor of - Physics i David L. Worcester, Senior Research Investigator (MURR) and Associate Professor of Biological Sciences The research work of this group is primarily focused toward disordered ; (amorphous or crystalline) materials and materials with a substructure of order 10 or more lattice spacings. The group in concert with other groups in the Neutron Materials Science Program has the responsibility for_ the development of the new 15m Small Angle Scattering spectrometer (SANS) and also for the redesign and upgrade of the Ames Triple Axis spectrometer (TRIAX)in a collaborative effort with C. Stassis and A. Goldman from the Ames Laboratory of Iowa State University. Both the SANS and TRIAX programs are the recipient of Instrument Development Grants from the : National Science Foundation for construction of these state of the art instruments. The SANS is funded under NSF grant DMR-8915199 in the amount of $395,000 (including MU match amount) and the TRIAX under NSF grant DMR-9103383 in the amount of $419,000 (including UM, MU and ; Ames Laboratory matching amounts). t 7 I o f W 69 I
PHYSISORBED MONOLAYERS'
' K.W. Herwig (MURR and MU Physics), P. Dai, S. Wu, B. Matthies (MU Physics) and H. Taub (MU Physics and MURR)
Our investigations have focused on the monolayers while suggesting a general . question of how the steric pmperties of a melting mechanism in monolayers of flexible, - molecule influence its behavior when rod-shaped molecules. In both cases, melting ' physisorbed onto a solid substrate. The requires the formation of vacancies in the film physical size, shape, and flexibility of a by motion of the molecule perpendicular to molecule can play a definite rolein the substrate. In butane, this occurs by - determining such properties as the melting tilting of the molecule, lifting one end slightly behavior of a monolayer film' and the growth off the surface, to create the required excess mode of multilayer films. This issue poses a area. For the longer hexane molecule it , problem of considerable interest in surface appears that this excess area is created by a J science and impacts on such basic areas as the conformational change of the molecule which .) theory of wetting as well as technological reduces the size ofits footprint on the problems related to lubrication and adhesion.- surface. l
\
We have sought to address this problem by We have employed quasielestic neutron i investigating the behavior of a series of scattering (QNS) to pmbe the dynamical _l isostructural md-shaped molecules, the n- behavior of these two molecules adsorbed on alkanes (C,H,,,), physisorbed on graphite. graphite t,th above and below the melting Our goal has been to determine the efTect of temperature. These experiments have been the molecule length (n) on the monolayer carried out on the QENS spectrometer at melting behavior and the wetting properties of Argonne Natior il Laboratory's Intense ~y multilayer films. In the following, we describe Pulsed Neutron Surce. In summer 1992 we - two experiments each designed to address one were allocated 90 weeks of beam time which of these issues. we used to cor'inue earlier experiments. Our goal was to rr urn with a complete (in the sense ofcov 'mg a broad range of Quastelastic scattering from hexane physisorbed temperatures and momentum transfers) set on graphite Elastic neutron difTraction of data for a near monolayer coverage of i studies have demonstrated that the melting hexane on graphite. transition in the n-alkanes physisorbed on graphite difTers greatly among representative Typical spectra in QNS contain an elastic molecules although they have similar solid component whose strength is related to the ' monolayer structures? The first three fraction of molecules which, on the time scale members of the series with an even number of set by the instrumental resolution and length 1 carbon atoms (ethane, butane, and hexane) scale set by the momentum transfer, are have a herringbone structure in their solid static. The second component is typically submonolayer phase, with a melting assumed to be Lorentzian in shape, with a temperature which increases monotonically Doppler bmadened width associated with the with molecule length. However, the butane diffusive behavior, either rotational or monolayer exhibits an abrupt, first-order translational, of the molecule. melting, while the hexane monolayer retains a large degree of f ranslational order ever, at Figure 1 shows the widths of this Lorentzian room temperature. component for both hexane and butane as a ; function of reduced temperature. T,, which is Molecular dynamics simulationsu have given the sample temperature divided by its welcome insight into the differences in the melting temperature, T,. To within 10 K of melting behm-ior of these two alkane T y, physisorbed butane exhibits no observable , i 70 4
b q i quasielastic scattering on either of the two length The multilayer growth of butane on graphite scales defmed by the momentum transfers of ;- ' In the past year, our measurements using : Figures 1(a) and (b). In contrast, hexane clearly the C-port diffractometer have focused on the exhibits quasielastic scattering at temperatures - layer-by-layer growth of butane on graphite.- well below T,. Previnus diffraction studies2demonstrated ' that butane forms a herringbone structure 600.
; with a unit cell similar to the (011) plane of ;
; bulk butane (the largest lattice spacing - l (a) ! mismatch is approximately 5%). Because of-i this similarity to the bulk solid, we believed 6 499' 9 j butane was a likely candidate for growing .
j j ,a crystalline m dtilayer films on graphite. 200.- j ~ During the course of our experiment, we f "" .
- collected approximately 100 data sets, .;
e'.'
~
covering a range of temperatures from 11 to 00 =, , , i : l . , 138 K, and a range ofcoverages,0, 0.00.2 0.4 0.6 0.8 1.0 12 1.4 1.6 corresponding to the material required to form 0.9 to 6.0 monblayers (ML). The large 1000.
' ' ' ' u ' ' "backgmund" associated with the substrate i .l' and the relatively weak signal from the 800.- (b) }. - adsorbed molecules required long experi-j ," mental runs in order to obtain good sta.tistics ,
^
9 600.- - in the difference data. Approximately two_
% !. days of beam time were required to obtain a -
[ 400. - ,,j - good diffraction pattern at the lower coverages. 200 - !. . * - i Figure 2 shows the low temperature,11 K, 0.0 =, , data for all the coverages studied. , 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 Diffraction peaks associated with the IR monolayer are observed as part of the . Fig.1 The HWHM. G, of the Lorentzian component in diffraction pattern at all coverages studied, the quasielastic spectra of butane (filled circles) indicating the continued presence of only one and hexane (ftlied squares) physisorbed on layer of crystalline film on the graphite
$ h n$te EgIe pe alurein surface. The stmng diffraction peaks which both plots. Pbt (a) shows the data collected at a cont.inuously increase in strength are . {
momentum transfer O of 12 A' white plot (b) associated with the growth ofbulk shows the data for o - 2.s A '. crystallites. Analysis of this data indicates that bulk crystallites begin to grow when O These data a e er.tirely consistent with the exceeds 1.8 ML. diffraction data which demonstrated that melting in butane occurs in an abrupt first-order manner Contrary to our expectations, it appears that while the melting behavior in hexane occurs over a herringbone monolayer forms a poor a much broader temperature range. The source of template for epitaxial growth of crystalline , the quasiclastic scattering observed in hexane overlayers. The reason for this may be that below meltir.g remains a question to be answered in bulk butane substantial tilting (greater by the computer simulation. A likely candidate is than 11 deg) of the molecules occurs relative i the conformational change of hexane predicted by to the (011) plane while butane lies flat on the simulation to occur prior to melting of the the graphite substrate. This difliculty of . monolayer. A more complete interpretation accommodating to the molecular orientation awaits calculation of the intermediate scattering in the monolayer may be a critical factor in functions from the simulation results. achieving multilayer growth. 71 ,
-t
- i The intensity of the difTuse scattering in . interpreted'as evidence for molecules in a second regiors where no Bragg peaks from either the layer, stabilizing the first layer so as to raise its film or the bulk crystallites are present mey melting temperature? These molecules must be -
be associated with the amount of disordered disordered with respect to molecules in the first > material present in the sample cell., This layer as they do not affect the monolayer intensity clearly starts to increase when O diffraction pattern. exceeds 1 ML. This observation indicates that some disordered material is present in The melting temperature was determined at two the film at the onset of bulk growth (at O = coverages, O = 2.2 and 3.1 ML. ~ All the 1.8 ML), and the amount continues to difTraction peaks, including those associated . increase dunng bulk growth. with the bulk crystallites, vanish at a temperature between 128 and 133 K,less than - Analysis of the temperature dependence of the melting temperature of bulk butane,135 K. ' the diffraction pattern at O = 2.2 ML The difTraction peaks are replaced by very bmad demonstrates that the monolayer component features consistent with a liquid film. ' This persists to 128 K,12 K above its melting behavior indicates that, at least up to O = 3.1' temperatum at O = 1 ML. This effect can be ML, butane forms relatively thick liquid films on graphite although only a single crystalline layer 3.0
' . . may be gmwn.
;j; .
2.8 - !! Ij ! In summary, we have demonstrated that butane = 2F !l jl: l - forms only a single crystalline layer when jj ; l physisorbed on graphite. There is considerable 2.4 - ii. 'i l , evidence in our data that molecules are b 7I j.
- 6.0 ML randomly distributed in a second layer before 22- r [j
~
bulk crystallites begin to form. The presence of
;" this amorphous second layer increases the y' 'E 2.0 - 4 . :
y : i' f 5.2 ut melting temperature of the crystalline first - 3 1.s -
-e a: i
)
i Jj
@ layer. The amount of disordered material in the film continues to increase during bulk growth.
8 16- ! ! i'; 1 - Finally, there appears to be a wetting transition I M 3,4_ , _ near (but below) the bulk melting temperature ' , 25 : i ji; i where butane is able to form thick liquid films ; y t2- ! : i' ' 2.2 ML on graphite. . b 1'0-This work has been funded by NSF grant DMR- !
! ! !!i i os- y : l 1.9 ML 9011069 since September 1990 in the amount of .
. i ;j : { $258,000,-
0.6 - ! i i :
. j,$ yt ,
0# 8 j pt
;,i References
- 1. F.Y. If ansen and II. Taub, Phys. Rev. Lett. 69, 02 : ::: '
652 (1992).
- k. jih _* R~ 2. H. Taub, in The Time Domain in Surface and 00 ' '
D.75 1 I5 ' ' 2' .I5,3 &'.I5' 4 IS Structuml Dynamics, edited by G.J. Long and . F. Grandjean, Kluwer, Dordrecht, NATO I OM) Advanced Study Institute Series, Ser. C,228, - . Fig. 2 Elastic neutron diffraction data from butane 467(1988). , adsorbed on graphite. The background signal 3. J.C. Newton, PhD thesis, University of 1 due to the bare grapNte and aluminum sample Missouri-Columbia (1989, unpublished). cell has been subtracted. and data have been 4. F.Y. Hansen and H. Taub,in Phase suppressed in regions of strong substrate Tmnsitions at Surfaces 2, edited by H. Taub, scanenng. The data points have been connected for cladty. Dashed lines indicate the location of G. Torzo, H.J. Lauter, and S.C. Fain Jr,' the diffraction peaks associated with the Plenum, New York, NATO Advanced Study monolayer film. Inctitute, Ser,C, 267,153(1991). 72 , l{ 4, u
p.- ..-gg SMALL ANGLE NEUTRON SCATTERING STUDY OF ELECTROCHEMsCALLY ETCHED ,
- SILICON' ,
B.J. Heuser, W.B. Yelon (MURR), M. Boley (MU Physics), S. Spooner (Oak Ridge National Laboratory), C.J. Glinka (National Institute of Science and Technobgy), A. Yelon (Ecole . Polytechnique, Montreal), and V. Petrova-Koch (Technische Unive'esitat Munchen, Germany) , The discovery of a form of Si with a evident from visual inspection with a - photoluminescence efficiency much higher microscope that this layer had cracked and than bulk Si has led to a flurry of research partially pseled off the underlying material. activity. This unusual form of Si is created Other resarchers have attributed this effect during electrochemical etching of oriented Jd single crystal Siin hydroflouric acid under a variety of conditions. The resultant ** material is very porous and often appears red in color. Small-angle neutron scattering - (SANS) measurements of four electro- 3*
~
,\
chemically etched, porous silicon (PS) j "N .s , samples have been performed. The y'; \
= 5 L
photoemission spectrum of each sample was 3
~
obtained as well. P '
'N The SANS responses of the four PS samples a
q are shown in Figure 1. The scattering = = a =+ c
- curves overlap and have been separated for 4 .u 4 .u 4 o a 4 .. . .u !
clarity. [ Time constraints limited the monw , measured range of scattering angles for the Fig.1 SANS response of PS samples. Sohd lines G1 and G3 samples.] The SANS data can be represent best fit of data with Eq.1 and power law. Individual data sets have been separated for modeled with a non-particulate, random ciag phase model2 over intermediate scattering angles range. The functional form of this to post-etching, evaporation-induced scattering behavior is given by stresses 8 The two curves for the M1 sample .; are before and after removal of this top ! _.b (Q, L) = 8n(rl') (1) layer. A check of the vertical uniformity of - dQ (1 + Q2L2)2 this sample is then facilitated by a comparison of the two measurements, where L is the correlation length scale of the random, inhomogeneous structures withir. TABLE 1 Random phase correlation the scattering system and c12> is the me'in length scales and power law square scattering length density fluctuation exponents for PS samples .t averaged over all points within the scattering system. The low scattering ingle Sample L n response of M1 and G2 follows a powe t law ID* [nm] behavior dTjdf1-Q", where Q is neutran - wavevector transfer. The parameters M1 before 1.0 -3.5 0.1 ; I 1 aner -3.3 1 0.2 obtained from fitting the data in Fir,ure 1 , g are presented in Table 1. l G2 0.9 -2.0 0.1 G3 1.7 An important physical characteristic of the -- M1 deserves discussion. The top layer of
- Before and after measurements are before this particular sample material was weakly and after removal of weakly bound top layer.
bound to the underlying PS layer. It was g , 73 t 4-r
I i i In general, the M1 curves are similar; the The photoluminescence spectra for all correlation lengths and pcwer law exponents samples are shown in Figure 3. The are equal to within experimental ermr. . ' asymmetric peak shapes from the M1 and
. Notice, however, that the plateau and shoulder G2 samples are due, at least in 'pa-t, to the are more pronounced in the M1 "afler removal" detection system efficiency goirel to zero at curve. The observed shouldering can be 930 nm; Notice the marked similarity interpreted as an interference effect between between the M1 and G2 spectra, and the scattering centers that make up the PS dissimilarity between these two spectra and material.8 Given this explanation, the those obtained from G1 and G3. Correla-enhanced shouldering after top layer removal tions between SANS determined structural ,
suggests that the interference effect is more characteristics and photoemission behavior clearly defined for the underlying PS material. can not be drawn, however, until the G1 and G3 SANS measurements are extended The possibility of microstructural snisotropy in to lower Q. the M1 (top layer removed) and G2 sample . materials was also investigated at low to References : intermediate Q. Figure 2 demonstrates the
- 1) P. Debye, H.R. .hderson, Jr., and H.
effect of tilt.ing the M1 sample 20* about a Brumberger, J. Aspl. Phys. 28,679 vertical axis. The G2 data showed little (1957).-
- 2) L.E. Friedersdorf, P.C. Searson, S.M. 3 1
,,- Prokes, O.J. Glembocki, and J.M.' t
- Macaulay, Bull. Am. Phys. Soc. 37,770 ,
n _ y (1992). : 1 -1 .w 3) P. Goudeau, A. Naudon, G. Bomchil, and a .- R. Herino, J. Appl. Phys. 66,625(1989). ! [24
- , ,3 7 %.::::E"' " S" " ^ * *#*
Horizontal Sector Average - 3 0 ,.
.3 __ m eam.o _ w ,a .
0, 4 \i _% 4 st D
~ -5
\2 D
I 2 6 3.4 -2.5
-2.2 -1.6 -1 -0.4 0.2 0.8 7 --
In Q [1/nm] . d Z_ ( , Fig. 2 Effect of tilting M1 sample (after removal of top
" 11111 * -
layer) 20' about a vertical axis. Microstructural
- anisotropy is evident over length scales ' rom 5 to
*~" *--'"-*
30 nm. - *
--o _. 63 ,
difTerence fmm the M1 measurement and are I~ - 2: not shown. The horizontal and vertical sector 2: Z: -i averages in this figure are averages over pie- 2: Il [ ahaped areas on the detector d-viating115" 2: Z: . from the horizontal and vertical detector L ,&111,41111A h 14.:.A11 n a center-lines, respectively. The no-tilt M1 -i Fig. 3 Phototuminescence measurements measurement, omitted for clarity, bisects the vertical and horizontal sector average curves more or less equally. Based on Figure 2, a certain degree of structural anisotropy does
- Neutron scattering experiments were exist in this PS sample that extends over performed at the Oak Ridge National Laboratory length scales of approximately 5 to 30 nm. It National Center for Small-Angle Scattering i is interesting to note the microstructural Research, Oak Ridge, TN and at the National
{ anisotropy disappears beyond length scales of ' Institute of Standards and Technology Cold i
~30 nm (Q values below 0.1 nm-3). Neutron Research Facility, Gaithersburg, MD. l 74 i
w -- --
s SMALL-ANGLE NEUTRON SCATTERING INVESTIGATION OF DEFORMED SINGLE CRYSTAL Cu* B.J. IIeuser (MURR), J.S. King and G.C. Summerfield (University of Michigan-Ann Arbor) - ' The first set of measuremuits designed to detector shadowed by the beam stop is investigate the SANS response of defects in - included in Figure 1.] The response of the metals were performed in May of 1992. The reference sample is flat over the Q range, goal of these initial experiments was to i idicating the quality of the single crystal ~ resolve disk > cation scattering in deformed rraterial is good. The asymptotic cross ; single crystal Cu. section of the reference sample is ! approximately 50% greater than expected The starting material was a 5N's pure Cu from incoherent scattering from Cn. The , single crystal ingot with a [110] cylinder reason for this is not clear-based on a axis. This ingot was supplied by Metron, measurement of a partially deuterated
- Inc. of Allamuchy, NJ. The four neutron - polystyrene sample in the same instrument scattering samples investigated were configuration, the water calibration is deformed in compression along the [110] correct to within 5%. 1 cyl;nder axis direction to 7%,16%,35%, and +
54% reduction in thickness. An undeformed ., ; , : reference sample cut from the same ingot was measured as well. All samples were c aca mechanically polished, with the final step -425- ***** .,**. using 1 micron alumina powder. " * * . ,' * * . , y ., a c- . .,, .... m Early theoretical work' predicts a Q-3 $d '. [".*.**'.-ha.s
^
scattering response from the 1/r clastic 5 .
."-'*7 $4 *.[
strain field of an edge dislocation. Epperson .u 1 " . *
- M. f.*a,i et at: have observed a Q-3 response in heavily deformed (greater than 95% 5 reduction in thickness) single crystal Cu. it 4 75 4.25 3 75 3 25 -2.75 -2 25.
Figure 1 shows our measured, radially rig. 2 in net dudaN. $o for deformed cu - averaged macroscopic scattering cross section of the four deformed samples and the reference sample. Absolute cross sections Figure 2 shows the radially averaged net were obtained by calibration against 1 mm scattering response (defined as deformed , of water. [ Note that the portion of the sample response-undeformed reference l
- n. 1 a- sample response) of the four deformed [
g3 ,, samples in in-In format. These data exhibit j us- *
- 5'
- c, j a Q22 power law over the entire measure- t
, . sacw i ment range, although the data for the 7% ,
"~ ;[
*, and 16% CW samples are poor. Figures 3
;c "'~
, = cw {
" C' I and 4 show the net scattering cross section i
$ ms - 1, '*. '" , of the 54% CW and 35% CW samples,- ,
m- .;Q "," respectively, with the measurement range .
* ~
2 - - now extending to low Q. ILow Q investi- ' m h;*" gation of the 10% CW and 7% CW sa.nples - l _{ ., j was not adequately performed in this study.] ' These figures demonstrate that the Q-2.2
=
a ur u. m us ei m
. ,,,% power law is maintained to at least Q ~ j Fig.1 dDda vs. O 1or deformed and reference Cu 0.007 A-1.
75 - 1
l l 01- Yde00 . m - y : == g., - 0.01 - e t N O 001 - ,' # 9 0.001 .., 10 ' - '
,0 _ _ .
0.01 e o pd3 0.1 0U ei o rid; 01 Fig. 3 in net dDda vs. In O for 54% CW sample Fig. 4 in not dDdQ vs. In O for 35% CW sample The observed scattering response is not References consistent with the 1/r dislocation strain 1. V. Gerold, G. Kostorz, J. Appl Cryst.11, field response discussed above. One possibic 376 (1978) and references therein. explanation is that an interference between 2. J.E. Epperson, G. Kostorz, C. Ortiz, P. dislocatien cores (which are expected to Furnrohr, and K.W. Gerstenberg, Acta scatter like 1/Q) and the 1/r strain field Metall 27,1363(1979). results in the Q 2 behavior. This seems unlikely, though, because this interference should depend on the degree of cold
- Neutron scattering experiments were working. Furthermore, we would not expect performed at the National Institute of such an interference efTect to dominate over Standards and Technology Cold Neutron the entire measurement range. Research Facility, Gaithersburg, MD.
SMALL-ANGLE NEUTRON SCATTERING INVESTIGATION OF DEUTERIUM TRAPPING AT DISLOCATIONS AND GRAIN BOUNDARIES IN Pd AND Nb* J.S. King, G.C. Summerfield, J. Steinhauer (University Michigan-Ann Arbor), and B.J. Heuser 7 (MURR) As a precursor to measurements performed in vacuum of10-5 torr. Two of the samples, Nb2. i November 1992 at Saclay, France, prototype and Nb3, were loaded with deuterium at 400* samples were measured on the 30 m SANS C to 34,400 and 13,200 atomic ppm, 7 instrument at Oak Ridge National Laboratory. respectively. Sample Nbl was not loaded with : The primary purpose of these measurements deuterium and served as a reference standard. was to ensure that the sample preparation i pmcedures employed were correct. Unfortu- The net absolute differential neutron nately, the majority of the measurements were scattering cross sections (defined as loaded inconclusive because of the poor counting sample cross section minus Nb1 reference , statistics. Three measurements did provide sample cross section) are shown in Figures 1 interesting results and are presented below. and 2. The scattering response is mcdeh d with . a combination of two power law behaviors; Three Nb samples were prepared from poly- dTJda - 1/Q + 1/Qi, where Q is the wavevector i crystalline stock. The samples were deformed transfer variable. The 1/Q component ; by rolling at room temperature to 62% represents deuterium trapping at disk) cations ' 1 reduction in thickness. All the samples were forming md-like scattering structures while the .j then heated to 700* C for 30 minutes in UQ4 component represents a Pomd response i l 76 i I
C L from internal surfaces.' In this case we suspect ^ As discussed below, we generally expect to -
- that surfaces oflarge Nb deuteride particles are observe a response from deuterium trapping at causing the Porod response.' Notice that . grain boundaries. However, the large amount .
dislocation trapping is the dominant behavior of- : of deformation of the Nb samples will flatten the Nb3 sample, but that a significant Pomd out the grains. This creates a situation where component exists in the Nb2 measurement. The - most of the grain boundary area is parallel to . room temperature soh us of the Nb-D phase the surface of the sample. -In the ' standard L diagram is approximately 30,000 atomic ppm. measurement configuration, this grain The larger Porod response ofNb2 may be boundary ama will no longer be perpendicular consistent with this deuterium solubility limit. to Q, a necessary requirement for grain boundaryinduced SANS. i
, . Figure 3 shows the SANS response from a
'l3,' polycrystalline Pd sample, PPdl, loaded with a 1., ; 7 - 6400 atomic ppm deuterium. This sample was a - .
swaged by the manufacturer, and had needle-~ like grains that were oriented with the needle 4 axis parallel to the incident beam direction. In - this case, the majority of the grain boundary ama was perpendicular to Q. The scattering [ 4 gN- response from deuterium trapped at oriented L grain boundaries is dI/dn = A&pyQ2, where u 4 u 4 ., . &p) represents an orientation average over the monmee a . Fig.1 SANS from Nb deuterides and from deuterium trapped at dislocations in Nb2 T,
- r tie Analysis of the dislocation trapping component is j, -
F 7 i j diflicult without an accurate measurement of the j
=
excess deuterium trapped at dislocations. It was not possible to measure the excess fraction h* ]} _
~
during the preparation of these samples, , however. The two deuterium loaded samples 4 - * = > -
]
were deformed to the same degree and we expect the dislocation response to be of appmrimately .
' - .E equal magnitude. This is in fact what was " * * ' * *
,,,,,,3 observed. Fig. 3 Deuterium trapping at grain boundares in PPD 1 j e-.~r e grain boundaries. For a Gaussian distribution T
h . m S(p) = 1/Dq, where Dq is the FWHM of the _a ik*, I ~7" distribution. The constant A includes the.- 3, 7 lC _ number of deuterons per unit area trapped at i 1 9,}I ' i. grain boundaries. This number is found to be a* approximately 0.15 deuterons /A' for PPdi, 5 compared with a value of 0.410.2 deuterons /A=
- for an undeformed Pd sample measured -
l l % m,., 1L previously.2 .. u - l
. References Ji
- 1) BJ. Ileuser, J.S. King, G.C. Summerfield, F. ll
- l. Boue, and J.E. Epperson, Acta Metall. Mafer. - -l p
i Fig. 2 Deute'tum trapping at dislocations in Nb3 39,2815(1991). ,j-
..)
l-
'Neutmn scattering menmements performed at the National Center for Small-Angle Scattering Research at Oak Ridge l National Laboratory, Oak Ridge. TN.
77 i -
STRUCTURAL ANALYSIS AND PHASE RETRIEVAL fAETHODS IN NEUTRON DIFFRACTION STUDIES OF BIOLOGICAL LIPIDS D.L. Worcester (MU Biological Sciences), H. Kaiser (MURR), R. Kulasekere, K. Hamacher (MU - Physics) and J. Torbet (University of Edinburgh Biochemistry) Studies are being made of using vapor phase Results for sphingomyelin and cholesterol addition of perdeuterohexane or other short bilayers presently show changes in hydrocarbons to bilayer arrays oflipid diffraction through nine orders from a mixtures as a means of obtaining structura' bilayer repeat spacing of 6.3 nm. A information and phase retrieval. The diffraction pattern is shown in Figure 1. ' method of vapor phase addition of hexane to Perdeuterated hexane was added in 20% ; hydrated single-component lipid bilayers volume mixture with heptadecane and the was originally studied for the purposes of solution introduced into the lipid sample understanding the thermodynamics of the container. The solution mixture determines process, and the location of the hexane in the vapor pressure of the hexane and hence the bilayer by perdeuteration and difference the amount that equilibrates into the lipid profiles.* The main finding of these studies bilayer sample. The density profile for was that the hexane enters the bilayers and bilayers of sphingomyelin, D-5 cholesterol is localized near the center of the hydro- and D-hexane is shown in Figure 2. The carbon region, at a center of symmetry. In perdeutero-hexane is clearly seen in a work at MURR, applications to bilayers of narrow region at the center of the bilayer. sphingomyelin and cholesterol and other The additional density at this location has , lipid mixtures have been investigated. The reduced the contrast so phase assignments intes est is to determine whether the hexane are mainly benefited by the " heavy atom" at is highly localized in bilayers containing a center of symmetry. This " heavy atom" , cholesterol and whether the hexane in must be well localized for best use. perdeutero form produces changes in diffraction intensities to 0.3 nm resolution Reference that can be used for phase retrieval and 1. G. King, R. Jacobs and S. White, structure analysis. Biochemistry 24,4637 (1985). w 4 1 2 a
,, ,, ,, ., o.._._.._,.,
m._, a . Fig. 2 Neutron scattenng density profile for Fig.1 Neutron diffraction pattem obtained on sphingomyehn and D-S cholesterol brayers instrument 2XC from about 20 milligrams of a with perdeutero-hexane introduced from the . mixture of sphingomyelin and D-S cholestelol vapor phase and present as additional hydrated with H,0 and with perdeutero hexano density at the center of the bilayer. The incorpo ated from vapor repeat spacing is 6.3 nm. I 78
STUDIES OF CHLOROPHYLL CYLINDRICAL AGGREGATES AND CHLOROSOMES: ENERGY : TRANSFER IN PHOTOSYNTHESIS ! David L. Worcester (MU Biological Sciences), T.J. Michalski and J.J. Katz (Argonne National - Laboratory, Chemistry Division) Chlorophylls hydrated in nonpolar solvents disaggregated by drying, as were cylinders can form hollow cylinders as aggregates. of other chlorophylls, suggr.u,ti ;; that the _ We have studied these cylinders previously ring-I hydroxyethyl group of Behl-c, rather using neutron scattering to determine than water, was responsible for the cylinder [ cylinder diameters, and reported cylinders aggregation. of diameters from 1.0 nm to 4.5 nm .j depending on chlorophyll type. Such In ChloroBexus the cylinders are reported to .i cylinders are ofinterest as models of be smaller (5.2 nm diameter), a size we had - chlorophyll aggregates in vivo because of the not found in vitro. As a new study, we ; cylinders reported in freeze fracture electmn tested if the absence of the ring V microscopy studies of chlorosomes in the carbomethoxy gmup in these chlorophylls, green photosynthetic bacteria Chlorobium together with aggregation without the , and ChloroBexus. Chlorosomes contain hydroxyl group, produces smaller cylinders.l ; proteins and much bacteriochlorophyll-c, To do this we studied hydrated aggregates of which serves to collect light energy and Pyrochlorophyll-a. The results (Figure 1) ; transfer it to photosynthetic reaction showed smaller cylinders, which were centers. The structural basis for these comparable to the sizes reported from . processes is ofinterest for understanding electron microscopy. studies of ChlomBcxus ! how efficient energy conversion is achieved. chlorosomes. The neutron scattering data i also demonstrated some dispersion of sizes The arrangement of protein and in our artificial aggregates. Neutron , bacteriochlorophyll-c in chlorosomes is scattering measurements on intact. controversial. Some groups claim that chlorosomes were recently initiated as the proteins form the cylinders, whereas other next part of this project. groups have :laimed that portein-free ; cylinders can be isolated. Thus,it is possible that the in ! vivo cylinders are chlorophyll , aggregates such as we have -c.5 - l studied in vitm, but detailed ! experimental comparisons of g, _; these structures are badly e needed. For this purpose we 3 , are using small angle neutron 1.5 - . .i scattering.
.u-We previously reported that artificial cylinders of '
Bacteriochlorophyll-c were -2.s
- c. coo caoo o.20o. o.sco ;;
much the same size as the Q**2 (1/nm**2) ; cylinder diameters reported for Fig.1 Guinier type plot of neutron scattering data obtained from hydrated Chlorobium chlorosomes (-10 pyrochlorophylle aggregates formed in deuterated octane. The . nm diam.). We also found that concentration is 9 mg/mi. The cylindrical radius of gyration - f Behl-c cylinders were not. determined from the plot is 3.7a nm. T 1 79
l I NEUTRON SCATTERING FROM NANODISPERSED MAGNETIC PARTICLESE l J.R. Childress and C.L. Chien (Johns Hopkins University), R.W. Erwin (National Institute of ' Standards and Technology) and J.J. Rhyne (MURR and NIST) - j i Granular magnetic materials, which consist clear ferromagnetic behavior, with 60% -i of fine magnetic particles dispersed in an remanent magnetization and a coercivity of amorphous insulating matrix, display a about 600 Oe. For our sample, the blocking number of unique properties as a result of temperatures T, above which the particles , their nanometer-scale microstructure.' become superparamagnetic are 75 K for , However, many properties of granular SQUID measurements (peak in the zero-- f magnetic composites ar still poorly field-cooled susceptibility and onset of 5 understood at the funda e al level, suc'a irreversibilities) and 210 K for MS ' as the exact nature of the magnetic ordering measurements (onset of magnetic hyperfine and magnetic excitations within and splitting). Above T,,little information on { between the pains. A well known property the magnetic ordering can be obtained by of singic donnain magnetic particles is the these methods. l occurrence of superparamagnetic relaxation, ! resulting from the thermally activated Previous SANS data'showed that the high- I iluctuation of the particle moment. Q (= 1.5 nm-1) data are well described by a .; Superparamagnetism can be observed on single Lorentzian-squared scattering : different time scales t by using ditTerent function. At the smallest wavevector :i magnetic probes, such as SQUID transfers, we find additionalintensity, magnetometry (t = 10 see) and 57Fe which was modelled by adding a 1/Q' term , M6ssbauer spectroscopy (MS)(t = 10-8 sec). to the scattering. The 1/Q2 term corresponds :! In contrast, neutron scattering has a much ' to a Lorentzian cross-section with a near-shorter interaction time (typically < 10 zero inverse correlation length, thus 10-13 sec), and measures approximately the reflecting correlations on a scale larger tFan instantaneous spin-pair correlation function. what can be measured in our experiment ; The use of total scattering techniques (e.g., (roughly a few tens of nm's), It is important . SANS) and also inelastic measurements to note, however, that the form of this cross- '! fe.g., using a triple axis spectrometer) section is not unique, and that further provide a mechanism to isolate dynamic refining of the data analysis is necessary to
- processes from longer time structural pinpoint the functional form and correlation i relaxation in these nanoscale materials. length associated with the low-Q scattering.
]
t The sample examined in this study was The Lorentzian-squared amplitude [ prepared using RF magnetron sputtering, decreases with decreasing temperature, l by co-deposition of Fe and Al,0, from a suggesting that this component of the ! single mixed target onto thin Al,0, scattering is dynamic in origin. The ; substrates kept at 200 C, The granular decrease is sharp below 200 K, flattening . microst.ructure was confirmed by out near zero below about 120 K.' The ! transmission electrtm microscopy, which correlation length 4 shows a related l reveals a narrow distribution of Fe particle temperature dependence. Starting at room i . sizes around 3 nm in diameter. The film temperature in the 1 nm range, ( increases ; ; composition of 35 vol% of Fe is well below only slightly with decreasing temperature the granular percolation concentration (- 60 until about 200 K, below which a rapid vol%), and, therefore, contains well-isolated increase is observed. However,instead of a particles 8 X-ray diffraction analysis shows divergence of &, we observe a saturation at that the particles retain the body-centered about 4 nm, very close to the average - cubic structure of bulk -Fe. Magnetic particle size. By contrast, the amplitude of hysteresis loops obtained a T = 5 K show a the Lorentzian comp (ment to the scattering 80
5
. is constant and nearly zero at high limited central peak which decreased with r temperatures. As T is decreased below 200 K, increasing temperature reficcting the intra- ;
the amplitude begins to increase and rises particle order parameter, and (2) a very sharply below 75 K, a behavior typical of order broad quasielastic Lorentzian line which parameter scattering. Because of the long . increased with increasing temperature correlations lengths associated with this presumably correlated with the inter - scattering, it is suggestive ofinter-particle particle coupling dynamic fluctuadons. ' ordering. Due to the short characteristic time scale, there is no evidence of magnetic References blocking in the SANS data in contrast to that L C.L. Chien," Physical Phenonmena in observed in the magnetization and Mussbauer Granular Materials," G.D. Cody, T.H. results. Geballe, and P. Sheng, eds., Mat. Res. Soc. Symp. Proc. 195,411i1990). -
- 2. B. Abeles, Appl. Solid State Sci, 6,'1 Additional data have been taken on triple axis (1976). ,
spectrometers using a range of energy 3. J.R. Childress, C.L. Chien, J.J. Rh'yne, resolutions to study the melasticity of the and R.W. Erwin, J. Mag. and Mag. .. ; scattering. These results showed the presence Matts.104-107,15S5(1992 L l of both very fast (< 10-11 see) and much slower dynamic processes. In particular, inelastic data taken with 850EeV ene@, 'Nmtmn scanning egrhnsta wem performe.1 at the NDS Reactor of the Natwnal Institute of Standards and - resolution showed (1) an elastic resolution Technology, Gaithersburg. MD 20899. MAGNETIC STRUCTURE Of DylSc SUPERLATTICES' ; F. Tsui, C.P. Flynn, R.S. Beach, and M.B. Salamon (University of Illinois-Urbana Physics), J.A. Borchers, R.W. Erwin (National Institute of Standards and Technology) and J.J.Rhyne (MURR and NIST) ; Molecular beam epitaxy techniques can be multi-layer spin cormlations show that the- . i used effectively to do atomic scale engineering range of this coupling falls offinversely with the on layered epitaxial specimens when it is thickness of the non-magnetic layer and is desired to control closely the number of consistent with the range calculated from the ' atomic planes or two (or more) elements in width of the generalized conduction electmn ' adjacentlayers. In addition the techniques susceptibility function (q) for Y (or Dy).8 These allow the building of multilayer sequences of functions show a sharply defined peak along the - 1 a prescribed number of bilayers, within each c* direction in recipmcal space at a value of . . . of which the number of atomic planes is reduced q corresponding to the periodicity of the~ -l closely controlled and reproducible. magnetic ordering (for those elements having 4f '! spins as in Dy, or for a pseudo magnetic . . Previous studies by this group' on c-axis growth ordering in Y) as dictated by the caliper - 1i layered structures of magnetic rare earth dimension spanning parallel sheets of the metals alternated with non-magnetic Y [e.g., Fermi surface. Perpendicular to the c* direction- [ Dy1Y] have shown that bulk-like magnetic the susceptibility function is centered at q = 0, ? orderis developed in each of the magnetic and is quite broad corresponding to a much . layers and that,-in the case of the periodically shorter (appmximately one neighbor) coupling ; ordered structures (e.g., Dy], this order shows a range in these directions. The anisotmpy in (q) -
- phase coherence from one magnetic layer to the - ' and its effect on the range of magnetic coupling l
. next. Suchresults imply a long-range spin was graphically demonstrated in superlattices ;
density wave type coupling which is propagated oflDy lY] gmwn along a basal plane direction8L .! across the non-magnetic layers. Studies of the which showed magnetic order within each l 81 - e r ~ .- . , _ - . .s..
l magnetic layer, but a total absence ofinterlayer in net superlattice moment (layer to layer coupling in contrast to the long range interlayer correlation) was achieved and even in fields as coupling observed in the e-axis growth direction large as 6T, full saturation was not achieved. superlattices. There was no evidence of any critical transition fields but only a smooth increase in net moment. Dilute alloy studies of magnetic ram earths in Sc8 have shown an anomalous critical Future investigations into the anomalous concentration behavior for the onset oflong exchange range effects in Se superlattices are range order in contrast to Yialloys which show underway. order for alloys as dilute as 1% magnetic ; impurities consistent with the ek ctronic 8000 , i
. structure predictions of very long range Sc(0002) interactions. In Sc the critical conwntrations l ;
are in the range of 25% of the magnetic element ,(l ! necessary to induce ordering. Such large magnitudes are more closely reminiscent of
- j nearest neighbor percolation arguments than of the long range spin-density wave coupling seen , l
.l {t -
in Y systems. Such a discrepancy is not found in -3 c g h the calculated x(q) functions. This anomalous y4000' diffemnce in Y and Sc was the motivation for E , investigating superlattices ofDy and Sc. In spite of the large basal plane lattice parameter b . mismatch (> 84 ) successful growth of several R-i . [Dy I Sc] superlattices was achieved. Jl l As shown in Figure 1, the neutron experiments on [Dy1 Sc] superlattices revealed only a very o broad temperature-dependent magnetic component underlying the nuclear scattering {0 2.3 2.6 . which is consistent with a ferromagnetic Oc .M Fig.1 Neutron diffraction scan along the {00021 i coupling of the Dy spins below a T,- 150 K. The direction in the superlattice [DyulSCA Curve magnetic state above 150 K up to the expected a is the nuclear intensity showinD fwe structural y ordering temperature of- 180 K was uncertain harmonics. curve b is a zero field scan at 10K -i although no evidence of a helically ordered state sh wing the devel pment I short-range 5 ferromagnetic order indicated by the solid hne was observed. The broad peaks corresponded to under the structurai peaks, and curve c is e scan a wrrelation length for the order extending taken with a 60 koe applied field following zero- 5 along the c-axis grov. . h direction ofless than the field <wling of the sample mustrating field-layer thickness. This result clearly showed that indu edierr magnet:ccoherence. the magnetic order was not propagated through the non-magnetic Se layers unlike the case for Y References , superlattices. 1. J.J. Rhyne, R.W. Erwin, J. Borchers, M.B.
- Salamon, R. Du, and C.P. Flynn,Physica B 159, -;
This puzzlinglack ofcoherence in Sc 1 111(1989). superlattices was further investigated in field "
- 2. C.P. Flynn, F. Tsui, M.B. Salamon, R.W. Erwin,:
dependent studies of the scattering in which the and JJ. Rhyne, Phys. Letters F 1,5997 (1989). field from a superconducting magnet was 3. H.R. Child and W.C. Koehler, Phys. Rev.174, . applied along a basal plane direction to 562(1968). art.ificially induce coherent order along the 4. J.A. Gotaas, JJ. Rhyne, L.E. Wenger, and J.A. , layers. These results at both 10K and 80K Mydosh, J. de Physique, Colloque C8, Suppl - showed only a very gradual monotonic increase #12,365(1988).
- Neutron sentiedngSxhments were pedormed at the NHS Reactor of the National Institute of Standards and Technology. Gaithersburg, MD 20899. ,
82 L r t I i. [
,t
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i
~
f i l NEW MURR HORIZONTAL SANS INSTRUMENT UPDATE y Brent J. Heuser, Mihai Popovici, Ronald R. Berliner, William B. Yelon, Olawale Oladiran, David ' Nickolaus, C1 ester Edwards, James J. Rhyne (MURR), and David L. Worcester (MU Biological Sciences) Design oithe new SANS instrument is well The primary fast neutron and gamma-ray L underway. This instrument will be located filtration will occurjust outside of the E ' j~ at beamport E and extend into the north port biological shield.' 'A beam stop/ filter vestibule of the beamport, flooc. Work. cryostat elevator will hold the neutron and , performed to date and significant aspects of gamma-ray filters in position during . the design are as follows. operation. Be and Bi filters will be used in the SANS channsi at this h> cation. A second filter position further downstream, b A two-wire, gas filled proportional counter manufactured by ORDELA was received in between the monochromator device and the April of 1992. The detector is being stored start of the incident collimation, aho is . . on the beamport floor until testing this included in the SANS instrument design. winter. The detector vacuum chamber -i
" Request For Proposals" was awarded to- The neutron monochromator device will ii the Paul Mueller Company in Springfield, consist of two Ni-Ti multilayers in an anti-MO, with delivery of the stainless steel . parallel arrangement. The first multilayer tank expected in January 1993. Detector . will be a stack of approximately 4 cm long . .
translation within the tank will allow wafers in soller geometry. The second continuous adjustment of the sample to multilayer, downstream from the first, will detector distance from approximately 1 to 8 be a single wafer approximately 2 meters , meters, long in reflection geometry. Extensive calculations indicate that this - In order to accommodate a total of three configuration maximizes the incident instruments, a new in-port collimator will current while providing good instrumental . be installed at beamport E. This collhnator resolution. In the current design, the ; will have two separate channels (a SANS downstream multilayer is slightly curved channel and a thermal channel) with a 3' in the diffraction plane. This eliminates divergence in the horizontal plane. A two the inherent resolution asymmetry of . channel collimatoris necessary to . multilayer monochromators and also accommodate the difTerent incident beam provides a certain degree of phase space . sizes and filter requirements of the E port focusing. Testing of pmtotype multilayer - instruments. Geometric constraints, both - depositions has been underway for the past . ; within the beamport and on the beamport six months. The results have been ' floor, dictate that the two channels are encouraging, with peak reflectivities of. divergent. The entire beamport, including approaching 95% in the best case. l the collimator section, will be filled with He :
. to eliminate long wavelength neutron ~f attenuation by air and water vapor. Current work on the projectincludes ;
Allowances will also be made for room further testing of multilayer depositions,1 ! temperature neutron and gamma ray detector support and beam stop design, and . [ filters within the beamport collimator. beamport E shielding design. ~
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TRIAX - MURR'S NEW TRIPLE-AXIS SPECTROMETER l i K.W. Herwig, S.A. Werner, and J.J. Rhyne (MURR and MU Physics) , The MURR Center and MU Physics staffin milimators: Cd-plated steel, an open [ collaboration with C. Stassis, J. Zaretsky, position, and beam stop. ; and A. Goldman from Iowa State University are developing a highly versatile, triple-axis The largest and heaviest single component : spectrometer, TRIAX, on beamport A of TRIAX is the monochromator drum which , funded by the National Science Foundation, rotates as the incident neutron wavelength 'i MU and the Ames Laboratory (DOE). is varied. This drum contains the
- Major components of the new instrument monochromator assembly at its center and were delivered to MURR from Oak Ridge serves to stop stray scattered neutrons and -
National Laboratory in mid-October 1991, the beam transmitted through the Since that time, these components have monochromator. The three focusing been thoroughly refurbished, and design monochromators will be accessible remotely, and construction of missing pieces initiated. the choice depending on the particular , When completed, TRIAX will be a world experiment. The focusing device-using class instrument used to address a variety copper, pyrolitic graphite and pressed silicon ' of problems in condensed matter physics monochromating crystals-has been and materials science. Here we summarize purchased. The system of shielding wedges 3 the progress that has been made on TRIAX that lift and lower as the drum rotates - ' and outune the remaining tasks. requimd extensive abuilding, and this task .; and other refurbishing of the main drum There are several principles which govern was completed earlier this year. the design and ultimately the effectiveness of the instrument. The goalis to maximize Cantilevered from the monochromator , the number of neutrons incident on the drum is an arm which holds the sample sample while minimizing the neutron and and analyzer tables, the assembly of seven gamma backgrounds in the immediate 1/2 inch diameter 8He detectors, and - vicinity of the instrument. The first is associated shielding. This arm required . achieved by optimizing the neutron optics of substantial modification and rebuilding of 'l the instrument while the second is satisfied the drives associated with the rotation , by the design of effective shielding. axes. In addition, an entirely new-shielding system for the analyzer crystal While design of the neutron beam path has was designed and is under construction, ! been completed (and construction under- with shielding wedges cast from a mixture i way), design of the surrounding shielding is of B,C and epoxy. New detectors have j only in the conceptual stage. Contained in been purchased and the associated i this heavy concrete shielding will be the shielding is being constructed. Eight .i double-axis monochromator, the filter stretched-film Soller collimators that will cryostat, and a Soller collimator elevator define the angular divergence of the assembly. A beryllium single-crystal, beams scattered by the sarnple and y viewed in transmission by the triple-axis analyzer crystal are nearing completion. i instrument, seems the likely choice of These items are being built in the Physics double-axis monochromator. F. Ross is Machine Shop by C. Holmes, S. Potts, R. responsible for the double-axis instrument. Schlotzhauer and W. Steifermann. The filter cryostat has been constructed and will contain three individual filters: B. McCracken and C. Edwards of the MURR pyrolitic graphite, beryllium and silicon. Facility Operations group are beginning the The Soller collimator assembly, designed design of the major shielding components to and under construction, will wmtain 'hree be located on the beamport floor. This work 84
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{! S ft - ->j , includes designing concrete shields and analyzer crystals) have either been purchased . -i reworking the beamport shutter. The or will soon be ordered. computer control program, based on the NeXT station,is being developed by R. lyer Although much work remains to be done, we and G. Moum of MURR's Computer believe that a realistic goal for installation i Development group. The interface and and testing of the machine is Marth 1993, at - motor drivers are being constructed by R. which time all major components should im ' > Berliner and his assistants in the MURR completed and ready for assembly and ; . Instrument Development group. In addition, testing. \ various pieces of peripheral apparatus .
'i (closedgele refrigerator, temperature This work is supported by NSF-DMR-controller, low-temperature cryostat, pyrolitic . 9103383 ($225,000); DOE Ames Laboratory . ,
graphite filters, and monochromator and ($50,000); MU Prime Fund ($144,0001 .: l e SS i t
NEUTRON OPTICS- GROUP . Samuel A. Werner, Group Leader and Professor of Physics Helmut Kaiser, Senior Research Scientist (Adjunct Associate Professor of Physics) This group is engaged in basic studies of the fundamental properties of the neutron utilizing two neutron interferometer instruments at-the MURR Center and is also developing a neutron interferometer. The group has broad .- international collaborations and the interferometry program has had continuous funding from the National Science Foundation for more than 15 years. The current grant is NSF-PHY-9024608 running from June 1991 - June 1995 in the total amount of $616,000. t 86
q NEUTRON INTERFEROMETRY S.A. Werner (MU Physics) and Helmut Kaiser (MURR) The perfect silicon-crystal neutron consisting of 4 small Firestone pneumatic , interferometer has provided us with a isolators. This arrangement is essential in , wonderful device to observe subtle order to provide for vibration-free and . quantum mechanical phenomena and microphonic-free operation. The interactions with clarity and elegance. We interferometer ased in this set-up is an LLL-have two neutron interferometry type device. The LLL stands for three Laue-experimental stations at MURR. transmission geometry reflections in the three crystal slabs which make up the The instrument at beamport B was interferometer. constructed during 1976-1977 with NSF , funding. A schematic diagram of this The continued growth of the neutron instrument is shown in Figure 1. A interferometry program at MURR over the monochromatic beam is produced in a past 15 years has created the demand for a double-crystal monochromator ass 2mbly second neutmn interferometry set-up at , which presently utilizes two copper (220) beamport C (Figure 2). This instrument crystals. This monochromator assembly utilizes a skew symmetric interferometer as produces a variable energy incident beam shown in Figure 3. The beam comes from a in the wavelength range of 0.9 to 2.4 A, vertically-focussing pyrolytic graphite (Po) - 3 which is allowed to pass through a series monochromator. The wavelength is fixed at i of slits and then onto the interferometer. A= 2.35 A. The beam passes through a PG The interferometer, along with the 'He filter to eliminate order contaminations detectors,is mounted inside an aluminum from the beam incident upon the inter-box, which providcs for thermally-isolated ferometer. Recently we have carried out operation of the interferometer. This box experiments on the Neutron Phase Echo is rigidly mounted on a rotator assembly effect, the efTect of Spectral Filtering in (for gravitationally-induced quantum Neutron Interferometry, and Time-of-Flight interference experiments)inside of a large Neutron Interferometry on this instrument. , dense Benelex 70 neutron shield, which in The experiments formed the basis of Russell turn rests on a vibration-isolation support Clothier's PhD thesis research.
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n We have two international collaborations: roo vu.c with the Vienna group of Professor Helmut-
*-'~'.- -
Rauch and his students, and with Professors ,
~#/2"~** ' A.G. Klein and G.I. Opat and their students
^~'"'. at the University of Melbourne, Australia.
. ~ ,- ...,
yCX4 '~~2C'~ _,_, The Aharonov-Casher effect experiment that p ! ~~-' attracted wordwide attention (it wcs written Lb , ,,,..,. [-{ ,,,,
; j
[f"L~ ,J/ h l 3 up in Physics Today, Science News, _ Scientific American, etc.) was carried out at beamport B in collaboration with the l l
, , . f Melbourne group. The recent experiment m
=.j,,j,,,,, _f,,, 1 f
wh' cn we observed the scalar AB effect for
~ ' ~ ~ ~ ~ '~
the first time was carried out at beamport C ! in collaboration with Brendan Allman, a student from Melbourne. The neutron ; phase echo, spectral filtering, and time-of.
-35)- #~W flight experiments were carried out in
'~- * ~' ~
collaboration with Harold W61witsch and W
.,.T *
) ,h. Helmut Rauch from Atominstitut, Vienna. I
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87, - We are also involved in a collaboration with ' l
--w) Drs. Muhammad Arif and Geoffrey Greene "S ~- g d'$_, ,',, at the National Institute of Standards and
$ 3 ,, -,~ ,,,. _- Technology in building a new, sophisticated e....'...........
g.-.
.f. neutron interferometry instrument at the
.r. . . . . ..n.::. . .y . . . . .
NBSR in Gaithersburg, MD. Ken Littrell, a graduate student of ours, is doing his PhD Fig, 2 Interferometer set-up at beamport c. thesis research there. A=235X BEAM FROM KrKXH 0fMTOR C. 3He DETECTOR mw . Bi SAMPLE . c, ., tL F ~/q. SLIT '
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g HeDETECTORS 88
I e
' A list of the experiments carried out in this Descriptions of several of these experiments program over the past 17 years is as follows: are given in a number of widely used physics textbooks, including J.J.Sakurai's
- Observation of Gravitationally- Quantum Mechanics and K. Krane's -
Induced Quantum Interference . Introduction to Nuclear Physics. =j (1975,1980,1985,1988)
- Observation of the Change of Sign of During the next year we will be upgrading the Wave Function of a Fermion due the instrument at beamport B. This impmement will e nsist of replacing the to Precession of 360 Degrees in a computer with a NeXT stat on, upgrading Magnetic Field (1976) the interface and modifying the double .
- Observation of the Effect of the crystal monochromator assembly so as to Earth's Rotation on the Quantum utilize a 4 inch high beam with a vertically-Mechanical Phase of the Neutron focussing second monochromator. This ;
(Sagnac EfTect),(1980) modification will yield an increase in
- Measurement of the Energy- counting rate of about a factor of 4.
dependent Scattering Length of Sm-149 in the Vicinity of a Thermal Nuclear Resonance (1983) Our agenda of experiments for the next .
* - Measurement of the Longitudinal three years is the following: .t Coherence Length of a Neutron Beam Effect of the moon and the sun on :f (1983)
=
Neutron Interferometric Search for quantum interference -
- Aharonov-Casher effect-stage II Quaternions in Quantum Mechanics l (1984) eKPeriment ,
- Experiment on the Null-Fizeau Effect
- Multi-photon exchange between a for Thermal Neutrons in Moving neutron and an oscillating magnetic :
Matter (1985) I'"Id Precision Measurement of the Bound-
- Search for quaternions in Q.M.-stage l Coherent Neutron Scattering Length II experiment of U-235 (1986)
- Wheeler-delayed-choice experiment a
Obser"ation of a Motion-Induced Highly precise gravitationally-induced Phase Shift of Neutron deBroglie quantum interference experiment, Waves Passing through Matter Near a checking the effect of x-ray Inletrogation areas Nuclear Resonance (1987) Observation of the Topological Construction oflarge-scale, split-Aharonov-Casher Phase Shift (1989) C mPonentinterferometer Observation of the Effects of Spectral
- Michelson-Morley experiment with . l Filtering in Neutron Interferometr'y neutrons o
- v (1990) Search for the Mashhoon efTect
. Observation of the Neutron Phase (coupling of spin to rotation)
Echo Effect(1991) . Coherence Effects in Time-of Flight This program has been funded continuously by ; l= Neutron Interferometry (1991) the Physics Division of the National Science Foundation. The current grant is NSF-PHY-Observation of the Scalar Aharonov- .i Bohm EfTect(1992) 9024608, June 1991-June 1995, $616,000. !
'l q
89 l
ELECTROMAGNETIC ACCELERATION OF NEUTRONS R.C.Casella (National Institutes of Standards and Technology) and S.A.Werner (MU Physics) Discussions of topological phenomena in the neutron gyromagnetic ratio relating its quantum mechanics, such as the magnetic moment p to its spin angular Aharonov-Bohm (AB) and Aharonov- momentum s. This acceleration would Casher (AC) effects, are most ea ,ily produce a maximal efTect on the neutron framed in the language of Dirac-Feynman kinetic energy when p is along its direction path integrals. Apart from the important of motion v, with E and B collinear while quantum phase, the path-integral normal to v. For reasonable values of IE l formalism allows us to employ classical (- 300 kV/cm) and of i B I (= 0.005 T) that concepts such as velocity, accelcration and can be achieved within the confines of a the orbit of a particle. This facilitates the neutron interferometer, the Anandan consideration of orbits winding around formula yields an oc leration ia i = 0.18 cnds". topological charges, such as the magnetic This would give rise to a measurabic phase flux in the AB effect and the linear charge shift by current neutron interferometry density in the AC effect, to calculate the techniques. phase shift in an interferometer experiment. However, as recent.ly stressed The Hamiltonian for the neutron moving in a , by Casella' in discussing variants of the region of space containing both an E field and neutron interferometry experiment on the a B field in the interferometer's frame is AC effect carried out by Cimmino et al, it is essential to treat the neutron spin as an H=p'/2m - pp,f U-(limc)pxEhz. intrinsically quantum variable. That emphasis is brought into focus here where Here o,=+1 or -1, p is the canonical we describe an attempt to search for an momentum, the axis of quantization is experiment to detect a putative along the unit vector z, parallel to the , acceleration of the neutron in the efTective field IB-(1/me)pxE]; and E and B combined presence of electric E and are each constant. It then follows magnetic B fields, as measured in the rest immediately, using Hamilton's equations, frame of the interferometer (Figure 1). that the acceleration a=0. This is contrary This acceleration, recently suggested by to the prediction of classical mechanics ; Anandan,8 is a=(y/me)Ex(pxB), where yis given by Anandan. , wtAK naA1 FGD .1
" eM$rron emoa This work is supported by NIST
" C"**4"7 a==7 (Department of Commerce) and NSF p- _O (grant number PHY-9024608). It has G I--- i been submitted to Phys. Rev. Lett. for u s* publication.
up cm; sm merunem PmSE RAG # nererences a p; 1. R.C. Casdla, Phys. Rev. Zett. 65,2217 i g ,
~m._._,
(1990).
- 2. A. Cimmino, G.I. Opat, A.G. Klein, H. ;
Kaiser, S.A. Werner, M.Arif, and R. ! Clothier, Phys. Rev. Lett. 63,380(1989). romenow Rg.1 Diagram mustrating a neutron interferometer arrangement 3. J. Anandan, Phys.Lett.138A,347 to search for the putatrve Anandan acceleration. (1989). 90
GAMMA-RAY SCATTERING GROUP PERSONNEL Guy Schupp, s .aup Leader and Senior Research Investigator (MURR) and Professor of Physics Fred Ross, Senior Research Scientist (Adjunct Professor of Chemistry) William Yelon, Senior Research Scientist (Adjunct Professor of Physics) FACULTY ASSOCIATES James Mullen, Professor of Physics, Purdue University This group at MURR is concerned with University of Florida. This group has materials science research conducted with the constructed a detector with a crystal-University of Missouri Gamma-ray lographically oriented germanium erystal. The Spectrometer (MUGS) and the QUasiElastic detector and its dewar assembly were mounted Gamma-ray Spectrometer (QUEGS) in the sam ple positian ofthe MUGS instrument instruments located on the beamport floor. to search for anomalous transmission Elastic scattering phenomena at photon accompanying the channeling effect. In addition, , wavelengths of 0.03 to 0.10 A are investigated the detector can be operated in coincidence with
-)
with M UGS whereas QUEGS uses M6ssbauer the transmission detector to analyze the energy photons with wavelengths in the 0.1 to 0.3 A cfrects orchanneled radiation. range to study non-clastic interactions in a manner that is unique in the world. Research with QUEGS has been supported since 1983 by the Department of Energy in a . A major application ofMUGS is the evaluation collaborative program with Purdue University. of crystal quality through the detailed These studies have ranged from fundamental investigation of mosaic structure by Bragg line-shape analyses to anharmonic effects in -i diffraction. This technique is routinelyapplied sodium and tungsten. These line-shape studies , to various materials being considered for have led to the most accurate values reported fabrication into detectors or monochromators, for interference parameters in five different An on-going project for MUGS involves the M6ssbauer transitions. In addition to a better evaluation of crystal perfection in mercuric understanding of the interference iodide grown by EG&G-Santa Barbara for the phenomenon,. systematic trends in these-I development of the technology for room- measurements have implications concerning temperature semiconductor detectors. time-reversal-invariance. Crystals grown in the micro-gravity environment ofthe space shuttle were analyzed Quasielastic broadening of the observed using MUGS to determine the role of gravity M6ssbauerlinewidth due to difTusive motions in the growth of high-quality HgI, crystals. in pentadecane and polydimethylsiloxane have
'alsobeeninvestigated. Asubstantialupgrade ,
Another collaborative research project using of QUEGS supported by the DOE and by MUGS is the measurement of radiation University sources is planned for completion ! channeling being pursued by a group from the in Fall 1993. 91 1
. MOSSBAUER CHARACTERIZATION OF TUNGSTEN DOPED YBCO HIGH Tc SUPERCONDUCTOR J. Day, J.G. Mullen (Purdue Physics), G. Schupp (MU Physics) and W.B. Yelon (MURR) Many studies have been carried out on the different tungsten sites (Figure 1).: One YBa,Cu,0,,(123) system since it was corresponded to that'of precipitated ; ~ found to be superconducting at -92 K in tungsten at the grain boundaries, and i 1987. A number of these studies have the other site was due to either a) dealt with modifying the 123 system by tungsten substituting for copper chain doping and ' hen investigating the changes sites, or b) precipitated WO,. The caused by the dopants. Besides offering precipitated tungsten can be seen in the insights into the physics of high transition figure as the large. center line (1), and - . temperature superconductors (HTSC), the substituting tungsten can be seen as ! altering the basic structure by doping can the hyperfine split lines (2), (3), and (4).- lead to enhanced superconducting Correcting for thelarge Debye :i characteristics such as the transition temperature of the precipitated , temperature T, or the critical current tungsten site, compared to the density J,. substituting tungsten, we calculated , that approximately six times as much - One such doped system is the YBa.Cu,W
, , 0,,
tungsten is located in the second site as . l (123-W) superconductor. Because there compared with the precipitated tungsten ; was some question of where the tungsten site. Another experiment with the ') site was located in the "*W structure, we YBCO superconductor absorber cooled to carried out a M6ssbauer experime it to 10 K will be performed to determine the l resolve this issue. location of the substituting site. Ifit turns out to be a copper chain site, the The M6ssbauer experiment used a "'Ta result will be exciting for [ source and a t2*W, x = 0.08 absorber using superconductor research. ; the QUasiElastic Gamma-ray ! Scattering 123-W (x = 0.08)-
- instrument * **
..,]., , , g ,, .,, J ;
(QUEGS) at MURR. -. - 100 r q,* i f ,l , Both the source and C . , , j absorber were .9
- 4 # .'
**** i cooled down to $ 99.5 .
_ .4 ~ liquid nitrogen temperature. The j **. s 3 lJ e 99 , 2 , , . M5ssbauer C spectrum was 6 , collected until the F 98.5 e. -5 , baseline had E .' , appmximately 8 pg .
** 1
- l 520,000 counts. g ,
Q. . Using precise line. 97.5 . y. shape analysis of- -7.5 -5 -2.5 h 2.5 5 7.5 the resultant-Spectrum, we were . able to determme that there were two ng 1 5% M5ssbauer spectrum for 8 atcmc % W doped YBCO th? 77 K - 92 o
GAMMA-RAY SCATTERING STUDIES OF ALKALI HALIDES IL Wagoner, J.G. Mullen (Purdur University Physics), and G. Schupp (MU Physics) The change in elastic fraction of Mussbauer filters. Further studies will focus not only photons upon Bragg reflection was on the clastic and inelastic senttering as a measured for Nacl, NaF and LiF crystals. function of Bragg angle, but also as a The Mussbauer width of 2.5 meV for the function of temperature. 46.5. kev photons from "W allowed energy s m a. cryu .i resolutmn not available in x-ray or neutron scattering methods. A natural tungsten foil ,Z", f analyzer) was Doppler shifled first in a ,- 'j ,' . , position between ine source and crystal (/ N under study (before position) and then in a / *"" '., position between the crystal and the photon ,' detector (after positionL The two arrange-ments are shown schematically in Figure 1. g' ,p Careful lineshape analysis gave the recoil- a rc* rhocaa 4 r.cror less fraction, f;, for the photons incident on , the absorber in the before case (which was
**d'""*'
also the same as the resonant fraction emitted from the source itself, f,L The un
"~ '
recoilless fraction for the after position, f,,, J' is related to f, by ,',' ' . , ,ry
' /.mn, l .' . ,
g'" _ (c +e i) 8g ' g' p where r and i are defined as follows. If N is " c- = * " " the number of M6ssbauer photons incident Fig 1 schematic geometns for the (a) before ard on the crystal, rN and iN are the number (d) after positions used in these studios. scattered clastically and inelastically, respectively,into the detector. The efTective r -- fraction, F, is given by l Table 1 Values ot F for the Crystals and Bragg Reflections Studied p c . _ _ _ . _ . _ - - - f* O_ E+1 . , reflection Fmeasured Fbest fit Our values of F for the crystals and Bragg l Nacl (200) 0.980(4) 0.984 reflections st udied are tabulated in Table 1. l (400) 0.966(4) 0.964 , The tungsten absorber was a natural foil l (600) 0.949(6) 0.949 I 50.8 mm thick. Data were collected for the j absorber and crystals at room temperature- NaF (200) 0.962(3) 0.973 It is noteworthy that the smallest value of F (400) 0.947(3) 0.945 is still 0.942( 5) for the (600) reflection from ! i600) 0.942(5) 0.939 Nacl even though the integrated intensity of this reflection is more than an order of LiF (200) 1.000(3) 0.996 magnitude smaller than the (200) reflection. , (400) 0.991(3) 0.993 Large values of F are important since these ; crystals are widely used as monochromating L_ _ _ _ _ _ _ _ _ 93
c , M6SSBAUER SPECTRA OBTAINED BY MODULATING A SCATTERING CRYSTAL G. Schupp, K. Barnes (MU Physics), W.B. Yelon (MURR) and J.G. Mullen (Purdue) Supported by an Instrumentation Grant of - oscillated along the scattered beam line. When
$74,065 from DOE and $52,000 in MU matching the channels are converted to velocities via our funds, plans are underway to upgrade the " crank function," the width of the crystal i M6ssbauer quasielastic gamma-ray scattering modulated spectrum, ru ,is related to the usual (QUEGS) instrument with a new source cask to M6ssbauer width, r, by r, = r/(2 sine), whem o is ,
give four beam lines and a cryorefrigerator to the Bragg angle for the reflection used. The data yield s 20 K source temperatures. In additian, shown in Figure 2A wem collected in 2.7 hours ' the plans include a modification of our present using the 400 Bragg reflection of a stressed LiF sourte cask to accommodate vek> city modulation crystal; data were also collected using the 200,__ , of the source. This modification would allow use 600, and 800 Bragg reflections. The . of a fixed MultifoilInternal Conversion Ekstron experimental values for r, are given in Figure 20 (MICE) detector which, in favorable cases, can along with the expected r/(2 sin 0) values for these give an improvement in the M6ssbauer signal to measurements. continuum ratio of more than a factor of 10. Another method for obtaining the velocity We were particulary pleased with the ease with - modulation with a fixed MICE detector (it gets which these data were obtained as well as with
- noisy when oscillated at high velocities for the excellent agreement seen in Figure 20.
extended periods)is to move the Further experiments are planned using the ~ a monochromating filter crystal along the MICE detector, different filtering cystals, and scattering vector (Q) while also leaving the difTerent scattering geometries to see if this source fixed. The difficulties associated with method would be better operationally than ' this approach are that the velocity component modulating the source. along the incident and scattered gamma-ray . beams is commonly small and the scattered _h ( intensity depends on the uniformity of both the motion (lack of vibrations) and the crystal over
~
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- 1. "7 N '
P Initial measurements on oscillating the filtering
=
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- Fig. 2 (A) Muftiscaling spectrum taken with the
.The minima in Figure 2 occur at the turning experimental arrangement shown in Figure 1. ]
points (positional extremes) of the oscillatory (B) Spectrum taken with the monochromating - l crystat fixed and the absorber oscillated along motion where the vek> cities are zero. Figure 2B l the scattered beam line. (C) Summary of the shows an ordinary spectrum taken with the observed hne widths versus the expected .j filtering crystal at rest and the absorber being widths for the four Bragg reflections used. j Fig.1 Schematic drawing for
"" ^ * * "
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REACTOR NUCLEAR ENGINEERING PROGRAM PERSONNEL J. Charles McKibben, Coordinator (acting) Kiratadas Kutikkad, Research Scientist ( Adjunct Assistant Professor, Nuclear Engineering) Wehr A. Meyer Jr, Reactor Manager Susan M. Langhorst, Health Physics Manger (Assistant Professor, Nuclear Engino: ring) Michael D. Glascock, Senior Research Scientist (Research Assistant Professor, Nuclear Engineering) Gary J. Ehrhardt, Senior Research Scientist (Assistant Researth Professor, Radiological Sciences) Robert M. Brugger, Senior Research Investigator (MURR) and Professor of MU Nuclear Engineering , Jay F. Kunze, Senior Research Investigator (MURR), Chair and Professor of MU Nuclear Engineering William H. Miller, Group Leader (MURR), Professor of MU Nuclear Engineering, Director of Energy Systems and Resources Pregram Mark A. Prelas, Senior Research Investigator (MURR) and Professor of Nuclear Engineering Roland A. Hultsch, Reactor Physicist Olawale B. Oladiran, Staff Engineer Sudarshun K. Imynlka, Senior Research Investigator (MURR), Professor of MU Nuclear Engineering and Director of Particulate Research Center Reactor Nuclear Engineering Program Group: Hydmgen Embrittlement and Non-Destructive Evaluation The n uclear engineering program at MURR addition of new research programs, is intertwined with the MU Nuclear instrumentation and equip-ment, a cold Engineering Program (MU NE) in the neutron source, improved reactor systems, College of Engineering. Reactor facilities a new fuel design and a powerincrease. The are used for laboratory classes and as the work to support this effort is spread base for a significant number of research throughout various MURR groups and also projects in collaboration with the MU NE involves many faculty associates. program. A few of these research projects are described in summaries following this The members of the Nuclear Engineering introduction and others are given in the Program are especially involved in the new Hydrogen Embirtilement and Non- fuel and power upgrade analyses. This part , Destructive Evaluation Group section. of the upgrade has provided excellent graduate research projects for students in MU is in the process of upgrading the the MU NE program. Currently five PhD research and operational capabilities of the and one MS projects arein progressinvoh ing l- MURR Center a n d associated facilities. The these areas. Since 198510 master's and 2 1- plans include an expanded research building doctoral theses have been completed > j that will double the laboratory space, the concerningthe new fuel and power upgrades. l-97
CONTAMINATED SHIPPING CASKS Jay F. Kunze, Bruce Gu, George Vosnidis, Jun Lu (MU Nuclear Engineering), Michael D. Glascock and J. Steven Morris (MURR) Spent fuel shipping casks will find major that were necessary to induce wwping. uses during the end of this decade, as spent Figure I shows a typical batch ofdata, from fuel is shipped from the 110 operating power a variety of envimnmental tests fmm 0" F to - reactors to the Monitored Retrievable 100" F, low to high humidity, and with Storage (MRS) sites to be established by the varying temperature gradients across the US Department of Energy. With the pipe wall and surface stresses, simulating .1
- l. shipments that have occurred over the last those that would be present in a shipping H l
15 years, there have twen significant health cask. As the figure shows, the weeping was : physics control problems encountered, as much as a factor of 10 (in a few cases as l .! known as " weeping" or " sweating" of high as 100) above the initial surface 1 adsorbed surface contamination. A number contamination. of violations have been issued by the Nuclear Regulatory Commission (NRC) to the As part of the assessment, measurements shipping organization when casks that were on the consistency of results of swipe checked out as being below the surface measurements were conducted, under a contamination limits arrived at the mceiving variety of conditions and using a variety of end well above the allowed " swipe" limits of health physics " technicians." The conclusion - 2?.,000 disintegrations per minute per 100 was that variations in swipe technique were square centimeters. negligible compared to the weeping effects found. it was also concluded that variations A cooperative research effort with the over the cask surface could be significant,- Callaway Nuclear Power Plant and and, therefore, that a 100 square centimeter sponsored by Sandia National Laboratory area for the swipes was too small an ama to exposed a number of 6-inch diameter pipe obtain a truly representative sample-or samples of typical shipping cask c ater rall alternatively, that many areas of 100 sq cm material in the Callaway Spent Fuel Storage needed to be swiped to obtain a repm-Pool. The pool water contamination is less sentative surface contamination than I radioactive atom per 1012 water measurement. molecules (0.6 atoms of cobalt and 0.1 atoms of Cs-134 plus Os-137 per trillion water Most surprising, however, was the result of molecules). The samples were then returned the total contamination measured on the to the University for analysis and samples, something that never could be done environmental testing to determine if on the actual shipping casks. In general, the weeping could be induced, and if so to try to measured " removable" surface contami-understand the cause, nation (as measured with a swipe) was only 1% or less of the total" fixed" contamination. The results were most mnclusive, Weeping Hence, the potential for just a few percent was seen on all samples, but could not be of the " fixed" contamination freeing itself - correlated to any specific envimnmental to become " removable" contamination condition. It appeared that time and would account for the enormous potential changing environmental conditions were all for " weeping "
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_y - . . . .. , , 4 Li j h Work then continued to attempt to determine - never occur. The magnitude of the ; how to remove this fixed contamination, contamination is only of the order of one a J ~ These " cleaning" methods are still being radioactive ion per 100,000 surface metal ' g investigated, but the preliminary conclusion - atoms, and appears to reach saturation at - ;
. is that there is no commercially acceptable - this level. IIence, it is being assumed that ;
method of successful removal Future work the actual interactions with the surface : ;) will address methods of passivating the atoms must involve dislocations or other M surface so that the contamination might rare aberrations on the surface. "" ! 10 > J
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- i. o'l three days of vanout, environmental testing. - The ordinate represents the ratio of the swipe on the given day to ;
l' that on the previous day, correcting for the efficiency of the swipe method and the actual amount of . j contaminaten removed by the first swipe. No weeplng would be represented by a 1.0 ratio. A ratio less than 1.0 : ' indcates eitner a fixing of removable contamination, a loss of some removable contamination, or merely 'i Stat 1SttCal Varlations if) the measurement. Values greatet than 1.0 (by far the predominant situation) impliet -~ either weeping or statistical variations. . ~f 7 y
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USING THE CODE RELAP FOR SAFETY ANALYSIS OF RESEARCH R$ ACTORS
- William Chao, Jay Kunze, Sudarshan Loyalka, Weimin Dai GIU Nuclear Engineering), Rol'and Hultsch, J. Charles McKibben, and Olawale Oladiran GIURR)
The loss of coolant accident (LOCA) in an When initially conducting the benchmark operating reactor is a most unlikely event, test, it was found that degassing of the yet one of the most severe safety concerns. dissolved gas in the water resulted in This involves a major leak that results in enhanced heat transfer at much lower sufficient loss of coolant that the removal temperatures than where nucleate boiling of shutdown (decay) heat from the core is would be e7pected to occur. Hence, enhanced compromised. The credible event that heat transfer resulted compared to code would initiate such an event is a major predictions. .The issue of degassified water is earthquake that would result in relative real for these research reactors, for most movement of plant components sunicient operate at several atmospheres pressure. In to rupture an inlet or outlet pipe to the the case of MURR, the solubility of the water . a core vessel. for air at operating temperature and pressure l is several times higher than for the fill - ;! The RELAP thermalhydraulics time conditions at room temperature and .l dependent computer code is one tool for atmospheric pressure. Yet during a LOCA, j analysis of a LOCA. The code boiling temperatures will be reached quickly, .! development was sponsored by both the preceded by complete degassing of the water Department of Energy and the Nuclear moving through the fuel plates. The effect is Regulatory Commission, and has been one of enhanced heat removal capability - certified by the NRC for analysis of LOCA initially, compared to what is predicted by ,
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for most of the commercial nuclear RELAP. There is also some resistance to the > clectric power generating plants. The flow reversal that occurs, resulting in upward ' code has not been tested through natural convection flow, but this is a much experiments on the quite different smaller overall effect on peak temperature conditions of research reactors, which than is the enhanced heat transfer. nonnally operate at near atmospheric pressure and temperatures generally well Comparisons between RELAP and a 1 below 100 C. benchmark experiment involving a single channel (with the same width as between R When the code was apphed to the LOCA MURR fuel plates) are shown in Figure 1.
- analysis of MURR, the results for the RELAP currently has no way of accounting targeted 30 MW operating level for the for the degassing, hence underpredicts the proposed upgraded reactor power , heat removal and overestimates the peak j indicated that fuel temperatures would cladding temperature. Furthermore,it even I approach within a few hundred degrees F under-estimates the heat transfer in single -
of the level that would result in cladding phase laminar flow. However, once true damage. Because the code had never boiling commences and dissolved gas is no - been " benchmark tested" under similar longer present, the RELAP code appears to conditions,it was proposed that an give an accurate prediction of temperature ; changes, even under those of pulsed boiling in appropriate benchmark experiment be conducted to check the code. This work the narrow fuel element channels. The - .- has been sponsored by DOE during the pinblem with laminar flow conditions is' l last three years, since concerns similar to somewhat under the input control of the user, .; MURR's were found for the high power since difTerent hydraulic diameter may be ; test reactors owned by DOE. selected. However, the incorporating of - j i 100 1 i
dissolved gas effects would require fuel temperatures for the LOCA at l computer code source program changes. MURR. Work is continuing on a The answer to the initial concerns about related project in attempts to find a I the safety analysis results is that RELAP way of encoding the dissolved gases . had significantly overpredicted the peak into the RELAP computer code. , 39; f 380 - g HEAT BLK-RELAP +' 37C - 23s0 .-
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TIME DEPENDENT FLUX CHANGES IN MURR - Mohammed Salih, Jay Kunze (MU Nuclear Engineering) and Kiratadas Kutikkad
-(MURR) l The MURR is a mactor with a substantially accident (LOCA). At such a time much different neatmn energy spectrum in the occurs in the first second, including a reflector ccmpared to that in the core, rapid change in the flux levels and flu 2 and the central flux trap also provides distribution thmughout the reactor.
significar.t diffemnces. The prompt The critical period for heat removal neutron iifetime differs substantially from the fuel plates is the moment that between these parts of the reactor. flow stops and reversal oomrs to the Though several related studies and. upward convective flow directbn._ This measnrements had been made on MURR happens within the first two se ends. arourid 1970(two PhD dissertation topics), the results were largely These studies of the flux distribution incenclusive concerning the ability of' changes in short time periods existing computer codes to analyze following rapid contiol rod insertion adequately neutron flux and power are being reexamined using newer or , changes with time during rapid positive more applicable computer codes than . er negative transients. were available in the 1970 studies. Where appropriate, the results will ; ; This question is being reexamined replace the use of point kinetics . i because of the issues related to .chutdmyn analysis for evaluating safety heat removal following a loss of coolant characteristics of MURR. REACTOR PLANT OPERATION DISPLAY SYSTEM and NUCLEAR PLANT RADIOLOGICAL DISPLAY SYSTEM Mohammed Enani, Jay Kunze (MU Nuclear Engineering) and Kiratadas Kutikkad ; (MURR) 1 Modern computer systems can provide considered necessary (for safety and cost - most helpful graphical displays of reasons), the advantages in case of conditions of a complex operating system unders.tanding current conditions and for such as a reactor. These systems can also providing simulator training are be used as training simulators to significant, albeit somewhat intangible, represent hypothetical emergency benefits. response conditions for a 1 operating reactor plant (or of other complex Attempts to program such useful systems). Incorporation of graphical graphical display and analysis systems displays and simulators for operator are now underway, primarily as_ a training has not beenimplemented at r,tudent research project. .One generally MURR to the extent that it has at the new developmental application will be . commercial power reactors throughout to use a nodal core analysis method to-the US. Although the implementation of ' display fuel reloading effects, such as these systems on MURR- may not be power distribution. 102
F [": EXPERT SYSTEM FOR THE MURR CONTROL ROOM i Gin-Weigh Wu and Jay F. Kunze (MU Nuclear Engineering), Kiratadas Kutikkad and Walt Meyer (MURR) Modern computer technology, especially desktop microcomputers, permit the fast - accumulation of many data points, storage of these to a hard disk, and on-line evaluation of trends in these data points. This application is designated an expert system,"i.e., a computer monitor of a complex operational system, providing on-line evaluation according to an engineer-supplied analytical method. Such a - system would not substitute for an operator, but would nlert the operator to development of off-normal conditions. With the vast number of data points to be monitored, the computer expert system can pracess much more data than can the operator's eyes and brain, and can analyce more readily these data for trends and subtle changes, usually alerting the operator to them long before a conventional trip set point would give an alarm. Only recently such systems are being applied to co:nmercial power reactors, where there are hundreds ofimportant data channels, any one of which might give an indication of potential plant shutdown. A brief shutdown of a 1200 MW(e) commercial nuclear power plant is costly, typically requiring purchase of about $1 million of replacement power. A brief shutdown at MURR is not nearly as expensive, but costly nevertheless in terms ofirradiation and experiment interruptions, and stress on plant components. An expert system is planned for installation in the Control Room at MURR. The connections to the control system must guarantee that the computer can provide no - feedback signal into the control system, and in no way affect the control system readings or response. The several dozen channels being monitored must be recorded at a rapid rate, at least once a second, and as much as 1000 times per second for some, so that Fourier snalysis of the signal can be performed. The data acquisition system now being a.~embled has a capability of 20,000 data points per [ second, and the computer to manipulate the data will have a capability of about 10 l MIPS (million instructions per second). Installation in or adjacent to the Control Room is anticipated in spring 1993 103
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' NON-DESTRUCTIVE EVA'LUATION GROUP _; t e PERSONNEL William H. Miller, 3roup Leader, Professor of Nuclear Engineering, Director of _ j Energy Systems and Resources Program ; Kiratadas Kutikkad, Research Scientist (Adjunct Assistant Professor, Nuclear , Engineering) ; The non-destructive evaluation group is a portion of the Nuclear Engineering program at the MURR Center. It encompasses a variety ofexperimental techniques
-other than neutron scattering techniques-which can be used for non-destructive ;
analysis. Current projects include: 1) the measurement of hydrogen content in , 1 materials ofinterest; 2) the relocation of the prompt neutron activation analysis facility; 3) the development of a depth profiling facility _; and 4) maintenance and ; utilization of the filtered beams on beamport F. With respect to hydrogen measurements, the modified notthed neutron spectrum ., technique has been refined to give an experimental uncerminty of 0.4 weight ppm in metals, or an absolute mass sensitivity ofless than 10 micrograms. The technique has now been applied to the measurement of hydrogen in steel, in Ti/Al alloys and in porous silicon. Work has been proposed to measure deuterium in metals (in suppor; of neutron scattering work) and water in archaeological samples. The prompt neutron activation m.nlysis facility has been remove 1 hom beamport A in preparation for the installation ofTRIAx there. Work is now mW arway to place this facility behind the scattering experiments on beamport D. The designs of l several other PGNAA facilities have been obtained from'other institutions in order to optimize the new design. Improvements in shielding design and detector placement are expected to provide modest improvements in sensitivity compared to the previous system. This new facility is also being designed to allow the addition of a depth profiling facility in the future. b r 105
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j I A DSP-BASED, SMART ANALOG-TO-DIGITAL CONVERTOR FOR NUCLEAR RADIATION 1 DETECTORS William H. Miller (MU Nuclear Engineering and MURR) and Ron R. Berliner (MURR) An innovative, digital signal Prog as to date includes the processor (DSP) based system is development of a wire-wrap, being developed for analyzing and prototype circuit that accepts pulses processing pulses produced by from the detector, triggers ADC - radiation detectors. This system conversion based upon a digital will provide more accurate analysis threshold, stores the result in a first of pulses from all radiation in, first out (FIFO) buffer, and spectroscopy systems including provides an interface to a computer those used for health physics for data transfer and ultimate data instrumentation, environmental analysis. This system is currently monitoring, and personnel running at a 10 MHz sampling rate monitoring. It is designed to and is shown in Figure 1. It is being replace pulse-type, Wilkenson and prepared for implementation on a successive approximation analog- printed circuit board. to-digital convertors (ADCs) that are currently used for pulse height Software development has also been analysis of detector pulses. Energy initiated. Cross-correlation information will be derived by functions for pulse shape digital integration of the detector discrimination have been tested in pulse, leading to a more accurate both D8P and 486 PL t.. honments. result. In addition, a DSP-based These fuactions provide excellent system will be capable of advanced pulse shape discrimination features (e.g., pulse validation, capabilities. Preliminary tests also pulse shape analysis, dynamic suggest that a combined pulse threshold determination, and noise height and pulse shape analysis can reduction) while using fewer and be performed at rates of10,000 simpler electronics for increased counts per second, which is reliability, reduced electronic noise adequate for most detector and less expense. applications. 106
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THE MODIFIED NOTCHED NEUTRON SPECTRUM TECHNIQUE FOR THE DETERMINATION OF HYDROGEN William IL Miller (MU Nuclear Engineering and MURR) The non-destructive determination of Several different types ofsamples - hydrogen content is important tp many containing hydrogen have been studied different disciplines. Unfortunately, using this new technique. Figure I shows techniques that accurately and typical data for hydrogen in steel. As can be nondestructively measure hydmgen content seen, accurate results below 1.0 wppm are at parts-per-million (ppm) levels have not possible. Samples ofTi/Al alloy have been been readily available. One possible loaded with large amounts of hydrogen (on : hydrogen measuring technique is the the order of 2% hydrogen by weight or :
- modified notched neutron spectrum 20,000 wppm) and measured. Experimental technique" that has been developed on measurements have been compared with beamport F at MURR. It is based upon a hydrogen weight gain measurements and technique that was suggested approximately the results have agreed to within 4%. It was ;
25 years ago and is currently in use at also found that the technique is linear over i EG&G Idabo, but has been refined here at the range from 20,000 wppm (for Ti/Al) to ; MURR to ivrease the sensitivity by 0.6 wppm (for steel). Finally, hydrogen .{ approximately a factor of 20. The resu! ting content in porous silicon has been measured sensitivity is 0.4 weight-parts-per-million at concentrations down to 40 micrograms. (wppm) of hydrogen in metals, or an q absolute sensitivity of 10 micrograms. This technique has utility for a wide variety of applications in which the amount of , The notched neutron spectrum technique hydrogen content must be determined. The uses a filtered spectrum that has been measurement process is straightforward, is , depleted of neutrons in the epithermal nondestructive, can be applied to radioactive energy range by absorption at resonances. samples, and provides a new analytical tool i The technique then measures the extent to for determining hydrogen content. which these resonance regions are repopulated by moderation of the neutrons through hydrogen scattering interactions. , By improving the geometry of activation foils that detect this moderation, the "Si ~ sensitivity of the technique is greatly DS45' d* ----
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UNIVERSITY REACTOR SHARING-The US Department of Energy has provided financial support for MURR's Reactor Sharing Program since 1980. During the annual reporting period completed early _ ' in FY92 DOE provided $73,000 to support the program and MURR has matched this ' with $33,507. DOE started this program to provide increased availability of. university nuclear reactor facilities to non-reactor-owning colleges and universities ' (user institutions). MURR, with our unique facility, also provides support to institutions with research reactors that do not have the capabilities to perform the required experiments. In FY92,39 research projects invohring 99 faculty and 41 students at the 31 institutions listed below were supported: Arizona State University University of Arkansas Auburn University University of California-Berkeley Cal State University-Fullerton University of California-Los Angeles Dartmouth College University of Chicago Franklin and Marshall College University of Cincinnati , Harvard University University of Conneticut Iowa State University University of Hawaii Johns Hopk. ins University University of Kentucky , Louisiana State University University of Massachusetts New Mexico Institute of Mining & University of Medicine and Dentistry of - , Technology New Jersey Oregon State University University of North Dakota Princeton University University of Rochester Purdue Univer sty Utah State University Ripon College Vanderbilt University Stephens College Washington University (St. Louis, MO) University of Arizona i Projects involved work in many fields including anthropology, archaeology, animal science, analytical epidemiology-nutrition, crystallography, geology, materials science, physics, cosmo-chemistry, biochemistry-nutrition, nuclear analysis , development, genetics and human nutrition. A list of some of the publications , resulting from Reactor Sharing projects at MURR follows. ; p b 111 , I
= ^
L PUBLICATIONS RESULTING FROM REACTOR SHARING PROJECTS Davis, A.M.; MacPherson, G.J.; Clayton, R.N.; Mayeda, T,K.; Sylvester, P.J.; Grossman, L.; Hinton, R.W.; Laughlin, J.R., Melt Solidification and Late-Stage Evaporation in the Evolution of a FUN Inclusion from the Vigarano C,V Chondrite, Geochimica et Cosmochimica Acta (submitted) Haas, J.R.; Haskin, L.A., Compositional Variations Among Whole-Rock Fragments of the LG Chondrite Bruderheim, Meteoritics (submitted) Korotev, R.L., Geochemical Stratigraphy of Two Regolith Cores from the Central Highlands of - the Moon, Proceedings of Twenty.First Lunar and Planetary Science Conference, Lunar and Planetary Institute, Houston, TX, March 12-16,1990 (submitted) Owens, B.E.; Dymek, R.F., Fe-Ti-P-Rich Rocks and Massif Anorthosite: Problems of , Interpretation Illustrated from the Labrieville and St. Urbain Plutons, Quebec, Contributions to Mineralogy and Petrology (submitted) Owens, B.E.; Dymek, R.F., Petrological Constraints on the Origin of Anorthosite of Extreme Composition: The Labrieville Massif (LBV), Quebec, Journal of Geology (submitted) P Shelton, M.E.; Green, M.A.; Mathias, C.J.; Welch, M.J.; Bergmann, S.R.; James, ILL.; Weinheimer, C.J., Assessment of Regional Myocardial and Renal Blood Flow Using Copper-PTSM and Positron Emission Tomography, Circulation (submitted) Smith, M.S.; Dymek, R.F.; Chadwick, B., Petrogenesis of Archaen Malene Supracrustal Rocks, NW BukseCordfen Region, West Greenland: Geochemical Evidence for Highly Evolved , Archaean Crust, Precambrian Resea.rch (submitted) Smith, M.S.; Dymek, R.F.; Schneiderman, J.S., Implications of Trace Element Geochemistry for the Origin of Cordierite-Anthophyllite Rocks from Orijarvi, SW Finland, Journal of Geology .1 (submitted) ! 1 Sylvester, P.J.; Ward, B.J.; Grossman, L., Chemical Compositions of Siderophile Element-Rich J Opaque Assemblages in an Allende Inclusion, Geochimica et Cosmochimica Acta (submitted) Wang, M-S.; Lipschutz, M.E., Consortium Study of MacAlpine Hills 88105 Lunar Meteorite, Geochimica et Cosmochimica Acta (in preparation) Windsom, K.E.; Seifert, K.E.; Anderson, R.R., Studies of the Precambrian Geology ofIowa: Part
- 1. The Otter Creek Layered Igneous Complex, Journal ofIowa Academy o/ Science 98(4),
170(1991) Windsom, K.E.; Seifert, K.E.; Anderson, R.R., Studies of the Precambrian Geology ofIowa: Part
- 2. The Matlock Keratophyre, Journal ofIowa Academy ofScience 98(4),178 (1991) 112
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NSF RESEARCH. EXPERIENCES FOR UNDERGRADUATES ATMURR L For the fourth consecutive year, MURR was selected by the National Science Foundation (NSF) as a site for a summer *Research Experience for Undergraduates" program, Eleven studenta representing seven universities participated and seventeen MU faculty and Reactor Center staffserved as mentors to provide research guidance and consultation for the students. Each student worked with one or two mentors to design and. carry out an individual research project. In addition, a dozen other faculty and reactor staffmembers joined the mentors in providing 35 hours oflecture/ discussion / training sessions for the students. MURR has now trained 44 future scientists in " Scientific Applications involving Neutrons
- under the sponsorship of the NSF. The program is -
currently funded for three years and will be offered again during the summers of1993 and 1994. Alist ofstudent : projects is given at the end of this section. Although copper is known to be an essential 1(b). The Cu-64 binding by certain pmteins trace element, a recommended daily was reduwd by preincubation with zinc, allowance of this elementis yet to be particularly superoxide dismutase (F3). This. , determined. Copper is bound to many technique was developed for studying copper- . important enzymes, and transport pmtcins binding proteins using high specific activity Cu- { are involved in binding this trace element and 64, and it appears to offer many advantages in - a facilitating absorption. Maggie Stammeyer the investigation of copper metabolism. undertook a project to study the binding of copper to pmicins. She worked to develop a Neutron diffraction can be used to obtain 1 model system to study how various information about the arrangement of parameters affect the binding of copper to mokcules on surfaces and about changes which known proteins, so that unknown copper- may occur during heating or cooling of the binding protein; could be characterized. The surface. Douglas Seman used a computer parameters investigated included pH, buffers, modeling method calkd molecular dynamics to i reducing agents, and the influence of other predict the behavior of n-propanol molecules absorbed on a graphite surface (Figure 2). As - O trace elements such as zine and iron on copperbinding. Known proteins (24)were with the shorter alcohols studied previously, blotted to nitrocellulose with a slot-blot hydrogen-bonding ithe affinity of a hydroxyl ; apparatus, subjected to varied conditions, hydrogen atom on one molecule for the oxygen ; probed with high specific activity Cu-64 (300 atom of another mokscule) appears to be the Ci/mg Cu), and autoradiographed. The dominant interactionin the system. The , results of one study are shown in Figure 1. molecular dynamics method uses the computer The binding of Cu-64 was protein depemdent, to generate all possible atom motions for a ! with greatest binding by carbonic anhydrase given strength ofmolecule-surface and - i (D1) and metallothionein (G2). Preincubation mok cule-mokeule interactions. When the . i with nonradioactive copper reduced Cu-64 model correctly predicts the behavior of the ; binding by all proteins, as indicated in Figure surface layer of atoms (i.e., the properties agree Fig.1 Scans of 3 autoradio-graphs. Figure 1(a)is the ;;
~ .,,, ; control, with no additional j e l = .' " "
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l 8 b c 115
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The ellipses are drawn to 3-y A S,% e( g% 8e) a4 illustrate the m cu ar 8' backbone in a space filling g ydr > sible for . h t d$rg hk a 9&sth Dh 9 79 /> h u a a a 4 6 a a a . x with thc se > ,ed from neutron scattering measurements), the intermolecular forces have been - adequately u .ribed. The model can then predict other properties of surface layers and properties of bulk (3-dimensional) solids and liquids which are not easily accessible by experimental methods. When silicon is used as an anode in an electrolytic cell with an HF solution as the ekdrolyte, a chemical reaction occurs on the surface of the silicon. The resulting y, material, apparently a residual skeleton . . _ from partial dissolution of the silicon, exhibits substantially altered physical and ; chemical properties. This " porous silicon" is obviously altered in color, it exhibita % '$ photoluminescence and it promises to have h-interesting electrical, chemical and $ quantum properties. David Gilliam's summer project was to synthesize porous (c) silicon and to use neutron and X-ray
~
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diffraction techniques to gain information about its structure. The results of David's difTraction experiments (Figure 3) show that porous silicon has lost most of the on
" L d- ; '
long-range structural order that the ' original material possessed and has < e e e e e e
- e ' '
incorporated substantial amounts of Angle (tw 4heta) hydrogen. Further studies to investigate Fig 3 Drftraction pattems of silicon powder for neutrons (a) and X-
. . rays (d) compared with porous sibcon diffracton of neutrons the catalytic properties orporous silic<m ,33 on, x4,y, <c3 rno ,,, n,,n.,ng,, p ,x, ,n ,33 ,,,,,,
are planned. from scattenng by boron nitride in the sample cem 116
Dale Witte's project called for
. engineering design and data analysis skills to be applied to residual stress measurements of welds in the Advanced Solid Rocket - ,. 7 rm %,,,,,,
Motor for the NASA space shuttle. "'*""** b oW ' ~ The Electronic and Mechanical - -.- ~ %f;M "/ l Properties group at MURR is . .- g, '. . studying a scaled-down model of one of the cylindrical sections L9. which will be welded together to make the musable rocket motor. Fi.i";'. N Recovery of the motor from the ocean for reuse is feasible onlyif n.va-.o , the problem of stress corrosion - m.,, N'""**"" cracking (initiated by chemical reaction of stressed steel with salts , , , , , , in ocean water) can be eliminated. The actual cylinder sections (12 fl. diameter by 10 ft tall,0.6" thick high-strength steel) were far too large to be handled and the 230 F,g. 4 sample volume studied by pound model(3 ft diameter by 1 ft n..i collimated neutron beams tall- also 0.6" thick) presented difliculties as well. Dale worked with several engineering professionals to program a computerized robot arm assembly ROW A which held the heavy modelin precise orientations in a small := , , , beam of neutrons from the reactor (Figure 4). Diffraction fmm the beam was analyzed to determine stresses at various points in the 3. . vicinity of the weld. Calculation of {
~
j o ""* the stress tensor at each point a required investigation from atleast $ , six different directions using a g , diffractometer designed to work with much smaller samples. Dale's [ calculations permitted the group to make the necessary measurements for accurate stress determinations o a 4 e e 5e sa 5a (Figure 5). The model will be heat-treated and remeasured to verify DEPfH (mm) that stresses associated with the rig. s variavons of stresses with dopin in sampie. welding process have been Note that radial stresses are relatrvely constant removed. Dale also helped analyze but anal and hoop stresses change sharpfy between 6 and 8 mm in depth. a flat plate model of the weld and developed computer programs to aid in data analysis. 117
1992 Summer REU Program : Student Projects Patience Bennett (MU Electrical and Computer Engineering),
- Automation of a Sample Changer for a Neutron Beam Hydrogen Spectrometer" Mentor - Dr. W. Miller, MU Nuclear Engineering Janice Bequette (Central Missouri State University industrial Safe'y), "An inventory of .;
Potentially Hazardous Chemicals at MURR" Mentor - Dr. S. Langhorst, MURR Hoalth Physics Albert Crook (St. Louis University Math and Physics), " Computer Simulation of Electrochemical Concentration Gradients" Mentors - Dr. T. Storvik (MU Chomical . Engineering) and Dr. L. Krueger, MURR Actinide Chemistry Group David Gilliam (Lincoln University Physics and Math), 'StructuralMeasurements of Porous Silicon with Neutron Di//raction" Mentor - Dr. B. Heuser, MURR Nanostructures and Excitations Group q Joseph Kim (Northwestem University Chemistry), " Toenails as an indicator of Arsenic and Selenium in Humans - Determination by Neutron Activation Analysis" Mentor - Dr. J.S. Morris, MURR Nuclear Analysis Program Kent Riley (University of Michigan Nuclear Engineering),
- Development of a Remote Processing Technique for Radiopharmaceutical Production" Mentors - Dr. A. Ketring and Dr. G. Ehrhardt, MURR Radiopharmaceutical Group Doug Seman (University of Michigan Engineering and Physics), "A Study of Molecular Dynamics of n-propanol Physiosorbed on Graphite using Computer Simulation" Mentor -
Dr. K. Herwig, MURR Nanostructures and Excitations Group . Maggie Stammeyer (MU Chemical Engineering), *A Procedure for the Study of Trace Metal l Binding to Proteins using High Specific Activity Cu-64" Mentors - Dr. T. Chaudhurl and Dr. K. Zinn, MURR Analytic Epidemiology, Nutrition and Immunology Group David Walters (University of Maryland Chemistry), " Chemical Characterization of Obsidian Sources in the American Southwest and Northem Maxico" Mentors - Dr. M. Gfascock and Dr. H. Neff, MURR Nuclear Archaeometry and Geochemistry Group Dale Witte (MU Mechanical & Aerospace Engineering), " Characterization of Residual
~
Stresses in a Sub-scale Cylinder of the Advanced Solid Rocket Motor" Mentors'- Dr. A. Krawitz and Dr. A. Winholtz, MU Mechanical & Aerospace Engineering and MURR Electronic and Mechanical Properties Group Kim Wood 2 (MU Electrical Engineering),
- Automation and Controlof a 4-circle Neutron Diffractometer" Mentors - Dr. H. Yasar and Dr. F. Ross, MURR Magnetic and Crystal Structures Group 118
2 i COURSE LECTURES AND LABS PRESENTED BY FULL-TIME STAFF July 1991 June 1992 DATE LECTURER COURSE TITLE AND SUBJECT OF LECTURE - 07/91 R. Berliner NSF REU: Neutron Powder Diffraction - 07/91 T. Chaudhuri NSF REU: New Radiotherapies for Cancer Treatment 07/91 T. Chaudhuri NSF REU: Areas of Fundamentals Related to Monoclonal Antibodies in Nuclear Medicine and Role of Surface Antigens in the Detection and Treatment of Ovarian and Other Cancers , 1 07/91 G.J. Ehrhan dt NSF REU: Radioisotope Generators NSF REU: Use of -Emitting Microspheres in Radiotherapy 07/91 G.J. Ehrhardt 07/91 J.W. Farmer NSF REU: Radiation and Defects in Solids 07/91 M.D. Glascock NSF REU: Nuclear Analysis Methods 07/91 B.J. Heuser NSF REU: Small Angle Neutron Scattering 07/91 H. Kaiser NSF REU: Neutron Interferometry i 07/91 A.R. Ketring NSF REU: Radiopharmaceutical Chemistry 07/91 C.L. Krueger NSF REU: Actinide Research at the MURR 07/91 J.S. Morris Columbia College, Introduction to Radiochemistry: Fundamentals of Radiochemistry 07/91 J.S. Morris NSF REU: Nuclear Applications in the Life Sciences 07/91 J.S. Morris Missouri Scholars Academy Laboratory: NAA Laboratory , V.L. Spate M.M. Mason C.K. Baskett C.L. Reams 07/91 H. Neff NSF REU: Nuclear Archaeology 07/91 F.K. Ross NSF REU: Introduc* ion to Neutron Scattering 07/91 W.B. Yelon NSF REU: Introduction to Gamma-Ray Scattering i 119- f
i COURSE LECTURES AND LABS l DATE LECTURER COURSE TITLE AND SUBJECT OF LECTURE - 07/91 K.R. Zinn NSF REU: Isotope Applications in Biochemistry and Nutrition 4 08/91 J.J. Rhyne - NSF REU. Magnetism and Neutron Scattering 08/91 G.J. Ehrhardt Chem 429, Nuclear Medicine and Radiology: Accelerator Production of Radioisotopes i 09/91 G.J. Ehrhardt Chem 429, Nuclear Medicine and Radiology: Particle i Accelerators and Nuclear Reactions Using Charged Particles r 09/91 G.J. Ehrhardt Chem 429, Nuclear Medicine and Radiology: Radioisotope - Generators 10/91 G.J. Ehrhardt Chem 429, Nuclear Medicine and Radiology: Nuclear Medicine Applications of' Jioactive Microspheres 10/91 A.D. Krawit.z Stephens College, History of Western Art I: Scientific Methodsin : Art History 10/91 K.R. Zinn Biochemistry 410, Seminar: Identification and Comparisons of ' Selenoproteins in Rat Brain and Mouse Neuroblastoma Cells , 11/91 M.D. Glascock NE 409, Interactions of Radiation with Matter: Instruction on Neutron Activation Analysis ; 12/91 J.S. Morris Chem 312 InstrumentalMethods ofAnalysis: Instrumental Analysis 01/92 J.R. Schuh NE 404, Reactor Lab: Indoctrination and General Health Physics' .; 02/92 G.J. Ehrhardt NE 406, Clinical Research and Applied Medical Physics: Radiotherapeutic Nuclear Medicine Research at MURR -i 02/92 M.D. Glascock NE 404, Reactor Lab: Neutron Activation Analysis ~' 02/92 M.D. Glascock Anthro 349, Artifacts and Data Analysis: Nuclear Techniquee ; Applied to the Study of Archaeological Materials ! 02/92 J.R. Schuh NE 471, Radiation Protection: Indoctrination and General Health l Physics i r 120
PRESENTED BY FULL-TIME STAFF DATE LECTURER - COURSE 11TLE AND SUBJECT OF LECTURE 03/92 W.A. Meyer NE 404, Reactor Lab: Reactivity Measurements , A.R. Schoone N.E. Tritschler 03/92 J.S. Morris Lincoln U, NAA Laboratory: Instrumental Analysis 03/92 J.S. Morris Chem 361, Introduction to Radiochemistry: Introduction to
- Radiochemistry 03/92 J.S. Morris Central Missouri State U, Chem 390: Instrumental NAA 03/92 H. NefT Anthro 349, Artifacts and Data Analysis: Compositional Analysis of Pottery 04/92 J.S. Morris Che n 12, General Chemistry: Nuclear Analysis 04/92 K.R. Zinn Biochemistry 410, Seminar: Selenium Metabolism in the Brain 96/92 T. Chaudhuri NSF REU: New Radiotherapies for Cancer Treatment OW92 S.L. Gunn NSF REU: Industri: ' '.!tilization of Research Reactors 06/92 M.D. Glascock NSF REU: NAA to Source Archaeological Obsidian OW92 M.D. Glascock NSF REU: Isotopes and Radiation, Neutrons and Nuclear i Reactions 06/92 K. Kutikkad NSF REU: Fission and Nuclear Reactors 06/92 S.M. Langhorst NSF REU: General Radiation Safety 06/92 W.A. Meyer Jr NSF REU: MURR: Past and Future ,
06/92 J.S. Morris NSF REU: Radioactive Decay, NAA, Gamma-Ray Spectroscopy 06/92 G.K. Moum NSF REU: The MURR Computer Network t 06/92 A.R. Schoone NSF REU: MURR Today 06/92 K.R. Zinn NSF REU: Radionuclides in Biochemistry 121
COURSES AND LABS TAUGHT i STAFF MEMBER COURSE TITLE AND NUMBER R.M. Brugger NE 403, Applied Topics in MP/ IIP (s) a) J.F. Kunze ' i J.W. Farmer ECE 124, Circuit Theory I (O l R.A. Hultsch Columbia College Physics (O A.D. Krawitz MAE 344, Composite Materials (w) J.F. Kunze NE 315, Energy Systems & Resources (w) NE 409, Interaction of Radiation with Matter (O > NE 435, Physics Diagnostics Radiology 1 (O J.F. Kunze NE 471, Radiation Protection (w) S.M. Langhorst , J.F. Kunze NE 403, Applied Topics in MP/ IIP (D W.H. Miller P.K. Lee S.M. Langhorst K. Kutikkad NE 402. Nuclear Fuel Cycle (w) - J.F. Kunze t S.K. Loyalka NE 411, Nuclear Reactor Theory 1 (w) NE 432, Nuclear Thermalhydraulics/ Safety (O W.H. Miller NE 346, Introduction to Nuclear Reactor Engineering I (O NE 391, Nuclear Radiation Detection (O NE 421, Nuclear Pulse Analysis (w) i NE 429, Radiation Dwimetry(w) W.H. Miller NE 301, Nuclear Science and Engineering for Secondary S.M. Langhorst Teachers (s) i 122 1
BY MURR STAFF AND RESEARCH INVESTIGATORS STAFF MEMBER COURSE TITLE AND NUMBER J.J. Rhyne Physics 478, Magnetism and Magnetic Materials (w) S.A. Werner E.O. Schlemper Chem 401, Introduction to X-Ray Diffraction (s) F.R Ross C.L. Barnes G. Schupp Physics 176, University Physics (O Physics 450, Research (s) Physics 450, Research (O E.O. Schlemper Chemistry 12, General Chemistry (O Chemistry 12, General Chemistry (w) P.R. Sharp Chemistry 12, General Chemistry (w) Chemistry 411, Dragonmetallies (O i H.Taub Physics 312, Introduction to Thermodynamics (w) Physics 314, Mechanics (O W.A. Volkert NE 328. Introduction to Radiation Biology (O W.A. Volkert Radiology 400, Radiopharmaceutical Chemistry (w) 1 A.R. Ketring G.J. Ehrhardt KV. Katti ; S. Jurisson R.A. Winholtz MAE 224, Engineering Materials I (O MAE 224. Engineering Materials I(w) l S.A. Werner Physics 176, University Physics (D , Physics 450, Research (s) Physics 450, Research (O i 123
9 l DEGREES COMPLETED . STUDENT DEGREE ADVISORS / COMMITTEE DATE DEPARTMENT MEMBERS THESIS University of Missouri System K-Y. Cheng MS R.M. Brugger A Study of New Seeds for December 1991 NE Medical Physics G.J. Ehrhardt Brachy Therapy ; S.M. Langhorst . W. Dai MS J.F. Kunze - Dissolved Air Effects in 4 May 1992 Nuclear S.K. Loyalka Narrow Vertical Channels ( Engineering R.A. Hultsch Experimental Verification . :!
, Related to MURR W. Jia MS E.O. Schlemper A Study of Rhenium .
December 1991 Chemistry G.J. Ehrhardt Labeled HSA Microspheres , K.R. Zinn as a Radiation Synovectomy
' Agent L.Lang PhD D.E. Troutner Radiolabeling Proteins _ j May 1992 Chemistry E.O. Schlemper with Bifunctional R.N. Loeppky Chelating Agents -
S. Jurisson - .; J.S. Morris W.A. Volkert i M. McNally MS T.S. Storvick Preliminary Process > May 1992 Chemical Engineering D.G. Retzloff Design for Pyrochemical- # P.R. Sharp Processing of Purex Waste - l J.D. Nurrenbern MS J.F. Kunze Investigation of i December 1991 NE Medical Physics W.H. Miller Radionuclide Release i P.K. Lee from Shipping Cask Surfaces ! L. Pellett PhD- D.T. Gordon The Interaction Between - December 1991 Food Science K.R. Zinn Dietary Iron and Copper R.A. Sunde and Nutrition Affecting R. Dowdy Ceruloplasmin Metabolism, T. Veum Cu-67 Retention, and - Macrophage Product;on of O, and H,0,
.124
s I BY MURR RESEARCH STUDENTS t l. l-
- STUDENT DEGREE ADVISORS / COMMITTEE DATE DEPARTMENT MEMBERS THESIS
'I K.J. Riggle PhD W.H. Miller Environmental Monitoring May 1992 Nuclear J.S. Morris for U and Np Using ENAA Engineering M.D. Glascock S-K.C. Wang PhD H.Taub Diffraction Studies of the .i May 1992 Physics H. White - Multilayer Structure of. ;
F.K. Ross Simple Physisorbed Films ; S. Satpathy ; M. Greenlief J. White MS D.E. Day Properties and December 1991 Ceramic Engineering, R.F. Brown Manufacturing Techniques , UMR G.J. Ehrhardt of Human Serum Albumin Microspheres Other Universities C.L. Chen PhD P.D. Whanger The Effect of Vitamin B y August 1931 Toxicology K.R. Zinn on Selenium and Arsenic Oregon State U Metabolism B. Saini-Eidukat PhD P. Weiblen Platinum Group Elements December 1991 Geology and M.D. Glascock in Anorthositic Rocks of the Geophysics, Duluth Complex, University of Minnesota Minnesota: Petrogenetic and Economic Implications 125
g , E , GRADUATE STUDENTS FUNDED BY MURR ll 1 NAME POSITION CAMPUS / DEPARTMENT- ! Agarwal, S.R. Student Assistant Professional Computer Science Bahadori, D. Student Assistant Technical Electrical and Computer Engineering , Barnes, K.J. Graduate Research Assistant Physics and Astronomy Bradford, D. Graduate Research Assistant Physics and Astronomy Chao, W-W. Graduate Research Assistant Nuclear Engineering
?
Cheng, T-P. Graduate Research Assistant Chemistry [ Clothier, R. Post Doctoral Fellow Physics and Astronomy i Cogswell, J.W. Student Assistant Professional Anthropology Date, S.V. Graduate Research Assistant Radiochemistry i Ding, X. Graduate Research Assistant Physics and Astronomy ., Elam, J.M. Graduate Research Assistant Anthropology Greenfield, M.C. Student Assistant Technical Nuclear Engineering Greenwood S. Graduate Research Assistant UMR Materials Research
-?
Griflin Jr, J.L. Graduate Fellow Nuclear Engineering Gulati, P. Student Assistant Professional Computer Science Hamacher, K.A. Graduate Fellow Physics and Astronomy i Hayashida, F.M. Student Assistant Professional U of Michigan Anthmpology
~
Hirtz, G.J. '1 Student Assistant Professional Nuclear Engineering l Hoard, R.J. Student Assistant Professional Anthropology
]
Hu, Z. Graduate Fellow / Grad Res Asst Chemistry Isnard, O. Graduate Fellow U of Grenoble Physica/ Materials Science i Iyer,R.R. Graduate Research Assistant Computer Science Jia,W. Graduate Research Assistant Chemistry Jimene4 H.N. Graduate Research Assistant Chemistry l 126
1
-)
. July 1991-1992-NAME POSmON CAMPUS / DEPARTMENT -
Kulasekere, R. Graduate Research Assistant UMR Physics ' -, Kulasekere, K.C. Student Assistant Professional Nuclear Engineering Lai, C-J. Graduate Fellow Nuclear Engineering Lee, W-T. Graduate Fellow Physics and Astronomy Liang, Q. - Graduate Research Assistant Chemistry Ma, D. Graduate Fellow Chemistry r Mann, J.T. Student Assistant Professional Undeclared Manning, G. Graduate Research Assistant Physics and Astronomy McIntyre. A.L. Graduate Research Assistant UMR Materials Research , i Messmer, J.P. Student Assistant Technical Physics and Astronomy , Reams, C.L. Student Assistant Technical Political Science Rong,X. Graduate Research Assistant Nuclear Engineering Salem, J.D. Graduate Fellow Physics and Astronomy , Salih, M.S.A R. Graduate Research Assistant Nuclear Engineering Su,Z. Graduate Research Assistant Physics and Astronomy Tang, Y.Y. Graduate Research Assistant Physics and Astronomy -i Wagoner, R.A. Research Assistant Purdue U Physics Wang, M. Graduate Research Assistrmt Chemistry , Wang, N. Graduate Research Assistant Chemistry ; Winslow, N.A. Graduate Research Assistant Physics and Astronomy Wu, G.W. Graduate Research Assistant Nuclear Engineering i Wu, Z. Student Assistant Professional Nuclear Engineering Xie,II. Graduate Research Assistant Physics and Astronomy Yi.n,H. Student Assistant Professional Industrial Engineering i 127 l
UNDERGRAD~UATE STUDENTS FUNDED BY MURR NAME POSmON CAMPUS / DEPARTMENT r Adams, C.G. Student Assistant Technical ' Civil Engineering & Geological Sciences ; ' Bell, B.J. Student Assisttmt Professional Washington U Pre-Medicine Bennett, P.A. Student Assistant Professional Electrical and Computer Engineering . Bentley, R.L. Student Assistant Clerical Education Benton, T. Clerk Stephens College Business . Bequette, J.M. Student Assistant Technical Central Missouri State U Industrial Safety & Safety Management Biere, N.N. Student Assistant Clerical Psychology Billings, B.J. Student Assistant Service Central Missouri State U Animal ' Technology i Bormann, L.M. Student Assistant Professional Northeast Missouri State U Chemistry Brewer, M.D. Student Assistant Technical Geological Sciences < Condra, C.W. Student Assistant Technical Business and Public Administration Crook, A.G. Student Assistant Professional St. Louis U Math and Physics . Cruz, J. Student Assistant Technical General Studies
- Dinger, R. Student Assistant Technical Journalism Elwell, W.S. Student Assistant Technical Geological Sciences
- Eubank8,W.A. Student Assistant Technical Electrical and Computer Engineering Gazaway, T.L. Student Assistant Clerical Biological Sciences German, G.E. Student Assistant Technical Forestry, Fisheries and Wilflife Gilliam, D.L. Student Assistant Professional Lincoln U Physics / Math I Gottschalk, S.E. Student Assistant Technical Arts and Sciences Undeclared
^
Gross, J.B. Student Assistant Professional Loras College Chemistry Hakimi, N.M. Student Assistant Technical Undeclared Hayes, W.W. Student Assistant Technical Food Science and Nutrition Hilburn, D.N. Student Assistant Clerical Human and Envir(mmental Sciences Hinderks, B.A. Student Assistant Clerical Chemical Engineering Hinkebein, K.W. Electronics Tech 11 Law Hodges, S J. Student Assistant Professional Stephens College Math / Computer Science Hogan, C.S. Student Assistant Technical Mechanical and Aerospace Engineering Hosch, M.D. Student Assistant Professional Central College Physics Jalbuena, R. Student Assistant Technical Electrical Engineering Johnson, T.N. Student Assistant Professional Southeast Missouri State U Sociology / Anthropology Jokerst, S.F. Student Assistant Technical Electrical Engineering Khanna,V. Student Assistant Professional Computer Science ! 128
F July 1991-1992 ; .1 b NAME POSmON CAMPUS / DEPARTMENT 3 Kim,J. Student Assistant Professional Northwestern U Chemistry Kruessel, T.M. Student Assistant Clerical Psychology Lane, D.G. Student Assistant Technical Chemistry / Biological Sciences / History 3 La w, H-M.R. Student Assistant Technical - Physics and Astronomy Love,J. Student Assistant Technical Chemical Engineering . Luginsland, J.W. Student Assistant Professional U of Michigan Nuclear Engineering Mills, D.S. Student Assistant Technical Chemical Engineering Noren, E. Student Assistant Professional Kansas State U Math / Science , Piechowski, M.F. Student Assistant Technical Geological Sciences , Radke, D.L. Student Assistant Technica. Electrical Engineering Riley, ILJ. Student Assistant Professional U of Michigan Nuclear Engineering Roberts, C.J. Student Assistant Technical Agricultural Economics Santee, J.L. Student Assistant Technical Business Scott Ill, J.L. Student Assistant Professional U of Notre Dame Computer Science Sellers, S.D. Student Assistant Technical Electrical Engineering , Seman, D.J. Student Assistant Professional U of Michigan Nucicar Engineering Stammeyer, M.M. Student Assistant Professional Chemical Engineering Stephens, L.S. Student Assistant Technical Liberal Arts-Stich, T.A. Student Assistant Technical Chemistry / Pre-medicine Stith, B.K. Student Assistant Technical History Stith, P.S. Student Assistant Technical Chemical Engineering : Stryker, K.S. Student Assistant Technical Art Hi. story and Archaeology , Stuck, J.T. Student Assistant Technical Electrical and Computer Engineering Thomas, B.L. Student Assistant Technical . Mechanical Engineering } Thomas, D.C.T. Student Assistant Technical Chemical and Environmental ti Engineering Tones, K.K. Student Assistant Clerical Arts and Sciences t Volkert. E.W. Student Assistant Technical Pre-Med Wald, M.A. Student Ar.sistant Technical Mechanical Engineering Wallman, A.T. Student Assistant Technical Industrial Engineering 'r Walters, D.B. Student Assistant Professional U of Maryland Chemistry
' Warren, B.D. Student Assistant Technical Accounting 7 Watring, T.S. Student Assistant Technical Mechanical Engineering Williams, M.L. Student Assistant Technical Electrical Engineering / Civil .
Engineering / Math j Witte, D.A. Student Assistant Technical Mechanical Engineering Electrical Engineering ' Woods-Bowen, K.Y. Student Assistant Professional 129
MURR TOURS July 1991 - June 1992 University of Missouri Amliation 486 Secondary Schools (High School, Jr. High, etc.) 1256 Elementary Schools 291 Other Universities 300 Walk-In 309 Professional Organizations 401 TOTAL 3,043 Special groups who toured the reactor facility this year include 28 members of the Missouri Valley Chapter of the Society of Nuclear Medicine and 11 South Korean delegates. Once again MURR hosted a series of tours for Parents Weekend (28 participants), MU's Summer Welcome Program (61), St. Louis Partnership schools (240 students) and the Missouri 1 Scholars Academy (260 students). ! The MURR Video was loaned to 16 Missouri high schools,5 elementary schools and two departments of the University of Missouri, two other universities as well as six professional organizations. 130
1 L i INTERNATIONAL VISITORS : July 1991 - June 1992 r
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h k REACTOR OPERATIONS . 3 Walter A. Meyer Jr, Reactor Manager Anthony R. Schoone, Reactor Operations Engineer i Roland A. Hultsch, Reactor Physicist l Charles M. Anderson, Shift Supervisor ; Barry C. Bezenek, Shift Supervisor i Gregory F. Gunn, Shift Supervisor ; Nolan E. Tritschler, Shift Supervisor j 1 Leslie P. Foyto, Senior Reactor Operator John L. Fruits, Senior Reactor Operator Robert A. Hudson II, Senior Reactor Operator , Vernon L. Jones, Senior Reactor Operator 1 J. Michael Kilfoil, Senior Reactor Operator Michael L. Wallis, Senior Reactor Operator -i Timothy P. Warner, Senior Reactor Operator Paul J. Muren, Reactor Operator - Philip C. Neel, Reactor Operator , William O. OMham, . Reactor Operator Michael L. Randolph, Reactor Operator . Robert E. Walker, Reactor Operator Viola W. Sharp, Senior Secretary Rebecca J. Brooks, Senior Secretary (since June 1992) ; Reactor Operations staff focussed their efTorts on maximizing the safe operation of the reactor to produce neutrons for MURR's broad-based programs in research, ' education and service. The staff continued to pursue the upgrade of reactor instrumentation and control equipment as well as reactor auxiliary equipment, to help ensure long-term reliability for producing neutrons. From July l,1991 through June 30,1992, the reactor operated at full power 90% of all available hours. There were 18 unscheduled shutdowns during the year. A challenging maintenance outage to replace the original primary isolation valves was completed in two stages, the first lasting about 24 hours and the second 12. l INSTRUMENTATION AND CONTROL SYSTEM UPGRADES ; Progress continues on the upgrade of thecomponents ofthe GammaMetrics ' < reactor instrumentation and control design NIS have been delivered. These systems. A DOE grant for University components are being tssted,~ with 'a y Reserach Reactor (URR) Instru- projected installation in late 1992. A J mentation upgrades helped finance second instrumentation grant for DOE ( replacement of MURR's Nuclear will help cover replacement of the Instrumentation System (NIS). Excep; existing control rod drive mechanisms, for the wide range linear drawer, all of with bids going outin September 1992. 135
REACTOR AUXILIARY SYSTEM UPGRADES Significant upgrades made this past year to reactor auxiliary systems should l enhance the reactor's availability. The reactor valve operating system was improved by the addition of a new air compressor dedicated to the valve operating system, . backed up by the facility air compressor. Installation of a new reverse osmosis.(RO)
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unit with over twice the capacity of the unit it replaced has enhanced our ability to produce reactor grade water for reactor and pool water makeup, as well as provide I facility DI water. !
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Operations staff are planning additional changes to the DI system in FY93. Splitting the reactor makeup water and the facility DI water systems will provide an important benefit: the ability to pump the pool to low levels more quickly for deep pool maintenance. f I
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l MURR Reactor Operations - Longevity STAFF RECOGNITION Chuck Anderson 15 years , Barry Bezenek 23 years The twenty members of Reactor te, poyto 4 years . Operations on staff at the beginning of j John Fruits 4 years , FY92 epresent 194 years of service, ! Greg Gunn 11 years .
- an average of nearly 10 years per ff,jt,}h l fIa$. f person. MURR longevity figures are !
. Vern Jones 14 years shown at right. Mike.Kilfoil - ' 12 years ;
Walt Meyer 17 years . ; The cumulative experience of our l 1 - [^"j hmn Qr , Operations staff, coupled with the Willie Oldham . 1. year
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impressive longevity of the majority of Mike Randolph 6 years t our members, provides a very strong Tony Schmne 10 years q team. MURR's Reactor Operations Vi Sharp 14 years !
; [After nearly 21 years ofdedicated staffis the heart af the Center, m; tent ! service to the university ofMissouri, vi on producing neutrons for the wide announed her early retirement, range of multidisciplinary research, 3 efective August 31,1992J J education and service programs that . I " Tritschler 22 ars
$^3g, make the MURR Center our nation's Mike Walns 8 years i premier university research reactor. ,
Tim Warner 12 years -
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REACTOR OPERATIONS *
SUMMARY
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July 1991 - June 1992' - t
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MURR operated 24- hours per day, 7 days per week (averaging ; j approximately 152 hours per week). MURR operated at full power 90% . .! of all available hours in FY92. f . FY92 TOTAL l.;
.i Total Hours Oper ated 7,938 165,304 i 1
Total Hours at Full Power 7,874 162,442- !
.i TotalIntegrated Power (MWD) 3,283 61,822' i- 1 q
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- There were 56 scheduled shutdowns for maintenance, refueling - l and sample changes in the flux trap, 1;
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*For details see " Reactor Operations Annual Report 1991-1992* .
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UPGRADE GROUP 1 PERSONNEL J. Charles McKibben, Group Leader (acting) Kiratadas Kutikkad, Research Scientist (Adjunct Assistant Professor, Nuclear Engineering) i Walter A. Meyer Jr, Reactor Manager Chester B. Edwards Jr, Facilities Manager Susan M. Langhorst, Health Physics Manager (Assistant Professor, Nuclear Engineering) . Roland A. Hultsch, Reactor Physicist Jay F. Kunze, Senior Research Investigator (MURR) and Chair and Professor of MU Nuclear Engince-ing , Will am E. Miller, Senior Resean h Investigator, Group Leader (MURR) and Professor of MU
% dear Engineering, Director of Energy Systems and Resources Program -
Olawale B. Oladiran, Staff Engineer The MURR Center presents to MU the BUILDING ADDmON With the evolution of opportunity and the obligation to become a reactor programs and MURR's administrative y leading universityin nuclear related fields. The transfer to MU from the University of Missouri development and advancement of industries System in 1989, the need for an expanded and laboratories in these areas of science and research laboratory building clearly emerged as engineering as well as national projects such as the highest priority. The reactor (as a neutron the Advanced Neutron Source depend upon the source) w not the limiting entity; it is fully availability ofhighly qualified and well trained capable of providing greatly expanded- ; personnel. Over the past 24 years, MURR has radioisotope production,sampleirradiations and progressed through a series of upgrades that beam research opportunities whenever the has increased greatly its versatility for research, necessarylaboratory facilities become available. , and efforts to expand and adapt to meet the growing needs of research and technology Last year, an extensive study ofspace needs for i continue. During 1985-1989, a major three-part reactor-based research involved more than 100 ) plan was drafted encompassing: faculty and staffin an in-depth planning process. This group comprised the respondees to an .j
- an addition to the researth laboratory extensive space nced and program questionnaire !
building sent to over 20 academic departments, and the .;
- an increase in the reactor power level laboratory needs identified in the surveyprocess a cold neutron source for enhanced beam weredevelopedintolaboratoryprofilesheets. A l research opportunities planning group reviewed and consolidated the - j original space requests into a reduced set of a 7j The proposed expansion to the research building total additional gross square footage of109,439 =;
will more than double the laboratory space. and estimated project cost of approximately .; Otheraspects ofthe upgradeinclude the addition $22.4 M. i ofnew research programs, instrumentation and equipment, improved reactor systems and a The conceptual design of the first phase of the new fuel design. Work to support this effort is building addition was completed by Sverdrup - j spread throughout various MURR groups and Corporation of St. Louis, MO, with the final imolves many faculty associates. report to be presented in FY93. This addition ! 139
will add 81,500 GSF to the building and has a With the help of this loop, we have 3 project cost of $15.25 million. The addition, managed to establish that the resulta j which includes the highest priority items as obtained using RELAP are quite
. recommended bytheReactorResearth Advisory conservative (see REACTOR NUCLEAR Subcommittee, has two parts: a 54,500 GSF ENGINEERING PROGRAM section),
addition on the north side of the building with laboratories, a guide hall. support shops, offices,
- MURR Loss of Flow (LOF) and Loss of etc.; and a 27,000 GSF south side addition with Coolant Accidents (LOCA) have been >
laboratories, hot cell, glove boxes, shipping and analyzed for 20,25 and 30 MW power 4 receiving, support shops, offices, etc. levels using RELAP. These analyses 'l 1 indicate that MURR can be taken safely , POWER UPGRADE The Upgrade Groupis to at least the 25 MW powwlevel. actively pursuing the plan to nearly triple the powerlevel ofMURR from the " administrative"
- Early on in the efforts to upgrade the 10 MW power limit to a technical limit. To power of the MURR,it was realized that facilitate the power upgrade, a new fuel loading one of the areas where considerable efr or t was designed for the plate-type fuel elements has to be put is in the environmental :t uith denser maximum fissile material loading impact of the power upgrade, including and a more uniform power density. The new the effects of the trace amounts of fuel elements will reduce significantly the fuel radioactivity that are released from the cycle costs by achieving a higher power history MURR due to routine operation. {These i per element compared to the current fuel minute amounts 'of radioactivity are elements. diluted and releasr4 at a higher ' M stion
- to make its impact on the - ment While NRC approval for operating the new fuel negligible.] To have a bet w die on at the current 10 MW power level was obtained the environmental tran+ ort of-in August 1990, fabrication and testing of the radioactivity, the' outdated wind new fuel are dependent upon startup funding measurement system at MURR was :
from DOE. This funding is anticipated within replaced by a state-of-the-art system the 1993 federal fiscal year. capable ofprovidint,information that can be fed directly into a computer. Studies - i Many facets of the power upgrade effort are were undertaken to compare various i done in close cooperation with MU Nuclear computer pmgrarns capable ofestimating Engineering. Efforts are made to interest t he effect oGndeorological conditions and - graduate students in many of these projects, terrain information on routine release. ', thus affording students valuable reactor After considerable review, the NRC-- j experience. Currently six students (five at the approved computer program XOQDOQ j PhD level) are invohed in various upgrade was selected andinstalled atMURR. As j related projects. Some of the areas where we apartofthepowerupgrade egest,NRC ] have made significant progress are listed below: mandates MURR to do an analysis ofthe worst-case accidental radioactive release
- A loop for simulating the thermal- situation. A similar computer program hydraulic conditions inside tha MURR review is underway to choose a program .
core was developed in association with that handles such calculations. MU's Nuclear Engineering Program to benchmark results from the NRC-
- Another area of on-going work is the approved transient' analysis computer neutranics (reactor physics) analysis of program RELAP for low' power,-low the new core at higher powerlevels. Plans pressure and low temperature reactors. arc to perform experiments to obtain basic 140
i l l
! A Cold Neutron Source j w Power increase to 20 30 MW
.A
; Building Expension Second Fuel Upgrade i
New Research Fac!Dties (ongoing) Instrumentahon and CoWol Replacement (ongoing) Research instrument Upgrades (1978-1989) Schedule Increase (1977) j Power increase to 10MW (1974) . l l F6rst Fuel Upgrade (1971) First Operetkon (1966) i t-Construction Started (1963)
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f i ! L _ . _ _ _ _ _ _ _ _ _ . _ _ _ _ _ _ j reactor physics data such as neutmn lifetime SUPPORT ACTIVITIES As part of the and the reactor response to reactivity efforts to reduce the volume of LLW transients. Information collected from these generated by the MURR Center, the investigations will be used to benchmark Upgrade group assisted the Reactor some of the computer programs that are Operations group in the redesign of being developed by gradus te students sample irradiation cans. Monte Carlo specifkally for analyzing MURR transients. analysis techniques were used to determine the effect ofreplacing cadmiu m a While trying to put together a new Safety with baron as the thermal neutron shield. Analysis Report (SAR) for upgrading the The revised can eliminated fully the power of MURR, it became apparent that production of radioactive Cd (a mixed there is no NRC-mandated standard format waste). for SARs for research reactors. We are in the process ofdrafling rudi an SAR format We also assisted the Service Applications applicable to all research reactors, with an group in improving and documenting estimated submittal time for NRC review their methodology fbr preparing the safety and approval in 1993, analysis reports of new samples before being irradiated in the reactor. The l
- Other planned improvements include Upgrade group maintains several state-implementation of expert systems and of-the-art reactor analysis computer graphicalinterfaces to help the operators programs for predicting many important
- and to assist them in better identifying parameters such as the reactivity effects l the onset ofabnormal operating conditions of new samples, heat generation rates l (see REACTOR NUCLEAR ENGINEERING and heat transfer rates in samples that._
l PROGRAM section). have never been irradiated before,
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t FACILITIES OPERATIONS - Chester B. Edwards Jr, Facilities Manager Olawale B. Oladiran, Staff Engineer C. Bradley McCracken, Staff Engineer ' David G. Nickolaus, Senior Drafting Technician Electronics Shop: Thomas H. Seeger, Chief Electronics Technician , Joe D. Baskett, Research Electronics Technician Mark Richardson, Electronics Technician (since January 1992) i Machine Shop: Mac L. Evans, Chief Research Engineering Technician ' Kenneth W. Beamer, Senior Research Engineering Technician Ronald R. Kitch, Senior Research Engineering Technician Charles L. Kribbs, Senior Research Engineering Technician Leah Moreau, Senior Secretary (since November 1991) i Facilities Operations staff provide and . Fire sprinklers were installed in the lli coordinate technical service on design, area outside the Alpha Laboratory in construction, installation, modification and compliance with the NRC Admini-calibration of reactor, research and service strative Judge's Order. equipment for MURR staff, faculty users and students. The Electronics Shop and Machine
- Cell Culture Laboratory (room 215) base i Shop deliver support to meet routine reactor construction was completed, with ,
maintenance and technical needs as well as specialized equipment and laboratory research program requirements. In addition. HVAC controls to be installed, tested , I the shops support the reactor services group and placed into service in FY93, i with construction and welding of sample cans, special tools and fixtures, and with hot cell
- The conceptual design of the building manipulators maintenance. Drafting Services addition was completed by Sverdrup provides a variety of services including design Corporation of St. Louis, MO, with the drafting of research instrumentation and final report and rendering to be laboratory facilities; graphics for publication presented in FY93. The distribution of in various technicaljournals; posters to display new and existing space assignments ;
scientific research; and various other projects. locates the programs handling multiple > curie quantities ofradioactive materials , Special projects during the year include: In hot cells and glove boxes in the south
- engineering support and collaboration addition; programs handling millicurie with Costar on the equipment upgrade to curie quantities of radioactive L
_ [ of the new Mark Ill irradiator case, web materials in the existing laboratory - i drive and gas system. The Mark III building; and progra ns handling ; irradiator equipment development was microcurie to millicurie quantities of completed and tested, with the exception radioactive materials in the north side. 1 of the gas system and control systems. The building addition on both the north -l The project was placed on indefinite and south sides matches the existing 'l hold with all equipment packaged and building basement and grade elevations .; stored by Costar. plus each has a second level. The addition l l 145- i
'?
2
results in 81,500 GSF, with
- Auxiliary annunciator. panel was i approximately- 54,500 GSF on the installed in the reactor Control Room to
-north side housing laboratories, a accommodate Costar equipment and - ;
guide hall, support shops, ofIices and other program needs.' '4 associated mechanical spaces; and 'l 27,000 GSFon the south side housing *
- Secondary water cooling system was laboratories, hot cells, glove boxes, upgraded. and- replaced with pH shipping and receiving, support shops . conductivity monitoring equipment for . j and associated mechanical spaces. piping corrosion control. 1 The reduced conceptual design is a JI
- $15.25 million FY93 building as
- New dedicated reactor valve-op' air l
recommended- by ' the Research compressor was installed and valve-op Reactor Advisory Subcommittee system removed from facility compressed 1 (RRAS). air system.' I A third temporary office building
- Two hot eell manipulators received from ,
(TOB-3),1960 sq ft, was ordered for Rockwell Ihternational as excess _. the south side of. the laboratory property were n odified and installed. : building west of the loading dock. '
- New facility exhaust stack radiation air -
SANS vacuum chamber and carriage monitor from NMC Corporation ~ was design and bid- documents were received and installed. - completed. A Request for Proposals i (RFP) was submitted to a number of
- Partial shipment ofnew reactor nuclear l ;;
fabricators and is due back in early instnament channels equipment from , FY93. Gamma Metrics was received, with ! L testing and installation expected in Design of a new topaz counting FY93.
- l
~~
machine with 48 canals operating linerally is well underway. The
- Atomic spectroscopy instrument was '
objective of the new system is - installed in laboratory 218. independent discrete counting ofeach canal. *- TRIAX instrument was received fromi ' Oak Ridge National Laboratory. Drum, .
- Two new sample rotators were air eylinder, and gear mount restoration designed, constructed and installed were completed, with installation to be. s for in-pool topaz irradiation holders completed in FY93.
and 4" and 5" silicon. I
. Cooling coil was added to pump room at
- Fixture design was started for the cooling tower basement to protect l residual sStress equipment to handle operating equipment in the area.
'l NASA's 1/4 scale Challenger booster -l rocket cylinder for evaluation of the- *
. New weather instrument was installed I weld areas. av verified operable in lab 213. j I
'I
- 1 146
REACTOR. HEALTH PHYSICS ,
' Susan M. Langhorst, Manager (Assistant Professor, Nuclent Engineering) ' John P. Ernst, Assistant Manager and Health Physicist 4 James R. Schuh, Health Physicist Ray W. Stevens, Senior Health Physics Techmcian Joseph W. DeMers, Senior Health Physics Technician (left September 1991)
Rex G. Ayers, Health Physics Technician (since August 1991) ; W. Derek Pickett Health Physics Technician (since January 1992) l Andrea J. Shipp, Health Physics Technician (upgraded from HP Trainee April 1992) Leslie M. Powell, Senior Secretary (upgraded from Secretary June 1992) { The primary responsibility ofthe Health Physics * . MU Hospital Co-60 Teletherapy Unit, (HP) group is the radiation safety program to License No. 24 00513-35 , support the multi-faceted research, service and
- MURR Exempt Release License No. 24-educational pmgrams conducted at MURR. 00513-36E Health physics coverage of these programs Each campus and the MURR Center have been presents a unique challengsto ensure radiation responsible for the operational function ofthese safety with regard to personnel training, licenses at their respective sites. For MURR, personnel dosimetry, reactor operations, this operational responsibility has been with '
processing of. radioisotopes, radiochemical the Isotope Use Subcommittee (to the Reactor research development for ultimate use in Advisory Committee) and with the MURR HP - , radiopharmaceuticals, transportation, system group. { design, environmental assessment, emergency response, radioactive material control and In recent years, the NRC has been focussing on accountability, contamination assessment and improving and strengthening administrative control, radwaste management, and facility / controls defined for materials licenses. To materials licensing. improve the effectiveness ofits radiation safety programs, the University requested in its Broad BROAD SCOPE LICENSE RENEWAL Scope License renewal that both licensing and . . opemtionalresponsibilitiesbeestablishedwithin . On February 27,1992, the University ofMissouri the respective committees and health physics System (UM) applied for renewal ofits Broad units by issuance of separate radioactive Scope License fLicense No. 24-00513-32). The materials licenses for each campus and for the existing Broad Scope License had established MURR Center. Defining administrative controls theadministrative structure forType A materials consistent and compatible with those already in , licenses at the University as follows: a Central place under the MGRR reactor license pmvides . Radiation Safety Committee (CRSC) and one the most effective and logical control of Radiation Safety Oflicer(RSO). The CRSC and radioactive materials at MURR. The NRC is l [ RSO are responsible forreviewing and approving currently reviewing the University's renewal the use of radioactive materials at the four application, and we are in the process of campuses under all the University's materials answering some of their questions concerning our reorganization and how we plan to conduct : licenses except for the Exempt Release Limnse. The materials licenses are: our radiation safety programs.
- Source and Special Nuclear Materials WASTE DISPOSAL License, No. SNM-247 .
3'
- Cobalt Irradiatorat MU campus, License ADCO Services, Inc. has continued to act as our
- No. 24-00513-33 institutional waste broker. Through ADCO,we
- MURR Cobalt-60 Irradiation Facility, disposed of 472.5 cubic feet of LSA material l License No. 24-00513-34 generated at MURR. ,
-l 147 1
f
t il L ALARA TRAINING The ALARA program imple- Inereased offorts to provide supplementary training forindividuals mentedtaimpmvethereview working at the MURR Center have resulted in the development and documentation of these .and/or presentation of the following special ketures and videos: efforts has continued to
' develop. . As stated in the
- Radiation Fundamentals MURRFY91 AnnualReport,
- HP Instrument Training the challenge ofinstituting a a General Safety (video) -
more meaningful ALARA
- Chemical Safety (videos) ;
program at MURR has been
- History ofRadioactivity ;
theorganizingofappropriate
- Personnel Monitoring ..j ALARA review levels that
- Radiobiology y initiate review and docu-
- Special Subjects for Custodial Personnel 1 mentation fora wide rangeof
- Biological Effects !
reasonable personnel doses.
- Radioactive Material Shipping Established investigational
- Radioactive Decay :
levels are shown in Table L .
. _ l Efforts continued on making the new stack monitoring system l The average monthly whole operational (Nuclear Measurements Corporation Model RAK- .l bodydeepdosesineachgmup 22ABIB-P.6, Continuous Air Monitor System). Equipment. and for FY92 are indicated in programming problems have delayed final testing and our :
Table 2. Reorganization of acceptance of the system as MURR's primary stack monitoring , research gmups did occur in system. In December 1991, a new access to the MURR containment ! April 1992, but the ALARA building roof was made in the North tower. This new necess port ; review program structure allows easier entrance to that area for inspection of the roof and .. ; remained constant for FY92 systems and instrumentation located in the area. Previous access , pending renewal of the was either through the facility stack exhaust system, which was -1 contract for personnel normally limited to times ofreactorshutdown, or by portable ladder . dosimetry services. from the laboratory roof. _l t f tai!LE 1 INVESTIGATIONAL LEVELS TABLE 2 FY92 AVERAGE MONTHLY WHOLE (mrem per month) z BODY DEEP DOSE LEVELt+ LEVEL 11' GROUP DOSE' !
! a Whole body; head and > 30 above > 50 above Computer Development minimal j trunk; active blood ar*d 33% of and 50% of Directors Office forming organs; lens average monthly average monthly Nuclear Engineenng' of eyes; or gonads dose' dose,' or >180 Radiation Effects Hands and forearms > 1000 > 3000 I Facilities Management - 10 mrem
~
(shanow dose) f' Instrument Development Nuclear Analysis Program :1 Skin of whole body * > 300 > 600 Neutron and Gamma-Ray Scattering ' j (shahow dose) Radioisotope Applications i
)ji
+ l Reactor Services 30 mrem ;j personnel dose noted 3 j
report required assessing personnel dose Health Physics 50 mrem
' average monthly dose based upon previous f ar quarters _
apphcable for signtficant quantities of bota emitters Operations 80 L mrem :?! l .) 1 L.,_'_____.__ .. . _ , . - . _ _ _ - . _ _ . - - . . . l
-148- ';
-t
4 COMPUTER. DEVELOPMENT.
-i i
Gene IL Moum, Senior Research Scientist (Adjunct Assistant Professor of i Computer Science) l Stephen P. Fox, Computer Programmer / Analyst II . i W. Michael Shell, Computer Programmer / Analyst II (left September 1991) Chao Wang, Computer Programmer / Analyst II (since October 1991) ,
-t The day-to-day operation of the MURR Center has become increasingly aided by computers. The variety of applications range from business oriented spreadsheets to computer aided design, from research data reduction and analysis to desktop l publishing. There are currently over 140 user accessible computers in' daily use at i
the Center. These are both workstations and multi-user computers. This total does . not include the dozens of dedicated computers that control spectrometer motors, monitor background radiation, control computer ' network traffic and do data ' l acquisition. The Computer Development group is responsible for the overall support and ' operation ofcomputers and computing facilities at MURR. We provide, support and , maintain the Local Area Network (LAN) within the Center that provides the . connectivity necessary for researchers to access their instruments and data, [
^
workgroups to access common databases, and staff to communicate and exchange ~ files electronically. ; The LAN spans four buildings with five wiring closets and 28 active network control - devices. Connection to the LAN is provided from every room in the building via 15 : miles of MURR-installed cabling. l The Computer Development group also supports the central computing facility for. [ the Center. This consists ofa pair ofMicroVAX III+ computers that provide support r for data reduction and analysis, word processing, spreadsheets and statistical analysis. Computer Development is involved in several long range projects: L
- a new irradiation monitoring system for the silicon program l
- a new generation control system for the new gemstone counting machine <
l
- a new generation ofcontrol computer system for the neutron and gamma-ray spectrometers for the several programs on the beamport floor. .
The Computer Development group generally supports two or three students in. ! l l! technical positions. We are currently supporting our second Master's candidate in - cooperation with MU's computer science department. . l 149 L
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INSTRUMENT DEVELOPMENT GROUP Ronald R. Berliner, Senior Research Scientist (Adjunct Associate Professor of Physics and Adjunct Associate Pmfessor of Electrical and Computer Engineering) Don Bryan, Computer Engineer Douglas Charlton, Computer Engineer ; The mission of the Instrument Development Group is the design and fabrication of - , electronic instruments for research. The group has concentrated on the development of position sensitive neutron detectors, and their support sofl. ware for neutron diffraction applications, the fabrication ofcomputer interfaces for neutron diffraction instruments and the development of special purpose micro-controllers for process. control applications. t These three areas of activity have dominated the activities of the group for the past year. The renewal of neutron diffraction resources at MURR and the construction ofseveral new inst ruments has required the ID group to devote substantial resources to the fabrication of spectrometer computer interfaces. Four new interfaces have been constructed and a total of 25 stepper motor controllers and 6 Timer-Counters have been fabricated. The group continues to be responsible for the maintenance of the high resolution powder diffractometer position sensitive detector system. Several new capabilities and hardware features have been added to the system in the course of the last year. The instrument has completed 650 runs during the period July 1, a 1991 - June 30,1992. Fortunately,it has required little maintenance during the year. : i R. Berliner was on leave at the Australian Nuclear Science and Technology , Organization during the period March 1992 -July 1992 but several projects initiated j prior to that time were approved or funded during that period. A grant for the ! construction of a position sensitive detector for the residual stress spectrometer was t l- funded and work on ihe definition of the analog and digital subsystems for that , instrument are underway. The group has also undertaken the development of a new - j process control micro-controller using the MC68HC16 micro-processor. Finally, the - l group is participating in the development of new techniques for nuclear signal processing as part ofits effort for the DOE funded Smart-ADC grant. 151 l'
A PEAK-DETECTOR ADC D. Charlton, T. Stuck and R. Berliner U Research on the development of a virtue of the new design is its simplicity as conceptually new analog-to-digital the complex analog-to-digital portion of the 'l converter (ADC) for nuclear pulse-height circuit is encapsulated in a commercial , ' analysis is in progress. The design single-chip off-the-shelf device. Figure 1 is a ' utilizes new techniques for determining block diagram of the new pulse height .l the time and magnitude of the occurrence analyzer. of a nuclear detector pulse such as those , from proportional counters. The The circuit has been tested and performs the occurrence of a peak is detected by - desired function. Tests are under way to ., differentiating the input pulse and using' measure its differential and integral + the zero-crossing to signal the pulse peak. linearity for a comparison with data 1 The peak amplitude is captured and obtained for existing Wilkinson ADC stored by an operational amplifier (op designs. Additional new features are being i amp) peak-detector circuit, which uses a incorporated into the new ADC. Tests of the high-speed op amp for the input stage and in-circuit performance of a digitally . a low bias current op amp for the output adjustable potentiometer (E2 POT) for use in i stage. The stored peak value is converted both the Wilkinson-ADC designs and the - to digital form by a fast-conversion-time, new ADC. This digitally adjustable ; 12-bit ADC integrated circuit. ' This is in potentiometer would replace many of the ; contrast to the " standard Wilkinson manually-adjustable potentiometers used in pulse-height-analyzer design that has the electronics that service the neutron been in use for many years. The major position sensitive detector systems.
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-D;gito t i Detector Input i Converter ,J j -
Gating i , ADC_OUT LLD . Discharge Compar- GT LLD . _ Control .__ ctor ADC_TJONE Fig.1 This block diagram of the peak-detecting system ADC shows the . . ULD separate subsystems that comprise tho - Compar- /GT_ULD - device. The actual hea't of the system 0t0" is the Peak Detector circuit and the analog-to-digital (ADC) subsystems. 152
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i A NEW PROCESS CONTROL MICRO-CONTROLLER D. Bryan, D. Charlton, W. Eubanks, T. Stuck, R. Berliner j Design and development of a process control port for sensor input or actuator output. The ! system using the Motorola MC68HC16 I/O lines can also be software configured for , micro-controller is underway. The micro- specific tasks according to their application ; processor that forms the heart of the system requirements. Drivers have been added to ' is a high speed 16-bit CMOS device with on - the micro-processor's address and data buses chip peripherals such as a multiplexed 10- so that off-board peripherials can be memory . , bit analog-to-digital converter (ADC), a mapped, simplifying software design for a :i
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general purpose timer (GPT),1024 words of variety of external devices. high speed static random access memory . l (SRAhD, and a queued serial communications The new controller communicates with its - ! y module (QSM). host computer via the IEEE-488 communi-cations interface, standard with all other :i L L- The process controller design utilizes most InstrumentDevelopmentspectrometer - l aspect.s of the 11C16 by incorporating an RS- computer interfaces. It has a capacity for up - ;
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232 serial interface into the QSM, which to IM-bytes of Read-Only-Memory (ROM) . allows the process controller to control and program space and 128 k-bydes of Raadom communicate with other RS-232 devices, using Access Memory (RAM) data space in addi- 1 the GPT to accumulate nuclear detector. - tion to the ik-byte high speed on-chip RAM. pulses, allowing the controller to service detector systems, and having 22 general Software development for this pmcess :I ' purpose inputmutput (I/0)1ines arranged as controller will be in C and Assembly. . - - two 8-bit parallel ports and one 6-bit paratlel language, allowing compact yet portable,
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modular code. Extensive applications for this controller can be developed 'due to its large program and data space and the flexible design of the hardware. A representation of the completed system is shown in Figures 1 and 2. The device as configured - is set up for one detector input and for input and output to both IEEE-488 and RS.232 communications.
-1 I Fig.1 A block diagram of the MC60HC16 process controller. The large box in the center is the 1" x 1" microprocessor chtp itself.
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SERVICE APPLICATIONS William F. Reilly, Assistant Director, Technical Applications Stephen L. Gunn, Reactor Services Engineer Martha A. Carter-Tritschler, Supervisor, Reactor Services Wei Jia, Reactor Services Project Specialist (since June 1992) Leonard H. Manson HI, Reactor Services Project Specialist Paul D. Miller, Reactor Services Project Specialist James P. Lanigan, Senior Research Laboratory Technician (promoted / transferred from Radiopharmaceutical group August 1991) Timothy G. Arnold, Research Laboratory Technician (since November 1991) Coralie T. Benson, Research Laboratory Technician J. Eddie Brooks, Research Laboratory Technician (since May 1992) . David A. Crawford, Research Laboratory Technician (hired as Laboratory Assistant August 1991; promoted March 1992) Melissa M. Gibbs, Research Laboratory Technician (since August 1991) L Joseph Henke, Research Laboratory Technician William D. Howell, Research Laboratory Technician , G. Lawrence Jesse, Research Laboratory Technician Stacy S. Lanigan, Research Laboratory Technician (left July 1991) Zelly Les, Research Laboratory Technician Geft July 1991) William A, Martin, Research Laboratory Technician (since August 1991) Vannak Phouk, Research Laboratory Technician Kathleen D. Pierson, Research Laboratory Technician (promoted from Laboratory Assistant December 1991) Matthew R. Sanford, Research Laboratory Technician (promoted from Laboratory Assistant September 1991) Janice A. Caldera, Laboratory Assistant Geft August 1991) Todd E. Gould, Laboratory Assistant Geft August 1991) : Khim Long, Laboratory Assistant Timothy L Morris, Laboratory Assistant (since August 1991) Thi T. Tran, Laboratory Assistant Jeffrey E. Valenti, Laboratory Assistant Geft August 1991) Kathryn A. Harbour, Secretary ! Susan A. Cable, Senior Clerk Typist 4 The Service Applications group provides the interface between experimenters and the~ reactor. The group evaluates experiments to ensure that all safety requirements are met, prepares samples forirradiation, processes irradiated materials, and packages and ships materials after irradiation. This group also handles the processing of production isotopes, silicon and gemstones that produce the bulk of revenue for research work. .; L During FY92, Service Applications performed work for 140 industrial customers,42 universities and four government agencies. . 157 .) i i
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i 4 i I l TABLE 1 IRRADIATION POSmONS
- CAN MAXIMUM MAXIMUM MAXIMUM PoSmoN DIAMETER SAMPLE SAMPLE THEF; MAL i (inches) DIAMETER LENGTH FLUX.
(Inches) (inches) (n/crn8-sec)
'I
, Flux Trap 1.125 1.00 3.75 .5 x 10"
.400 0.275 1.00 5 x 10" l
I Row 1 1.125 1.00 3.75 8 x 10'8 + Row 2 2.350 2.00 10.00 5 x 10" ) j Row 3 3.350 - 3.00 10.00 3 x 10" ; J Row 4 4.350 4.00 10.00 6 x 10'8 1 1
! Row 5 5.350 5.00 10.00 1 x 10" -l
; a
, . - . _ . . _ ___ -._ _ _ t SERVICE lRRADIATIONS The Service ISOTOPES MURRhasbeen activein Applications group performs work finding new uses for radioisotopes. i for both University and non- Certain radioir,otopes, such as P-32 -
University users. The two major and S-35, are produced in large volumo 1 areas are the reflector, which is and sold by the Curie on a routine , accessible any time for inserting or basis. Other isotopes are produced on ' ' removing samples,and the flux trap, demand as serviceirradiations. Figure whichis accessible once a week during 1 shows the numberof type Aand type scheduled maintenance shutdowns. B shipments of radioisotopes during All irradiations for experimenters FY92; Table 2 is a list of the isotopes outside the University are charged shipped. by a standard charge schedule. . Unfunded researchers at other NTD SluCON The facility has been - Universities may apply for DOE active in treating silicon _ by funded Reactor Sharing support. transmutation of Si to P since 1975. The current treatment capacity exceeds Two one-inch diameter pneumatic 40 tonnes per year at 1 ppb P. Plans tubes permit samples to be positioned are being made to double that capacity rapidlyin high flux reflector positions in 1993 due to strong worldwide for short irradiations and then demand. returned for neutron activation j analysis. Specialized work in lower GEMSTONES The service group -_ flux positions includes neutron operates a gemstone enhancement f]j radiography and membrane filter program to crea te blue topaz by trea ting production. MURR alsc has a cobalt white topaz with fast neutrons. The- 4 facility for intense gamma resultant blue topaz must be analyzed irradiations. stone by stone to ensure compliance- ;
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.. - .- . - ~ - . - . . . . - - .. .. . . - . . - - . . . . - . _ - _ _ _ - _ _ _ _
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' TABLE 2 ISOTOPES SHIPPED ~ j
. i Ag-110m Dy-159 f r-192 Re-186 Sr-85 0 Au-198 Dy-165 Lu-177 Rh-105 - Ta-182 , Br-82 Er-169 Mn-56 Ru-103 Tb-161 ; Ca-45 Eu-152 Na-24 S-35 Te-123m ! Ca-47 Fe-55 Os-191 Sb-124 Te-125m I Cd-109 Fe-59 P-32 Sc-46 Te-125 - Co-141 Gd-153 Pd-103 Se-75 Tm-170 , l ' J Co-58 Gd-159 Pr-142 Si-31 W-187 , Co-60 Ge-71 Pt-191 Sm 145 Y-90. , { Cr-51 Hg-203 Pt-193m Sm-153 Yb-169 1 l
- Cs-134 Ho-166 Pt-195m Sn-113 Zn-67 i Cu 64 In-114m R b-86 Sn-119m Zr-95
- with US NRC release criteria. The current capacity is about 'six milhon ~
j discrete analyses per year. The analysis program is also ofTered for material i treated at other facilities. SHIPPING The service group also operates hot cells and provides a complete l l shipping program to ensure that material can be returned to experimenters. I 180 -- I t E Type A Shipments [ ,33 ,, E TypeB Shipments , 140 -- 120 -- i 100 -- l BD -- ; 60 -- 40 -- l 20 -- I O I I I i l i ! I 1 I i !
.wm a ,n sen omm m.m o=+ mm **m n-m - ae r anym w Fig.1 Radioactive shipments from MURR.
159 i
y L SILICON ANALYSIS PROGRAM Michael D. Glascock, Senior Research Scientist (Adjunct Assistant Professor, Nuclear Engineering) Hector Neff, Research Scientist (Adjunct Assistant Professor, Anthropology) Jeffrey R.' Denison, Senior Research/ Laboratory Technician 1 The Silicon Analysis Program was other high purity materials. NAA developed in the early 1980s by ofTers many advantages over other Dr. Michael D. Glascock. While analytical techniques, such as: ; the program was originally
- An ability to analyze simul-designed to satisfy the analytical taneously for approximately. .
needs of a rapidly grmving forty _ elements. 1 semiconductorindustry, the past
- An ability to detect _ accurately decade has brought steady growth elemental concentrations in and a broadening of scope. In the the ppb range and below.
beginning, the work performed
- An ability to perform the ,
mainly involved bulk impurities analysis without destruction , analysis for research and or loss of the sample. development divisions of a Table 1 lists the elements handful of US companies. Today, determined and typical detection y in addition to the R & D work, limits of a standard analysis of_ ' companies are using the Silicon high purity silicon. Analysis Program to provide quality assurance analysis on Several changes made to the materials such as silicon, high standard procedures over the last purity graphite, high purity year have improved the program ; quartz and 22B. The program is significantly. The first was the ; internationally recognized and replacement of the old graphite , performs analysis for companics irradiation containers with high ' in Denmark, Japan and Italy as purity graphite containers. This well as the United States. During not only reduced the sample , FY92, the program performed contamination poter,tial from work for 11 industrial customers graphite dust residue but also and two universities. Figure 1 significantly reduced the activity ; illustrates the FY92 sample level of the containers after - 1 volume. irradiation. Second, a mandatory j de-ionized water, ultrasonic l The Silicon Analysis Program cleaning prc,r ' was added. 1 utilizes neutron activation This new procet , has proven to analysis (NAA) to determine trace clean the samples more impurities in semiconductor and thoroughly than rinsing with DI I 160
) l l ! water alone. Third, a short data quality, container activity irradiation analysis service has level or container reusability been developed for non-silicon exited. A disadvantage to using matrix samples. The short analysis quartz over graphite is cost, i can provide the customer with data with quartz irradiation on short-lived element isotopes such ccmtainers being about 3 times . l as Al, Cl, Mg, Mn and Ti. more expensive than graphite l containers. - So, for the present, . Earlier this year the Silicon the Silicon Analysis Program ' Analysis Program was awarded will continue to use high purity a $4,000 contract from Eagle- graphite containers. ;
- Picher, Inc. to perform a 1 feasibility study to determine if Future program improvements 1 high purity quartz irradiation include the possible installation
]
, containers held any advantages of a soft-walled clean room for ! over the presently used high pre-irradiation sample handling purity graphite containers. The and an increased sample results of the study indicated irradiation time to improve f i that no significant advantages in detection sensitivity. b l- 100 ! l 90 80 ------=====- - 70 -
-- =- - = -
.l 60 - -
50 =
~
0 I I '1 i i t i 1 t t I I ( Jul-91 Aug41 ,Sep41 Oct41 Nov-91. Dec-91 Jan-92 Fet>92 Mar-92 Apr-92 May42 . Jun 92 Fig.1 Number of sampics anatyred during FY92 , i i 161 I
r ,
' Table 1 Approximate detection limits for impurities in an undoped silicon specimen ;
- welghing 15 grams after a 40-hour irradiation in a thermal neutron flux of 2.5 x 1013 n/cm'/s.*
I Concentration Atoms /cc _ Element atoms per
?
Elements 6'PB by weight of sliicon billion silicon atoms 1 Ag 1.5E-03 -2E+10 4E-04 + As 2.5E-03 5E+10 1E-03 ' Au 1.5E-05 1E+08 ! 2E-06 Ba 1.0E-01 1E+12 2E . Br 3.0E-03 SE+10 1E-03 Ca 6.0E+01 2E+15 4E+01 Cd 2.5E-02 3E+11 SE-03 I Ce 2.0E-02 2E+11 4E-03 Co 4.0E-04 2E+10 2E-04 Cr 2.0E-02 SE+11 1E-02 c i Cs 1.0E-04 1E+09 2E-05 - Cu- 3.0E-02 6E+11 1E-02
- Eu 4.5E-04 4E+09 BE-05 Fe
-l 8.0E-01 2E+13 4E-01 Ga 4.0E-03 -8E+10 . 2E-03 Hf 1.5E-03 1E+10 2E-04 l Hg 4.0E-03 3E+10 6E-04 , in 8.0E-03 1E+11 2E-03 ~
l Ir 1.5E-05 1E+08 2E-06 ! l K 5.5E-01 2E+13 4 E-01 ! I j La 1.0E-03 1E+10 2E-04 R Mo 1.5E 01 2E+12 4E-02 Na 3.5E-02' 2E+12 4E-02 Ni 4.0E-01 1E+13 2E-01 Pt
.l' 7.0E+00 SE+13 1E+00 .
-l'
. .i Rb 1.5E-02 3E+11 6E-03 ;
Sb 2.0E-03 2E+10 4E-04 : Sc 6.5E-05 2E+09 4E-05 Se 6.0E-03 1E+11 2E-03 Sn 2.0E-01 2E+12 4E-02 Sr 2.0E-01 3E+12 6E-02 Ta 2.5E-04 2E+09 4E-05 Tb 2.0E-04 2E+09 . 3E-05 ' Th 6.5E-04 4E+09 8E-05' Ti 2.0E+02 5E+15 1E-02 U 1.5E-03 1E+10 2E-04 W 1.5E-03 1E+10 2E Yb 6.0E-03 ' SE+10 1E-03 Zn 4.5E-02 1E+12 2E-02 Zr 3.0E-01 -SE+12 1E-01
- Determined by using a high-resolution HPGe detector to perform two measurements of 30 -
minutes after 2 days and 6 hours after 15 days, respectively. L _....m_._ . _ . 162
y Radiopharmaceuticals Group ISOTOPE SERVICE In addition to the production ofisotopes for MURR and MU research work, the MURR Radiopharmaceutical group (RPG) performs numerous irradiation and processing services for other researchers at MU, other universities and industry. Typical examples of such work include:
- Production and pmcessing of the short-lived
- The MU Department of Chemistry and tracers K-42 and Na 24 for studies of the Center for Radiological Research essential hypertension by Pmfessor Allan (CRR, which has been
- spun off" from Jones and other scientists at the MU MURR) receive frequent shipments of Physiology and Pharmacology Departments Au-198, As-76, Pd-109, Rh-105, and Cd-have now been turned over to MURR 115/In 115m, Dy-166410-166, and W-Service Applications after more than 15 188/Re-188 generators for their years of continuous supply by RPG. RPG researth in the biological applications has supplied well over 2000 samples during of radioisotopes and for lab course this time, supporting substantial external work. Some of these isotopes, notably grant money to the above departments. Rh-105, require substantial and complicated processing at MURR.
- Fluxtrap irradiaton and processing of high-specific-activity Re-186 for radioimmuno-
- Several irradiations producing therapy clinical trials in colon, lung and isotopes of hafnium were performed ovarian cancer patients sponsored by for Professor Girit at Yale University -
NeoRx Corporation in Seattle, St. Louis, for research in physics; University of Los Angeles, and Davis, CA have been a Missouri physicists also occasionally major effort, with treatment of 4C-50 receive shipments of Pd-103 and patients annually and 1-2 samples Pr-142 for ~ search and calibration processed per week, each exceeding 1 Curie purposes. Preparation of Te-128 and of Re-186. A patent is held jointly by MU Te-125m for Professors Boolchand and NeoRx on a novel rhenium reactor and Bresser at the University of target material which has made the Cincinnati for Mussbauer studies has processing at MURR and NeoRx simple, been done also. safe, and convenient.
- 1rradiation of Pd-102 to produce Pd-
- Weekly production of rare-earth 103 commercially for use in radioisotopes such as Ho-166. Lu-177, TheraSeed implants for the r Sm-153, and Gd-159 for commercial treatment of prostate cancer in the medical research in radioimmunotherapy US is performed at MUFR. RPG has and for patient trials of Sm-153 EDTMP, a also transferred this duty to Service !
novel bone cancer pain palliation agent Applications, which involves 20-30 > invented at MU and MURR. Sm-153 pneumatic tube irradiations of EDTMP currently is entering Phase III samples of Pd-102 each year to trials in US pauents, supported by support the quality control program l production at MURR and sponsored by the used by the manufacturer of Dow Chemical Corporation. TheraSeed, 'I heragenics Corporation in Atlanta, GA.
- Production of Pt-195m for Professor Walter l Wolf at UCLA for use in the preparation of - Irradiation of hydroxyapatite GIA)
Pt-195m cisplatin, an experimental microspheres for CeraMed Corporation radiodiagnostic agent tracking the response in support of Mallinckrodt Medicars to cisplatin chemotherapy in human brain development of Ho-16G HA cancer patients. About 25 patients are micmspheres for rheumatoid arthritis treated each year. radiotherapy by radiation synovectomy. 1 i
u Nuclear Analysis Program ' RADIOISOTOPE ~ PRODUCTION The three-part mission of MURR-research, education and service-is often overlapping and interconnected. Many research efforts iiwolve developing a tool, technique or technology that evolves into a service application, perhaps even is , picked up by industry and carried out on a much larger scale. ' Nutritional - - research carried out in the Nuclear Analysis Program at MURR has in the past several years employed some high specific activity radioisotopes that are not commercially available. MURR is the nation's only supplier, allowing scientists at many institutions to conduct new investigations into the role . ! of specific trace elements.
?
Cu-67/Cuf4 High specific activity become a national supplier. Se-75 Cu-67 and Cu-64 are produced on a requires a long, uninterrupted monthly basis at MURR. These irradiation and chemical speciation radionuclides are provided to following processing. Different researchers throughout the United chemical forms of Se-75 are being - ' States for experiments in nutrition considered currently, since various and radiopharmaceutical evaluations chemical forms behave differently at such institutions as Purdue, biologically; for example, soine forms Washington University and the may be anti-cancer agents. Se-75 is Human Nutrition Research Center supplied for a wide spectrum of (U'SL)A-ARS, Grand Forks, ND). selenium research to some 20 laboratories throughout the country, So-75 Researchers use this including the National Cancer impo+ tant tracer to study the Institute, the National Institutes of ' I nutritional significance of the Health, Oregon State, Vanderbilt, essential trace element selenium and the University of Rochester and - l possible roles it may play in cancer Utah State. This past year shipment prevention. The tracer was first of Se-75 went international, investigated and used by MURR accommodating researchers in researchers in nutritional studies, Germany, Sweden, Great Britain and by the le 1980s MURR had and India. 164-i
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Physics, Chemistry and Materials Science PUBLICATIONS
, - Allman, B.E.; Cimnuno, A.; IGein, A.G.; Opat, G.I.; Kaiser, H.; Werner, SA, A Scalar Aharonov-Ikihm ,
Experiment with Neutrons, Phys Rev Iett 68,2409 (1992) Beach R.S.; Borchers, J A; Erwin, RW.; Flynn, C.P.; Matheyn, A.; Rhyne,JJ.; Salamon, M.B., Magnetic Order in Dy/Lu Superlattices, J Mag and Mag Matle 104-107,1915 (1992) Ecchtold, J.; Xue, Y.Y.; Huang, ZJ.; Hungerfani. E.V.; Hor, P.H.; Chu, C.W.; Maruyama, X.K; Backe, H.; Buskirk, F.R; Snyder, D.D.; Jean, Y.C.; Farmer, J.W., Defect Size Dependence of Critical Current DensityEnhancement forhradiated YBa,Cu3 0u ,Physicu C191,199(1992) Berliner, R., The University of Missouri Researth Reactor (MURR),Neutmn Neus 2(4),13 (1991) Berliner, R; Smith, H.G.; Copley, J.; Trivisonno, J., The Structums of Sodium Metal, Phys Rev B (accepted) Borchers, J A; Salamon, M.B.; Erwin, RW.; Rhyne, JJ.; Nieuwenhuys, GJ.; Du, RR; Flynn, C.P.; Beach, RS., Structural and Magnetic Pmperties of Er Thin Films and EnY Superlattices. R Modification of the Commensurate Spin States, Phys Rev B44,11814 (1991) Casella, R.C.; Werner, SA, Electromagentic Acxx leration ofNeutrons, Phys Rev Iett 69,625 (1992) Childress, J.R; Chien, C.L.; Rhyne, JJ.; Erwin, RW., Small Angle Neutron Scattering ofNanodispersed Magnetic Particles, Journal ofMagnetism and Magnetic Materials 104-107,1585 (1992) Dahlberg, E.D.; Pieme D.T.;Yelon, W.B. editors, Proce< dings of the Fiflh Joint Magnetism and Magnetic Materials-Intennag Confemnce, JAppl Phys 70, 5733(642 (1991) , Dai, P.; Wang, S-K; Taub, H.; Buckley, J.E.; Ehrlich, S.N.; Lamse, J.Z.; Binnig, G.; Smith, D.P.E., X-Ray-Diffraction and Scanning Tunneling Micmcopy Studies of a Liquid Crystal Film Adsorbed on Single. Crystal Graphite, IBM Research Report RZ 2257 (#76787, if292); also submitted to Phys Rev B Dennison, J.R; Wang, S.K; Dai, P.; Angot, T.; Ehrlich, S.N.; Taub, H., Ultra-High Vacuum Chamber for - Synchrutmn X-Ray DifEaction fmm Films Adsorbed on Singh<rystal Surfaces,Rev SciInstrum 63, 3835(1992) Giebultowicz, T.M.; IGosowski, P.; Rhyne, J J.; Samarth, N.; Luo, H.; Funiyna, J.K, Incommensurate Antifernnnagnetic Orderin Strained Layer MnSdZnTe Superlattices, Physka B180-181,485 (1992) Hadjipanayis, G.C.; Wang, Y.Z.; Singleton, E.W.; Yelon, W.B., RarwEsth Nitrides and Carbides, A New Class of Permanent Magnet Materials, Joumal ofMat Eng & Performanm 1,2 (1992) + Hansen, F.Y/, Taub, H., Melting Echanism in Monolayers of Flexible Rod-Shaped Mokcules, Phys Rev t l Left 69,652(1992) Herbst, J.F.; Fuerst, C.D.; Yelon, W.B., Neutmn Powder Diffraction Study ofTbfe y B, Joumal ofApplkd Physics facwpt<d) , t Herwig, KW.; Simmons, RO., Inelastic Neutmn Scattering fmm Gaseous Hydnen, Molecular Physics 75 6),1393(1992) 167 i
l PUBLICATIONS - Physics, Chemistry and Materials Science Herwig, KW.; Trouw, F.R, Ethanol on Graphite: The Influence of Hydngen-Bonding on Smfam Melting, PhysimiReviewIstters (in press) Heuser, BJ.; Spooner, S.; Wignall, G.; Yelon, W.B.; Yelon, A; Petmva-Koch, V.; Ikiley, M.S.; Mobley, R; Miller, W.H., Characterization of Electrochemically Etched Si, Bull Am Phys Soc 37(1), 770 (1992) llindi, MXt; Kirrub, RL.; Nagy, H.J.; Schupp, G., Double K-Shell ionization in the Elecimn Capture Decay of"Fe, Phys Ree C44f 5),2237 (1991) Hor, PJ1.; Ikchtold, J.; Xue, Y.Y.; Chu, C.W.; H ungerfoni, E.V.; Maruyama, X.K; Backe, H.; Buskirk, F.R; Connors, S.M.; Jean, Y.C.; Farmer, J.W., Irradiation Efrects on Flux Pinning and J, in High Tempcrature Supenx>nductors,Physica C185-189,2311 (1991) Hutchinus, M.T.; Krawitz, AD., cditors, Measwement ofResidual and Applied Stms Using Neutwn Di/(metion, Klumer Academic Publishem, Donlrecht (1992) Kaiser, H.; Clothier, R; Werner, SA; Rauch, H.; W61witsch, H., Cohemnm and Spectral Filtering in Neutmn Interfennnetry, Phys Rev A45,31 (1992) Kaiser, I L; Werner, F A, Neutmn Interfemmetry A Unique Tool for Quantum Measurementa, Confemnae . Pmeeedings of the XIIth Moriond Workshop, la Ans, France, January 25 - February 1,1992 (in pmss) Ka e.er, H.; Werner, SA; Clothier, R; Rauch, H.; Wulwitsch, H., Quantum Interference ofNon-Gaussian . Wave Packets, Conference on The Foundations of Quantum Echanics, Santa Fe, NM, May 27-31, 1991, World Scientific Publishing Company PTE. Ltd., pp.115-123 (1992) Ltti. KV.; Barnes, C.L., The Hetematanic Chelation ofMixed Phosphine (or Arsine) and Phmphineoxide - Ligands with Re(V) Inorg Chem 31,3231 (1992) Katti, KV.; Cavell, RG., Application of Phosphoraniminephosphine Backbones to Early-Late Transition Metal Heterobimetallic Compound Formation Synthesis and Characterization ofa New 'H-Pd Hetembimetallic Framework CPCl ytin =PPh CH,PPh,. y PdCl, Organometallics 10,539 (1992) Katti, KV.; Cavell, R.G., Rearrangement of a Phosphorus-Carbon-Phosphorus Bond, Inorg Chem 30,2631 0 991) Katti, KV.; Singh, P.R; Barnes, C.L., Transition Metal Chenustry ofMain Group Hydrazides 1, Inorg Chem 31,4588(1992) Katti, KV.; Singh, P.R; Barnes, C.L.; Kopicka, K; Ketring, A.R; Vohrt, WA, The Potential of Phosphinimines as Building Bkcks for a New Generation of Radiopharmamuticals,Phosphoms, Sulfur and Related Elements (in pmss) Katti, KV.; Singh,1_R; Katti, KK; Kopicka, K; Volket, WA; Ketring, AR., First Exmnples of Hetematamic Chelation ofReOf*ReOf"'TcOf and PdCif with a Phosphine-Phosphineoxide (or a Ihphinimine) Bridged Bifunctional System, J Lobl Crimpd Radiopharm (acmpted) Katti, KV,; Singh, P.R; Ketring, AR; Volkert, WA, Functionalized Phosphorus Hydrazides as Novel Chelating Ligands to Transition Metals, Phosphoms Sulfur and RelatalElements (in ymss) . 1($
Physics, Chemistry and Materials Science PUBLICATIONS Ltti, KV.; Sngh, P.R;Volkert, WA; Ketring, AR; htti, KK, A New Neutml-Lipophilic Tc-99m - Complex with a Bishydrazine Phosphine (BHP ligand), int J Appl Rad andIsotopes 43,1151 (1992) - Klosowski, P.; Giebuhowicz, T.M.; Rhyne, J J.; Samaith, N.; Luo, IL; Furdyna, JK, Antiferromagnetism in Epilayers and Superlattices Containing Zine-Blended MnSe and MnTe, JAppl Phys 70,6221 (1991) Klosowski, P.; Giebultowicz, T.M.; Samarth, N.; Lua, IL; Furdyna, JK; Rhyne, JJ., Irwestigation of ZnMnTe Weakly Diluted fec Magnetic Semiconductors,Physica B180-181,114 (1992) Klosowski, P ; Giebultowicz, T.M.; Samarth, N.; Luo, H.; Fmdyna, J.K; Rhyne, JJ., Magnetic Critical Phenomena in FCC Antifermmagnets-Role of Strain and Dimensionality, Journal ofMagnetism and Magnetic Materials 104-107,1795 (1992) Krawitz, AD., Stress Measumments in Composites Using Neutmn Diffraction, Measumnent ofResidual and Applied Simss Using Neutmn Diffmetion, M.T. Hutchings and AD. Krawitz, editors, Klumer Academic Publishers, Donlrecht, pp. 405-420 (1992) Krill III, C.E.; Li, J.; Etti, C.; Samwer, K; Yelon, W.B.; Johnson, W.L % tic Mean-Square Displamment as an Indicator of the Crystal-to-Amorphous Transformatir_,a Non-Crys Solids (in press) Marasinghe, GK; Pringle, O A; Long, G J.; James, WJ.; Yelon, W.B.; Grandjean, F., A Neutmn Diffraction and Mussbauer Effeet Study ofthe Magnetic Structure ofY Te,)in)yB,JApplPhys 70, 6149(1991) Popovici, M.; Stoica, AD., Line Shifts in Crystal Powder Diffractrometers, JAppl Cryst 25,331 (1992) Popovici, M.; Yelon, W.B., On the Optical Design of Heat-Loaded Double Crystal Monochmmators for Synchmtmn Radiation, J Appl Cryst (acapted) Popovici, M.; Yelon, W.B., Design Relations for Synchmtmn Radiation Curved Two-Crystal Monochmmatora, Nuct Instr Meth (accepted) Priest, V.; Cowan, D.; Yasar, IL; Ross, F., ESR, Optical Absorption, and Lumines nce Studies of the Peroxy-Radical Defect in Topaz, Phys Rev B44(18),9877 (1991) huch, IL; Wolwitsch, H.; Clothier, R: Kaiser, I L; Wemer, SA, Time-of-Flight Neutron Interferometry, Phys Rce A46,49 (1992) Rhyne, J J.; Erwin, R.W.; Iknthers, JA: Salamon, M.B.; Tsui, F.; Du, R: Flynn, C.P., Magnetic Rare Earth Artificial Metallic Superlattices, The Science and Technolqqy ofNanostructured Magnetic Materials, Plenum hss,New York, pp.117 (1991) Rietzel, M.; Egert E.; Katti, KV.; Roesky, ILW., Formation ofSpirocyclic Imidophosphinato Complexes: Crystal Structure ofVanadium and Molybdenum Compounds,J Chern Soc Dalton Tmns 1285 (1991)
- j. Salamon, M.B.; Beach, RS.; Boithers, JA; Erwin, RW.; Flynn, C.P.; Matheny, A; Rhyne, JJ.; Tsui, F.,
Magnetism of Ram-Earthy and Ram-Earth /Lu Superlatti s and Films,JournalofMagnetism and Magnetic Materials 141-107,1729 (1992) 169
l PUBLICATIONS Physics, Chemistry and Materials Science Shi, N.; Arsenault, RJ.; Krawitz, A.D.; Smith, LF., Deformation-Induced Residual Stan Changes in sic Whisker Reinfomd 60G1 Al Composites, Afetallurgical Tmn.9 actions (in prtss) Srnith, L.F.; Krawitz, A.D.; Clarke, P.; Saimoto, S.; Shi, N.; Arwenault RJ., Ihsidual Stnses in Discontinuous Metal Matrix Composites, Matt Sci Eng (in prvss) Su, Z.; Farmer, J.W., Captum Kinetics of the Individual DX Center Irvels, Materials Scicna Forwn 83417, . 817(1992) Su, Z.; Farmer, J.W., Charge Redistribution in the Multiple levels of the DX Center, Applied Physics Irtter 59,1746(1992; Su, Z.; Farmer, J.W., The Echanism ofEkctnin Capture by DX Centers, Applitd Physics letter 59,1362 (1991) Tsui, F.; Flynn, C.P.; Salamon, M.B.; Bonhers, JA: Erwin, RW.; Rhyne, JJ., Layer Thickness Dependence ofAnisotropic Coupling in GdY Superlattices, Journal ofMagnetism andMagnetic Materials 104107,1901(1992) Vandersande, J.W.; Farmer, J.W., Neutmn Irradiation Damage in SiGe Alloys, Radiation E/Jit1s and Defirtsin Sdids118,125(1991) Wagoner, RA.; Bullard, B.R; Mullen, J.G.; Schupp, G., Pnrision Measurements ofIh<uil.Fne Fract. ion and Interference 4th Hundred Curie Sourcer.,, Hypergrw Inteructions (accepitd) Wagoner, RA; Mullen, J.G.; Schupp, G., Double Absorber Mussbauer Spectn* copy in *W, Physics Ictiers B279,25(1992) Wang, Y.Z.; Ilacljiparmyis, G.C.; Kim, A;; Sellmeyer, DJ.; Yelon, W.B., Structure and Magnetic Pmperties of RFe,V,N, Compounds, JournalofMaguaistn and Magnetic Materials 1st-107,1132 (1992) Werner, SA; Rhyne, JJ., Spin Density Waves in Spin Glasms, Ram-Earth Metallic Alloys, and Artificial Superlattices, Recent Pmgress in Random Magnets, D.M. Ryan, editor, World Scientific Publishem (1992) Wom*r, DL; Kaiser, H.; Kulasebre, R; Torbet, J., Phase Determination Using Transform and Contrast Variation Methods in Neutmn Diffraction Studies ofBiological Lipids, SPIEPnmdings 1767, Inverse Pmblems in Scattering and Imaging, M. Fiddy, editor (in press) Yekm, W.B , George, P.; Zhum, J.; Goldfadi, R; Ramanan, V.RV., editors, Proacdings ofthe Intanational Magnetism Conferrnoe Intermag'92, IEEE Transm.tions on Magnetism, (in pnss) Yekm, W.R; 1huljipanayis, G.C., Neutron Diffraction Studies of Rare Earth Transition Metal Nitrides, IntermagV2,IEEE Tmnsactions on Magnetics 23 (in press ^) 170
7 Engineering and Technology PUBLICATIONS Auman, L.; Miller, W.H.; Graham, C.; Stretch, D.; West, L.; Welty, T., An Inter-Comparison of Neutron Dosimeters and Detectors for In-Containment Dosimetry, Health Physics 62(2),191 - (February 1992) Hassan, N.; Hines, A.L.; Ghosh, T.K.; Loyalka, S.K.; Ketring, A.R., New Apparatus for Measuring Radon Adsorption on Solid Adsorbents,Ind Eng Chem Res 30(9),2205 (1991) Johnsca, J.C.; Langhorst, S.M.; Loyalka, S.K.; Volkert, W.A.; Ketring, A.R., Calculation of Radiation Dose at a Bone-to-Marrow Interface Using Monte Carlo Modeling Techniques - (EGS4), Journal ofNuclecr Medicine 33(4),623 (April 1992) McKibben, J.C.; Rhyne, J.J., Update on the University of Missouri-Columbia Reeearch Reactor - Upgrade, Trans Am Nucl Soc 64,244 (1991) McKibben, J.C.; Rhyne, J.J., Update on the University of Missouri-Columbia Research Reactor Upgrade, Proceedings of the 2nd Meeting of the International Group ofResearch Reactors, Saclay, France (in press) Miller, W.H.; Berliner, R., A DSP-Based Analog-to-Digital Convertor for Nuclear Radiation - Spectrosocopy, Trans Am Nucl Soc (in press) Miller, W.H.; Brugger, R.M.; Meyer, W., Measurements of Hydrogen at the PPM-levels Utilizing the Modified Notched Neutron Spectrum Technique, Trans Am Nucl Soc 65,185 (1992) Miller, W.H.; Kumar, A.; Meyer, W., New Techniques for Measuring Low Levels of Hydrogen or - Uydrogen Bearing Materials in Solids, Journal ofNondestructive Evaluation 10(4),151 (1991) Miller, W.H.; Neumeyer, G.M.; Langhorst, S.M., Nuclear Science and Engineering Workshop for Secondary Science Teachers, Transactions ofAmerican Nuclear Society 65,15 (1992) Zinn, K.R.; Morris, J.S.; Fairfax, C.A.; Berliner, R.R.; Liu, H.B.; Brugger, R.M., The Development of a Rectilinear Scanner Utilizing High Resolution Gamma-Ray Detection, Journal of Radioanalytical and Nuclear Chemistry 157(1),15 (1992) 171
p ! PUBLICATIONS Life Sciences ; I Anderson, C.J.; Connett, J.M.; Schwarz, S.W.; Rocque, P.A.; Guo, L.W.; Philpott, G.W.; Zinn, KR; -
- Meares, C,F.; Welch, C.J., Copper-64 Labehd Antibodies for PET Imaging, Journal o/ Nuclear hiedicine tin press)
Anderson, C.J.; Schwarz, S.W.; Rocque, P.A.; Connett, J.ht; Guo, L.W.; Philpott, G.W.; 7 inn, KR; Meares, C.F.; Welch, C.J., Copper-Labeled Antibodies for PET Imagmg, Journal ofLabeled , Compounds and Pharmaceuticals (accepted) ' Anderson, H.D.; Morris, J.S., Contaminatirm Studies in the Use of Human Nails for Dietary Studies: The EITect af Clippers, Journal ofRadioanalytical andNuclear Chemistry, Articles, 158(2),251 (1992) E Anderson, J.H.; Goldberg, J.A.; Bessent, RG.; Kerr, D.J.; McKillop, J.IL; Cooke, T.G.; McArdle, C.S., The ~ ' Use of Glass Yttrium-90 Microspheres for Colorectal Liver Metastases, British Journal ofCancer (paper describes work performed on TheraSphere@ developed at MURR/UMR) Baskett, C.R; Spr.te, V.L.; Mason, htM; Reams, C.L.; Morris, J.S., The Determination of Selenium in Urine, Journal ofRadioanalytimi and Nuclear Chemistry (accepted >_ t Brown, RF.; Lindemuth, L.C.; Day, D.E., " Holmium-Containing Glass for Internal Radiotherapy of Tumors, Nuct Afed Biol 18(7),783 (1991) l Corlija, M.; Katti, KV.; Volkert. W.A.; Hoffman, T.J.; Higgenbotham, C.; Holmes, R.A., Formation of a -i Stable Tc-99m-Trishydrazide Phosphine Oxide (Tc-99m-THP) Appl Radiat Isot (in press) - I DiZio, J.P.; Anderson, C.J.; Davison, A.; Ehrhardt, G.J.; Carlson, KE.; Welch, M.J.; Katzenellenbogen, 1 J.A., Technetium. and Rhenium-Labeled Progestins: Synthesis, Receptor Binding and In Vien , Dist ribution of an "b-Substituted Progestin Labeled with Technetium-99 and Rhenium-186, Journa! ! o/ Nuclear Afedicine 33 A ), 558 (1992) i i Ehrhardt, G.J.; Symes, Sc, Guimon, RK; Zinn, K.R, Radioisotope Generators ibr Nuclear Medicine 'r Based on Fajan's Absorption on Glass Microspheres, Journal ofNuclear Science and Engineering (in ; press) Graham, N.M.H.; Somnsen, D.; Odaka, N.; Brookmeyer, R.; Chan, D.; Willett, W.C.; Morris, J.S.; Saah, A.J., Relationship of Scrum Copper and Zine Levels to HIV-1 Seropositivity and Progression to Aids, Journal ofAcquimd immune Deficiency Syndn>mes 4. 976 (1991) ! Liu, H.B.; Brugger, RM.; Shih, J-L.A., Neutron Capture Therapy with 2"U Seeds, Afedical Physics 19(3), . 705 (May/ June 1992) ! I lengnecker, M.P.; Taylor, P.R; Levander, O.A.; Howe, M.; Veillon, C.; McAdam, P.A.; Patterson, K.Y.; i Holden,1M.; Stampfer, M.J.; Morris, J.S ; Willett, W.C., Selenium Tissue Levels and Dietary Intake in Relation to Health Status in a Seleniferous Area, American Journal ofEpidemiology (accepted) . Mason, M.M.; Reams, C.L.: Baskett, C.K.; Spate, V.L.; Morris, J.S.; Mills S., Determination of Total and Bound Solenium in Sera Via INAA, Journal ofRadioanalytical and Nuclear Chemistry, (1992) (accepted)
)
172
Life Sciences PUBLICATIONS Maxon III, H.R; Thomas, S.R; Hertzberg, V.S.; Schroder, LE.; Englaro, E.E.; Samaratunga, R.; Scher, H.L; Moulton, J.S.; Deutsch, E A; Deutsch, KF.; Williams, C.C.; Ehrhardt, G.J., Rhenium-186 Hydroxyethylidene Diphosphonate for the Treatment of Painful Osseous Metastases, Seminars in Nuclear Medicirt(in press) i Maxon HI, H.R; Thomas, S.R; Hertzberg, V.S.; Schroder, L.E.; Englaro, E.E.; Scher, H.L; Moulton, J.S.;
- ^.
Deutsch, E A; Deutsch, KF.; Williams, C.C.; Ehrhardt, G.J., Rhenium-186 Hydroxyethylidene Diphosphonate for the Treatment of Painful Osseous Metastases,Nucleair Geneeskundig Bulletin, . , ISSN 0169-1279, No. 2,14 (1992) -! Milunsky, A.; Morris, J.S.; Hick, H.; Rothman, KJ.; Ulcickas, M.; Jick, S.S.; Shoukimas, B.S.; Willett, W.C., Maternal Zinc and Fetal Neutral Tube Defects, Teratology 46,341 (1992) > Morris, J.S., The Missouri University Research Reactor Nuclear Analysis Program, Journal of ' Radioanalytical and Nuclear Chemistry (accepted) : Morris, J .S.; Spate, V.L.; Baskett, C.K.; Mason, M.M.; Reams, C.L.; Hunter, D.; Willett, W.C., Determination of Fluoride in Human Nails Via Cyclic Instrumental Neutron Activation Analysis (ClNAA), Journal ofRadioanalytical and Nuelcar Chemistry, (accepted) i Prohaska, J.R.; Sunde, KA.; Zinn, K.R. Livere from Copper-Deficient Rats hve Lower Glutathione f Peroxidase Activity and mRNA Levels but N,rmal Liver Selenium Levels, Journal o/ Nutritional Biochemistry (in press) Sahini, S.; Stampfer, M.J.; Morris, J.S.; Hennekens, C.H., Prediagnostic Sertun Selenium and Risk of ' , Myocardial Infarction Among US Physicians, Journal ofAmerican Medical Association (JAMA) (accer.ted)
~
, Shih, J-LA: Brugger, R.M., Gadolinium as a Neutron Capture Therapy Agent, Medical Physics 19(3), 733 tMay/ June 1992) [ Shih, J-LA; Brugger, RM.4 Neutron Induced Brachytherapy: A Combination of Neutron Capture i Therapy and Brachytherapy, Medical Physics 19(2),369 (Mar /Apr 1992) Singh, P.R; Corlija, M.; Troutner, D.E.; Ketring, A.R; Volkert, WA, Synthesis, Characterization and Biodistribution Studies of a Neutral-Lipophilic Tc-99m N,S, Chelate, Int J Radiat Appl Instrum Part B Nuct Med Biol(in press) Singh, P.R; Volkert, WA; Ketring, A.R; Troutner, D.E.; Katti, KK.; Katti, K.V., A New Chelating Heterodifunctional Phosphorus-Nitrogen Ligand for Radiolabeling of Proteins, J Labl Compd - Radiopharm (in prers) Volkert, WA; Goeck.eler, W.F.; Ehrhardt, G.J.; Ketring A.R, Therapeutic Radionuclides: Production and Decay Property Considerations, Journal ofNuclear Medicine 32,174 (1931) Volkert, WA; Singh, P.R; Katti, KK.; Ketring, A.R; Katti, K.V., A New and Versatile Multifunctional Phosphorus Hydrazide Ligand for Formulating Neutral-Lipophilic Complexes of **>Tc, "Re and -
'*Pd Radioneclides, J Labeled Compd Radiopharm (accepted) ;
i Zinn, KR; Morris, J.S.; Fairfax, C.A.; Berliner, RR; Liu, H.B.; Brugger, RM., The Development of a i Rectilinear Scanner Utilizing High Resolution Gamma-Ray Detection, Journal ofRadioonalytical ' andNuclear Chemistry, Articles 157(1),15 (1992) i t 173 l t
n; v i PUBLICATIONS Natural Sciences -; i
^
Bove, F.J.; NefT, H.; Lou, B.; Medrano, S., Early Classic Ceramic Traditions of Pacific Coastal Guatemala: Compositional Evidence, Chemical Characterization of Ceramic Pastes in , Archaeology, H. NefT, editor, Prehistory Press, Madison, WI, April,1992 Braswell, G.E.; Glascock, M.D., A New Obsidian Source in the Highlands of Guatemala, Ancient , Mesoamcrica 3,49 (1992) Clark, C.; Glascock, M.D.; Neff, H., Neutron Activation Analysis of Late Woodland Ceramics from the Lake Superior Basin, Chemical Chameterization ofCeramic Pastes in Archaeology, H. Neff, editor, Prehistory Press, Madison, WI, April,1992 Cobean, R.H.; Vogt, J.R.; Glascock, M.D.; S%cker, T., High-Precision Trace-Element - Characterization of Major Mesoamerican Obsidian Sources and Further Analyses of Artifacts . from San Lorenzo Tenochtitlan, Mexico, Latin American Antiquity 2,69 (1991) Coveney, R.M. Jr; Murowchick, J.B.; Grauch, R I.; Nansheng, C., Field Relations, Origins, and Resource Implications for Platiniferous Molybdenum-Nickel Orcs in Black Shales of South. : China, Exploration and Mining Geology 1,21 (l992) , Elam, J.M.; Carr, C.; Glascock, M.D.; NefT, L., Ultrasonic Disaggregation and INAA of Textural Fractions of Tucson Basin and Ohio Valley Ceramics, Chemical Characterization ofCeramic Pastes in Archaeology, H. Neff, editor, Prehistory Press, Madison, WI (April,1992) Elam, J.M.; Glascock, M.D.; NeiT, H., Source Identification and Hydration Dating of Obsidian - Artifacts from Oaxaca, Mexico: Preliminary Results, Precolumbian Arrhaeometry, Getty Conservation Institute publishers, Los Angeles, CA fin press) Fish, P.R.; Fish, S.K.; Whittlesey, S.; Neff, H.; Glascock, M.D.; Elam, J M., An Evaluation of the Production and Exchange of Tanque Verde Red-on-Brown Ceramics in Southern Arizona,
. Chemical Characterization of Cemmic Pastes in Archaeology, H. NeiT, editor, Prehistory Press, Madison, WI (April,1992)
Glascock, M.D., Characterization of Archaeolog cal Ceramics at MURR by Neutron Activation i Analysis and Multivariate Statistics, Chemical Characterization of Ceramic Pastes in Archaeology, H. Nefr, editor, Prehistory Press, Madison, WI (April,1992) Glascock, M.D., Recent Advances in the Investigation of New World Obsidian, Prreolumbian Archaeometry, Getty Conservation Institute publishers, les Angeles, CA (in press) 174
5 Natural Sciences PUBLICATIONS Glascock, M.D.i Neff, H.; Stryker, K.S.; Johnson, T.N., Sourcing Arcl- sological Obsidian by an Abbreviated NAA Procedure, Journal ofRadioonalytical Chemistry (in press) Hoard, R J.; Glascock, M.D.; Neff, H.; Elam, J.M.; Holen, S.R., Neutron Activation Analysis of - Stone from the Chadron Formation and a Clovis Site on the Great Plains, Journal of Archaeological Science (in press) Hodge, M.G.; Neff, H.; Blackman, M.J.; Minc, L.D., A Compositional Perspective on Ceramic Production in the Aztec Empire, Chemical Characterization of Ceramic Pastes in Archaeology, H. Nefr, editor, Prehistory Press, Madison, WI (April,1992) Hodge, M.G.; Nefr, H.; Mine, L D.; Blackman, M.J., The Regional Structure of Black-On-Orange Ceramic Production in the Aztec Empire's Heartland, Latin American Antiquity (in press) NefT, H., editor, Chemical Characterization of Ceramic Pastes in Archaeology, Prehistory Press, ; Madison, WI (April,1992) Neff, H., Int roduction, Chemical Characterization of Ceramic Pastes in Archaeology, H. NefT, editor, Prehistory Press, Madison, WI (April,1992) Neff, H , Theory, Sampling and Analytical Techniques in the Archaeological Study of Prehistoric Ceramics, American Antiquity (in press) Neff, H.; Bishop, R.L.; Sisson, E.B.; Glascock, M.D.; Sisson, P.R., Neutron Activation Analysis of , Late Postelassic Polychrome Pottery from Central Mexico, The Mixteca-Puebla Concept in Mesoamerican Archucology: A Further Examination, H.B. Nicholson and E. Quibones Keber, editors, Labyrinthos Press, Culver City, CA (in press) ' NefT, H.; Bove, F.J.; Lou, B.; Piechowski, M.F., Ceramic Raw Materials Survey in Pacific Coastal Guatemala, Chemical Characterization of Ceramic Pastes in Archaeology, H. NeIT, editor, Prehistory Press, Madison, WI (April,1992) Stark, B.L.; Heller, L.; Glascock, M.D.; Elam, J.M.; Neff, H., Obsidian Artifact Source Analysis for the La Mixtequilla Regen, South-Central Veracruz, Mexico. Latin American Antiquity (accepted) 175
i l ' PATENTS ISSUED OR FILED July 1991 - June 1992 Brugger, R.M.; Day, D.E.; Ehrhardt, G.J., Brachytherapy Seeds, Discloced Day, D.E.; Ehrhardt, G.J., Composition and Method for Radiation Synovectomy of . , Arthritic Joints, Granted (US #5,039,326) ~ -l Ehrhardt, G.J., Glass Microspheres, Granted Osrael #77079) Ehrhardt, G.J., Glass Microspheres, Granted (European no. 86900686.6) Ehrhardt, G.J., Improved Targetry For Rare-Earth Targets, Disclosed Ehrhardt, G.J., Method and Apparatus for the Generation of Radioisotopes, Granted (US
#07/665,33D
'L Ehrhardt, G.J.; Liang, Q., New W-188/Re-188 Generator Chemistry, Disclosed -
Ehrhardt, G.J.; Zinn, K.R.; Day, D.E., Rhenium-Labeled Protein or Polypeptide Microspheres for Radiation Synovectomy, Submitted Katti, K.V., Production of Trifluoracetates of Transition Metals and Lanthanides from the Water Catalyzed Reactions of Trifluoracetic Acid with the Metals, Disclosed ' Katti, K.V.; Cavell, R.G., Carbonylation of Methanol Using a Novel Transition Metal il Catalyst Precursor, applications filed in USA, Japan, Poland, Mexico and European
- Community (EPC)
Katti, K.V.; Volkert, W.A.; Ketring, A.R., New Multifunctional Ligands for Potential Use 4 in the Design of Therapeutic or Diagnostic Radiopharmaceutical Imaging Agents, Submitted 1 Katti, K.V.; Volkert, W.A.; Ketring, A.R., Multifunctional Ligand for Use as a Diagnostic or Therapeutic Pharmaceutical, Submitted (US #SN 649,142); applications filed in Australia, Canada, Japan and EPC Miller, W.H.; Berliner, R., A DSP-Based Analog-to-Digital Convertor, Disclosed l Popovici, M.; Heuser, B.J.; Yelon, W.B., Neutron Monochromator for Small Angle Scattering, Disclosed I Vanderheyden, J-L.; Su, F-M.; Ehrhardt, G.J., Soluble Irradiation Targets and Methods for the Production of Radiorhenium, Granted (US #5,053,186) 1 176 7
t Physics, Chemistry and Materials Science PRESENTATIONS. , Invited Farmer, J.W., Radiation Effects in Materials, Cooper Nuclear Power Group, Nuclear Engineering Seminar series, University of Missouri-Columbia, August 6,1991 - . Herwig, K., Neutron Diffraction and Inelastic Scattering from a Two-Dimensional Hydrogen Bonded System: Ethanol on Graphite, Physics Condensed Matter Seminar series, University . of Missouri-Columbia, November 20,1991 Kaiser, H., Coherence Experiments with Thermsl Neutrons, Physics Condensed Matter Seminar series, University of Missouri-Columbia, September 18,1991 > Kaiser, H., An Overview of Neutron Interferometry, Argonne National Laboratory-IPNS, Argonna, IL, December 20,1991 Kaiser, H., Neutron Interferometry: A Unique Tool for Quantum Measurements, XIlth Moriond Workshop, Les Arcs, France, January 25 - February 1,1992 Katti, ILV., New Tc-99m and Re-188 Complexes Derived from Multifunctional Phosphorus Hydrazides, Center for Radiological Research, Columbia, MO, August 10,1991 Katti, K.V., .New Directions in Ligand Design for Chemistry with the "Early and Late" Transition Metals, University of Missouri-Columbia Chemistry DYNAMITE @ Seminar series, November 2(i,1991
.t Katti, K.V., First Examples of Heteroatomic Chelation of 188ReO4-99mTcO4- and PdCl42- with a Phosphine-Phosphineoxide (or a phosphinimine) Bridged Bifunctional System, Ninth International Sympwium on Radiopharmaccutical Chemistry, Paris, France, April 6-10,-
1992 l Katti, K.V. Linear, Cyclic and Polymeric Phosphazines as Building Blocks for New Tc-99m, Re-188 and Pd-109 Complexes, Anorganisch Chemisch Institut, University of Gottingem, West Germany, April 13,1992 Katti, K.V., Biochemical and Catalytical Applications of Transition Metal Chemistry Derived from Novel Phosphorus-Nitrogen Systems, Anorganische Chemisch Laboratorium, University of Amsterdam, The Netherlands, April 16,1992-Katti, K.V.. Synthesis, Structure and Reactivity Aspects of New Multifunctional Phosphorus-Nitrogen Compounds, MURR, June 3,1992 Katti, K.V.; Singh, P.R.; Ge, Y.W.; Volkert, W.A.; Ketring, A.R.; Corlija, M.; HofTman, T.J.; Holmes, R.A., The Potential of Unconventional Phosphorus-Nitrogen Backbone Ligands for ' Use in Formulating New Radiopharmaceuticals,39th Annual Meeting of the Society of Nuclear Medicine, Los Angeles, CA, June 9-12,1992 Katti, K.V., New Multifunctional Phosphorus Hydrazides and Phosphinimines for Complexation with Electron Poor and Electron R;ch Metals, Zynaxis Cell Science, Ir.c., Malvern, PA, June 22,1992
'i t
177
I b PRESENTATIONS Physics, Chemistry and Materials Science Krawitz, A.D., Residual Stress Analysis Using Neutron Diffraction, Chalmers University of Technology, G6thenberg, Sweden, August 12,1991 Krawitz, A.D., Residual Stress Measurements in Composites Using Neutrons, Chalmers i University of Technology, G6thenberg, Sweden, August 13,1991 Popovici, M., Curved Two-Crystal SR Monochromators, Advanced Photon Source, Beamlines Group, Argonne National Laboratory, Argonne, IL, February 28,1992 , Popovici, M., Focusing Techniques in Neutron (and SR) Crystal DifTractometry, Brookhaven National Laboratory, Upton, NY, March 27,1992 ' Popodei, M., Focusing Techniques in Neutron Scattering - Elastic and Inelastic, Oak Ridge National Laboratory, Oak Ridge, TN, June 15,1992 Rhyne, J J., Magnetism in Rare Earth Metallic Superlattices,39th Midwest Solid State , Confemnce, Ames, IA, September 27-28,1991 Rhyne, J.J., Neutron Scattering: A Window on Magnetic Phenomena, Physics Dept. Colloquium, Kansas State University, Lawrence, KS, December 5,1991 Rhyne, J.J., Magnetic Exchange Interactic.ns in Rare Earth Artificial Metallic Superlattices, Physics Dept. Colloquium, Washington University, St. Louis, MO, February 26,1992 Rhyne, J.J., The MU Research Reactor (MURR) and Neutron Applications in Materials Science, Nuclear Engineering seminar series, University of Missouri-Columbia, March 31,1992 Schupp, G., M6ssbauer Scattering Studies with High-Intensity Sources, Physics Seminar, . Tennessee Technical University, Cookeville, TN, September 24,1991 Schupp. G., Mussbauer Scattering Studies with High-Intensity Sources, Physics Colloquium, University ofIdaho, March 30,1992 Schupp, G., M6ssbauer Scattering Studies with High-Intensity Sources, Physics Colloquium, Boise State University, Boise, ID, April 3,1992 Schupp, G., M6ssbauer Scattering Studies with High-Intensity Sources, Physics Colloquium, Idaho State University, Pocatella, ID, April 6,1992 Schupp, G., Mussbauer Scattering Studies with High-Intensity Sources, Physics Colloquium, Utah State University, Logan, UT, April 8,1992 Taub, H., The Multilayer Structure and Growth of Simple Films Studied by Neutron and , Synchrotron X-Ray DifTraction, Chemistry Department Seminar, University of California-Berkeley, November 1,1991 Taub, H., The Multilayer Structure and Growth of Simple Films Studied by Neutron and , Synchrotron X-Ray Diffraction, Physics Department seminar, Washington University, St. Louis, MO, February 3,1992 178
. - ~ .-
Physics, Chemistry and Materials Science PRESENTATIONS
. Werner, S.A., Is Copper-Manganese a Spin Glass?, International Conference on Magnetism, ICM-91, Edinburgh, Scotland, September 4,1991 Werner, S.A., Cu-Mn: The Prototype Spin Glass is Not a Spin Glass, Physics Seminar, University of Missouri-Kansas City, November 1,1991 Werner, S.A., Spectral Filtering in Neutron Interferometty, Southeast Section of the American Physical Society meeting, Durham, NC, November II,1991 Werner, S.A., Neutron Interferometry: Quantum Interference on a Macroscopic Scale, Physics department seminar, University of Texas, Austin, January 22,1992
+
Werner, S.A., Neutron Interferometry: Quantum Interference on a Macroscopic Scale Physics department seminar, Arizona State University, Tempe, AZ, January 30,1992 , Werner, S.A., Is Cu-Mn a Spin Glass?, Physics department seminar, McGill University,- l Montreal, Canada. February 13,1992 Werner, S.A., Neutron Interferometry-Quantum Interference on a Macroscopic Scale, Physics department seminar, McGill University, Montreal, Canada, February 14,1992 Werner, S.A., Neutron Interferometry, Physics department seminar, Northeast Missouri State' University, Kirksville, MO, April 1,1992 Winholtz, R.A., Microstress in the Mechanical Behavior of Materials, Physics Condensed Matter Colh>quium, University of Missouri-Columbia, October 9,1991 Yelon, W.B., Structural Studies of Rare Earth-Iron Nitrides by Neutron Diffraction, Physics Department, Washington University, St. Louis, MO, March 2,1992 , Yelon, W.B., Neutron DifTraction Studies of Rare Earth Transition Metal Nitrides, INTERMAG'92 Conference, St. Louis, MO, April 12-15, 1992 Contributed Ding. X ; Farmer, J.W., Lattice Parameter Changes in Neutron Irradiated YBa2Cu307, March meeting of the American Physical Society, Indianapolis,IN, March 16-20,1992 Dozier, W.D.; IIerwig, K.W.; Shinar, R.; Jia, II.; Shinar, J., Study of Short-Range Motion of Atomic Ilydrogen in Amorphous Silicon by Neutron Re0ectometry,1992 Spring Meeting of the Materials Research Society (MRS), San Francisco, CA, April 26 - May 1,1992 Dozier, W.D.; Shinar, R.; Jia, H.; Shinar, J., Neutron Reflectometry (NR) Study of Short-Range II , Motion in a-Si:li, American Physical Society March meeting, Indianapolis,IN, March 16-20, 1992 Farmer, J.W., Neutron Diffraction and Defect Studies of High Tc Superconductors, Midwest , Superconductivity Consortiurn, West Lafayette, IN, August 5,1991 179
PRESENTATIONS . Physics, Chemistry and Materials Science - > Farmer, J.W., Radiation Effects and Hardening, Lecture for Cooper Nuclear Station Visit, , Columbia, MO, August 12,1991 Farmer, J.W., Neutron Diffraction and Defect Studies of High Tc Superconductors, Midwest ;i Suepreonductivity Consortium, Columbus, OH, January 8,1992 Farmer, J.W.; Su, Z., Capture Kinetics of t.he Individual DX Center Levels,16th International l Conference on Defects in Semiconductors, Bethlehem, PA, July 21-25,1991 Farmer, J.W.; Su, Z., Nonexponential Optical Ionization Kinetics of DX Centers in AIGaAs, March meeting of the American Physical Society, Indianapolis, IN, March 16-20,1992 - Hansen, F.Y.; Taub, H., Melting Mechanism in Monolayers of Flexible Rod-Shaped Molecules, March meeting of the American Physical Society, Indianapolis,IN, March 16-20,1992 1 Herwig, K.W.; Trouw, F., The Melting Behavior of Ethanol Physisorbed on Graphite, APS March meeting. Indianapolis, IN, March 16-20,1992 lleuser, B.J.; Spooner, S.; Wignall, G.; Yelon, W.B.; Yelon, A.; Petrova-Koch, V.; Boley, M.S.; Mobley, R.; Miller, W.H., Characterization of Electrochemically Etched Si, APS March meeting, Indianapolis, IN, March 16-20,1992 Kirk, M.A.; Farmer, J.W., Flux Pinning by Neutr m Irradiation Induced Defects, Gordon - Conference on Superconductivity, Oxnard, CA, January 15,1992 Mitchell, J.; Ross, F.K.; Cowan, D.L., A Structural Study of Radiation-Induced Damage in Topaz, lf American Crystallography Association Annual Meeting, Toledo, OH, July 21-26,1991 Popovici, M.; Yelon, W.B., Design Relations for Synchrotron Radiation Curved Two-Crystal Monochromators, National Conference on Synchrotron Radiation Instrumentation, Baton Rouge, LA, October 28-31,1991 Tang, Y.Y.; Yelon, W.B.; Heuser, B.J., Neutron Diffraction Studies of Hydrogen in Ti-Al Alloys, 1991 Gordon Conference on Hydrogen / Metal Systems, Tilton, NH, July 15-19,1991 ) l Trouw, F.; Herwig, K.W., The Melting Behavior of Ethanol Physisorbed on Graphite,' American 1 Physical Society meeting, Indianapolis, IN, March 16-20,1992 Wagoner, R.A.; Mullen, J.G.; Schupp, G.; Yelon, W.B., Precision Measurements of Elastic 5 Scattering from Alkali Halides, March meeting of the American Physical Society. Indianapolis, IN, March 16-20,1992 Wang, S-K ; Dai, P.; Angot, T.; Ehrlich, S.N.; Larese, J.Z.; Taub, H., Synchrotron X-Ray Diffraction Study of the Multilayer Growth of Xe on AgG11): Preliminary Results, March meeting of the American Physical Society, Indianapolis, IN, March 16-20,1992 - t Xie, Q-Y.; Hu Z.; Mitchell, J.; Schlemper, E.; Ross, F.K., Electron Density Analysis with X-Ray and Neutron Diffraction Data, American Crystallography Association Annual Meeting, Toledo, OH, July 21-26,1991 180 l I
Engineering and Technology PRESENTATIONS. Invited Ehrhardt, G.J.; Volkert, W.A., Ketring, A.R., Production ofIsotopes at Nuclear Reactors',4th
' International Symposium on the Synthesis and Applications ofIsotopes and Isotopically Labelled <
Compounds, Toronto, Canada, September 3-7,1991 Kunze, J.F., State of the Nuclear Engineering Program at the University of Missouri-Columbia, MU Nuclear Engineering Seminar Series, University of Missouri-Columbia, September 3,1991 liyalka, S.K., Risk Assessment, .MU Nuclear Engineering Seminar Series, University of Missouri-Columbia, October 29,1991 McKibben, J.C., Status of the TRUMP-S Litigation, Test. Research and Training Reactors meeting, Cambridge, MA, October 23-25,1991 McKibben, J.C., The University of Missouri hsearch Reactor,1AEA Technical Committee Meeting on hscarch Reactor Problems of the 1990s, Dhaka, Bangladesh, June 22 26,1992 L McKibben, J.C.; Rhyne, J.J., Status of the MURR Upgrade, Test, Researth and Training haetors meeting, Cambridge, MA, October 23-25,1991 McKibben, J.C.; Rhyne, J.J., Update on the University of Missouri-Columbia Research Reactor Upgrade, Winter 1991 American Nuclear Society meeting, San Francisco, CA, November 10-14,1991 - McKibben, J.C.; Rhyne, J.J., Update on the University of Missouri-Columbia Research Reactor Upgrade, l Second Meeting of the International Group of Research Reactors OGORR), Saclay, France, May 18-19,1992 McNally, M.G., TRUMP-S Research, MU Chemical Engineering Seminar series, University of Missouri - Columbia, February 25,1992 Meyer, VI.A.; Hultsch, R.A., Status of Efforts to Obtain a Spent Fuel Shipping Cask, presented by J.C. McKibben, Test, Research and Training Reactors meeting, Cambridge, MA, October 23-25,1991 i Meyer, W.A.; Tritschler, N.E.; Hudson, R.A.; M uren, P.,L, Randolph, M.L., Reactor Startup Demonstration, Summer 1992 Nuclear Science for Secondary Teachers Workshop, University of Missouri-Columbia, June 24,1992 .
.+
Riggle, K.J., Environmental Monitoring of Uranium and Neptunium Using Epithermal Neutron - ,.. Activation Analysis, MU Nuclear Engineering Seminar, University of Missouri-Columbia, April 7, 1992 Storvick, T.S., Japanese Plan tu Reprocess Nuclear Fuel, Summer 1992 Nuclear Science for Secondary Teachers Workshop, University of Missouri-Columbia Nuclear Engineering Department, June 24, 1992 Contributed Kunze, J.F.; Smith, D.; Bennett, P.C., Contamination Clean Up and Subsequent Weeping Observation on .; Metal Shipping Cask Surface Materials, Annual Meeting of Health Physics Society, Washington, DC, July 25,1991 181
w PRESENTATIONS Life Sciences r Invited ' Chaudhuri, T., Radioimmunodiagnosis and Treatment of Ovarian Cancer, American Society for Microbiology and Immunology Symposium, Columbia, MO, April 3,1992 Chaudhuri, T., Radioimmunodiagnosis and Treatment of Ovarian Cancer, MURR, April 8,1992 ; i Ehrhardt, G.J.; Volkert, W.A.; Ketring, A.R., Production ofIsotopes at Reactors,4th International Symposium on the Syribesis and Applications ofIsotopes and Isotopically Labeled Compounds, Toronto, Ontario, September 3-8,1991 Ehrhardt, G.J., Nuclear Medicine Applications of Radioact,ive Microspheres, MU Chemical Engineering Department seminar, Columbia, MO, October 22,1991 Ehrhardt, G.J., Applications of Radioactive Microspheres for Liver and Kidney Malignancies and Rheumatoid Arthritis Therapy, Brookhaven National Laboratory, Upton, NY, February 26, 1992 Ehrhardt, G.J., Recent Developments in Nuclear Medicine Research at the University of Missouri Research Reactor, Iligh Country Nuclear Medicine Meeting, Vail, CO, March 16-20, 1992 Ehrhardt, G.J., Nuclear Medicine Radiotherapy with Labeled Microspheres or with Re-186/Re-188, MU Chemistry seminar series, University of Missouri-Columbia, June 5,1992 Ehrhardt, G.J.; Curtis, R.L.; Lattimer, J.C.; Day, D.E.; Bartlett, B.; Quesenberry, J.; Ross, G.; Volkert, E.W.; Lanigan, J.P.; Evans-Blumer, M., Investigation of Pre-Operative Sterilization ' of Kidney Cancers Using Intra-Arterial Samarium-153 Microspheres,39th Annual Meeting of the Society of Nuclear Medicine, Los Angeles, CA, June 9-12,1992 , Jimenez, H.N., Synthetic Pathways to Metal Labeled Steroids of High Receptor Binding Affinity for Therapy, MU Chemistry DYNAMITE @ seminar series, University of Missouri-Columbia, Mareh 31,1992 > Ketring, A.R., Radiotherapeutic Agents for the Treatment of Pain Associated with Metastatic Bone Cancer, Brookhaven National Laboratory Medical Department, Upton, NY, April 29, , 1992 ! Ketring, A.R., Development of Therapeutic Bone Agents, MU Chemistry seminar series, University of Missouri-Columbia, June 25,1992 Lang, L., Radiolabeling Proteins with Bifunctional Chelating Agents, MURR, May 4,1992 Liang. Q., New Peroxide Process for W-188/Re-188 Gel Radioisotope Generators, Schlemper Research Group-University of Missouri-Columbia, January 29,1992 Morris, J.S., Determination of F in Biological Samples via NAA, MU Chemistry DYNAMITE
- seminar series, University of Missouri-Columbia, March 10,1992 182
Life Sciences PRESENTATIONS L L Morris, J.S.; Spate, V.L.; Baskett, C.K.; Mason, M.M.; Reams, C.L., Determination of Fluoride in Human Sera Via Cyclic Instrumental Neutron Activation Analysis (CINAA), Second International Symposium on Nuclear Analytical Chemistry (NAC-II), Toronto, Canada, June 3-5,1992 Wang,31., Multifunctional Phosphorus Hydrazides as Potential Chelating Agents Diagnostically and Therapeutically Useful Radionuclides, MU Chemistry DYNAMITE
- seminar series, l
University of Missouri-Columbia, March 31,1992 Wang, N., Labeling of Protein Microspheres with Radiorhenium as a Radiation Synovectomy Agent, Schlemper Research Group-University of Missouri-Columbia, February 18,1992 Contributed I Anderson. C.J.; Schwarz, S.W.; Rocque, P.A.; Connett, J.M.; Guo, L.W.; Philpott, G.W.; Zinn, K.R.; Meares, C.F.; Welch, C.J., Copper-Labeled Antibodies for PET Imaging, Ninth International Symposium on Radiopharmaceutical Chemistry, Paris, France, April 7-10, 1992 (abstract) Baskett, C.K.; Spate, V.L ; Mason, M.M.; Reams, C.L.; Morris, J.S., The Determination of Selenium in Urine, Second International Symposium on Nuclear Analytical Chemistry (NAC-II), Toronto, Canada, June 3-5,1992 Ehrhardt. G.J.; Curtis, R.L.; Lattimer, J.C.; Day, D.E.; Bartlett, B.R.; Quesenberry, J.T.; Ross, ! G.; Volkert, E.W.; Lanigan, J.P.; Evans-Blumer, M., Investigation of Pre-Operative ! Sterilization of Kidney Cancers Using Intra-Arterial Sm.153 Glass Microspheres in a Rabbit Model, High Country Nuclear Medicine Conference, Vail, CO, March 16-20,1992 Ehrhardt, G.J.; Curtis, R.L.; Lattimer, J.C.; Day, D.E.; Bartlett, B.R.; Quesenberry, J.T.; Ross, G.; Volkert, E.W.; Lanigan, J.P.; Evans-Blumer, M., Investigation of Pre-Operative Sterilization of Kidney Cancers Using Intra-Arterial Sm-153 Microspheres, Society of Nuclear Medicine meeting, Los Angeles, CA, June 8-12,1992 (poster) Ehrhardt, G.J.; Vanderheyden, J-L.; Su, F-M.; Fritzberg, A.R., Experience with Aluminum / ) Perrhenate Targets for Reactor Production of High Specific Activity Re-186 for Radioimmunotherapy, High Country Nuclear Medicine Meeting, Vail, CO, March 16-20, 1992 (poster) Gordon, D.E.; Peluso, M.; Zinn, K.R.; Stoops, D.; Ratliff, V.; Trokey, D.E., Retention of Ca-47, Mn-54, Fe-59, Zn-65, and Se-75 in Rats Fed Diets Containing Different Types and Amounts of Dietary Fiber, Institute of Food Technologists annual meeting, New Orleans, LA, June 18-20,1992 Hunter, D.J.; Willett, W.C.; Morris, J.S., Use of Toenail Clippings as Biomarkers of Trace Element Intake, First International Conference on Dietary Assessment Methods, University of Minnesota, Minneapolis, MN, June 10-13,1992 183
. PRESENTATIONS Life Sciences.
Jimenez, H.; Singh, P.R; Katti, KV.; Ketring, A.R; Volkert, W.A., New Approaches to Pd-109 > Chelates and their Bioccajugates,39th Annual Meeting of the Society ofNuclear Medicine, Los Angeles, CA, June 9-12,1992 Kopicka, K.; Katti, KV.; Ketring, A.R; Volkert, W.A., Methylene Bridged Phosphineoxide-Phosphine as a Versatile Chelating Agent for Re-188,39th Annual Meeting of the Society of 1 Nuclear Medicine, Los Angeles, CA, June 9-12,1992 i Mason, M.M.; Reams, C.L.; Baskett, C.K.; Spate, V.L.; Morris, J.S.; Mills, S., Determination of ' Total and Bound Selenium in Sera Via INAA, Second International Symposium on Nuclear Analytical Chemistry (NAC-II), Toronto, Canada, June 3-5,1992 Morris, J.S., The Missouri University Research Reactor Nuclear Analysis Prograrn, Second International Symposium on Nuclear Analytical Chemistry (NAC-H), Toronto, Canada, June 3-5,1992 Singh, P.R; Katti, K.V.; Kopicka, K.; Katti, KK.; Ketring, A.R.; Volket, W.A., New Bifunctional i Framework Derived from Phosphorus Hydrazide Chelating Agents for Labeling Proteins with Tc-99m and Re-188,39th Annual Meeting of the Society of Nuclear Medicine, Los Angeles, CA, June 9-12,1992 Singh. P.R; Volkert, W.A.; Ketring, A.R; Troutner, D.E.; Katti, K.K; Kaf ti, KV., A New ; Chelating Heterodifunctional Phosphorus-Nitrogen Ligand for Radiolabeling of Proteins, Ninth International Symposium on Radiopharmaceutical Chemistry, Paris, France, April 6- - 10,1992 Spate, V.L., Applications of the University of Missouri Research Reactor and Food Preservation , Using the Co-60 Gamma Facility, Rock Bridge Elementary School, Columbia, MO, February ' 26,1992 Volkert, W.A ; Katti, KV.; Corlija, M.; Meyer, K.; Franklin, T. Singh, P.R.; Ketring, A.R.; Holmes, RA., Small Molecule Neutral-Lipophilic Tc-99m Agents Derived from Functionalized Phosphinimines,39th Annual Meeting of the Society of Nuclear Medicine, Los Angeles, CA, June 9-12,1992 i Volkert, W.A.; Singh, P.R.; Katti, RK: Ketring, A.R.; Katti, K.V., A New and Versatile Multifunctional Phosphorus Hydrazide Ligand for Formulating Neutral-Lipophilic ' Complexes of Tc-99m, Re-186 and Pd-109 Radionuclides, Ninth International Symposium on ! Radiopharmaceutical Chemistry, Paris, France, April 6-10,1992 Wang, M.F.; Ge, Y.W.; Kopicka, K; Katti, KV.; Singh, P.R.; Katti, K.K.; Volkert, W.A.; Ketring, A.R.; Meyer, K.; Corlija, M.; Hoffman, T.J.; Holmes, R.A., New Tc-99m Radiopharmaceuticals Built on Multifunctional Phosphorus Hydrazides,39th Annual Meeting of the Society of Nuclear Medicine, Los Angeles, CA, June 9-12,1992 Zinn, KR.; Chaudhuri, T.; Trokey, D.E.; Sunde, R; O' Dell, B., Identification and Comparisons of Selenoproteins in the Brain and Mouse Neuroblastoma Cells, FASEB meeting, Atlanta, GA, April 19-28,1992 184
Natural Sciences ' PRESENTATIONS - invited Glascock, M.D., Recent Advances in the Investigation ofNew World Obsidians, Archaeometry and Technology of Pre-Columbian Materials session of the International Symposium on Archaeometry, Los Angeles, CA., March 21-28,1992 Hayashida, F.,Inka Provincial Administration: A Ceramic Perspective, MURR, January 28, 1992 Contributed Bove, FJ., El Proyecto Paryjuyu: Resultados Preliminarios y Implicaciones,5th Annual Symposium on Guatemalan Archaeology, Guatemala City, Guatemala, July 23-27,1991 Elam, J.M.; Glascock, M.D.; Neff, H., Source Identification and Hydration Dating of Obsidian Artifacts from the Valley of Oaxaca, Mexico, International Symposium on Archaeometry, Los Angeles, CA, March 21-28,1992 Ericson, J.E.; Glascock, M.D., Obsidian. Flow Differentiation by INAA, Coso, California, Society for American Archaeology Conference (SAA), Pittsburgh, PA, April 8-12,1992 (poster) Glascock, M.D., Recent Advances in the Investigation of New World Obsidian, International Archaeometry Symposium, Los Angeles, CA, March 23-27,1992 Glascock, M.D.; Ericson, J.E., Chemical Characterization of Obsidian Flows and Domes of the Coso Volcanic Field, China Lake, Califernia,28th International Symposium on Archaeometry, Los Angeles, CA, March 23-27,1992 Glascock, M.D.; Ericson, J.E., Chemical Characterization of Obsidian Flows and Domes of the Coso Volcanic Field, China Lake, California, Society for American Archaeology Conference (SAA), Pittsburgh, PA, April 8-12,1992 Glascock, M.D.; Neff, H.; Stryker, K.S..; Johnson, T.N., Sourcing Archaeological Obsidian by an Abbreviated NAA Procedure,2nd International Symposium on Nuclear Analytical Chemistry, University of Toronto, Canada, June 3-5,1992 (poster) Johnson, T., Sourcing and Dating of Obsidian Artifacts from Pacific Coastal Guatemala, Missouri Academy of Science Annual Meeting. Rolla, MO, April 24,1992 Neff, H., A Role for Sourcing in Evolutionary Archaeology, Society for American Archaeology Conference (SAA), Pittsburgh, PA, April 8-12,1992 Sisson, E.B.; Neff, H.; Bishop, R.L., Regional Sub-Styles and Provenience of Polychrome 'Laca' with Codex-Style Motifs,47th International Congress of Americanists, New Orleans, LA, 7 July 8,1991 Stryker, K.S., A Chemical Investigation of Mississippian Pottery from Moundville, Alabama Using Neutron Activation Analysis, Missouri Academy of Science Annual Meeting. Rolla, MO, April 24,1992 185
GRANTS' AND CONTRACTS PRINCIPAL INVESTIGATORS, TITL E AGENCY / AMOUNT ' PERIOD Benfer, R.A.; Elam, J.M., Source Analysis and NSF 07/91-12/91 Hydration Dating of Post-Formative Period $8,480 Obsidian Artifacts from the Valley of Oaxaca, Mexico Brugger, R.M.; Kunze, J.F., Investigation of DOE -10/90-09/92 Reactions and Moderators for an Accelerator $143,700 Based Epithermal Neutron Source for Boron Neutron Capture Therapy Ehrhardt, G.J., Radiorhenium for NeoRx Corp. 10/89-06/93 Radioimmunotherapy $525,354 Ehrhardt, G.J.; Ketring, A.R., Further Development of Mallinckrodt 06/91-05/92 the W-188/Re-138 Gel Generator for Radiotherapy Medical, Inc.
$39,587 Ehrhardt, G.J.; Zinn, K.R.; Day, D.E., Mallinckrodt 06/90-05/92 Radiation Synovectomy with Re-186 and Re-188 Medical Labeled Prc,tein Microsphere Conjugates $99,876 Glascock, M.D., The Archaeometry Laboratory NSF 01/92-12/94 at MURH . $300,000 Glascock, M.D., Center for.Archaeo;netric NSF 01/91-12/91 Research at the University ofivussouri $109,977 Heuser, B.J., A Novel Approach in the Study of Defects MU Research 06/92-12/92 in Metals Council
$1,478 Kaiser, H.; Werner, S.A., US-Austria NSF 03/88-08/91 Cooperative Research: Comparison $12,200 of Interferometric Measuring Methods (Physics and Materials Research)
Ketring, A R., Development of Facilities for Supply Mallinckrodt 06/92-05/93 of Holmium-166 ("*Ho) and Samarium-153 Medical, Inc. P3Sm) $70,000 Ketring, A.R.; Katti, K.V.; Volkert, W.A., Mallinckrodt 06/92-05/94 Development of New MRI Contrast Agents Medical, Inc. and Radiopharmaceuticals $307,815
- O is amount to MURR 166
GRANTS AND CONTRACTS PRINCIPAL INVESTIGATORS, TITLE AGENCY / AMOUNT PERIOD Ketring, A.R.; Strin;; ham, L.M., Dow Chemical 05/88-10/92 i Supply of *Rh, "*Ho, *Sm and Company "Sm-EDTMP $702,969 Kunze, J.F., National Academy for Nuclear Institute of Nuclear 08/90-07/91 Training Fellowships in Nuclear Power Operations Engineering, 1990-91 $10,000 Kunze, J.F.; Alger, D.M.; Blanchard, P.; Brugger, Oak Ridge 09/90-08/95 R.M.; Langhorst, S.M., US Department of Associated Universities Energy Radioactive Waste Management $ varies / approved Fellowship Program, Participatory Status Renewal for 1990-91 through 1994-95 Kunze, J.F.; Alger, D.M.; Blanchard, P.; Brugger, Oak Ridge 09/90-08/91 R.M.; Langhorst, S.M.; Lee, P.K.; Loyalka, S.K.; Associated Universities Manahan, S.; Miller, W.H.; Peyton, R.L.; Prelas, $18,400 M.A., US Department of Energy Radioactive Waste Management Fellowship for Michcel Chung f Kunze, J.F.; Glascock, M.D., pH Efrect of Sandia National 08/91-02/92 Decontamination of Metal Surfaces Laboratories
$26,997 Kunze, J.F.; Langhorst, S.M.; Glascock, M.D.; Argonne National 07/91-01/92 Meyer Jr, W.A., Irradiate and Evaluate Lithium- Laboratory Aluminide Targets $8,902 -
Laporte, R.; Morris, J.S., Selenium in Prospectively N)H 01/89-12/92 Collected Human Sera and Cancer Risk $533,000 University of Minnesota (24,000)* Loyalka, S.K.; Anderson, H.D.; Ku k, B.D.; Chan, P.C.; NSF 03/90-09/91 Krawitz, A.D., Research Experiences for Under- $40,023 graduates in Particulate Systems Engineering, Summer 1990 Maxon, H.; Ehrhardt, G.J., Efficacious Skeletal NIH 04/87-03/92 Imaging Radiopharmaceuticals $1,175,537 University of Cincinnati (12,000)* McKibben, J.C.; Meyer Jr, W.A.; Edwards Jr, C.B.; DOE 09/90-09/92 Langhorst, S.M.; Morris, J.S., MURR FY1991 $225,000 Upgrade of Equipment and Instrumentation
- O is amount to MURR 187
i4.e i{
-l 1 , .- GRANTS AND CONTRACTS i
PillNCIPAL INVESTIGATORS, TTTLE- AGENCY / AMOUNT PERIOD Miller, W.lL, Determination of Prompt Neutron ORNL 0592-02/93 :i Emissions for Actinide Waste Isotopes subcontract through - Texas A&M University
$7,000 -
t Miller, W.II., National Academy for Nuclear Institute of Nuclear 08/91-07/92 ~ Training Fellowships in Health Physics, Power Operations l 1991-92 $10,000 Miller, W.IL; Banerji, S.K.; Blanchard,- P.E.; Carson, Oak Ridge Associated 07/90-06/95 i W.; Kunze, J.F.; Langhorst, S.M.; Loyalka, S.K.; Universities ! Manahan, S.; Morris, J.S.; Peyton, R.L.; $ varies / approved ! Mossman, l>.J.; Carroll, S.A., US Department of Energy Enviromnental Restoration and Waste ; Management Fellowships, Participatory Status for ' 1990-91 through 1994-95 , Miller, W.IL; Berliner, R., A DSP-Based, Smart DOE /ER 04/92-04/94 ADC for Nuclear Radiation Detectors Special Research : Grant Program
$164,000 , i
-i Miller, W.H.; Kunze, J.F.; Banerji, S.K., The Callaway Nuclear 09/91-08/93 - i Determination of Radioisotope Levels in Power Plant (Union Municipal and Industrial Sewage Sludge Electric Company)
$60,000 l
Morris, J.S., Analytic Epidemiology Support via Microbiological 10/90-09/91 Neutron Activation Analysis: Determination of Assoc. Inc. Selenium in Iluman Serum $94,723 3 Morris, J.S., Heactor Sharing DOE 09/91-08/92
$70,000 Morris, .1.S., Reactor Sharing DOE 09/90-08/91
$70,000 Morris, J.S., Trace Elements and Human Health . NIH 07/89-12/93
$376,969 Morris, J.S.; Glascock, M.D.; Farmer, J.W.; NSF 04/90-10/92 Berliner, R.R.; Zinn, K.R.; Kaiser, H.; $82,000 Ehrhardt, G.J.; Ketring, A.R.
- O is amount to MURR 188
GRANTS AND CONTRACTS PRINCIPAL INVESTIGATORS, TITLE AGENCY / AMOUNT PERIOD , Neff, H., Archaeological Research in Pacific MU Faculty 02/92-03/92 Coastal Guatemala Research Council
$893.50 Nefr, H.; Glascock, M.D., Prehistoric Chronology MU Weldon Spring 06/91-05/92 of the Oaxaca Valley Fund Competition '
1990-91
$20,480 Ponnamperuma, C.; Gehrke, C.W.; Caldwell, W.; NASA 10/89-09/92 Carle, G.; Desiderio, D.; Eisenstark, A.; Freeman, $350,000 D.; Gibson, E.; Hare, E.; Hobish, M.; Knoll. A.; (7,500)*
Kumar, S.; Kuo, K.; McEntire, J.; Morris, J.S.; Smith, M.; Stalling, D.L.; Zumwalt, R., A Lunar- i Based Chemical Analysis Laboratory (LBCAL) Rhyne, J.J.; Berliner, R.R.; Worcester, D.L., Upgrade NSF Division of 05/90-10/91 of the University of Missouri Small-Angle Neutron Materials Research Scattering Spectrometer Instrument $182,000 Rhyne, J.J.; Werner, S.A.; Stassis, C.; In NSF 06/91-03/93 collaboration with Yelou, W.B.;'faub, H.; $225,000 Ross, F.K.; Kaiser, H.; Berliner, R.; Goldman, A.I.; Zaretsky, J.L., Development of a Triple-Axis Neutron Spectrometer at MURR Ross, F.K., Hgl, Crystal Perfection Studies EG&G Energy 08/91-09/92 Measurements Santa Barbara Operations
$25,000 Ross, F.K.; Berliner, R.; Chaudhuri, T.; Ehrhardt, G.J.; NSF 02/92-07/95 Farmer, J.W.; Glascock, M.D.; Ketring, A.R.; $165,000 Morris, J.S.; NefT, H.; Yelon, W.B.; Zinn, K.R.,
Scientific Applications of Neutrons at a University Research Reactor Ross, F.K., Subcontract to "An Orientable High University of Florida / 07/90-04/93 Angular Resolution Array of Gamma Ray US Department of the Navy Detectors" No. N00014-89-J-3030 '
$40,540
- O is amount to MURR 189
^
t GRANTS AND CONTRACTS
. PRINCIPAL INVESTIGATORS, TITLE AGENCY / AMOUNT PERIOD Storvick, T.S.; Krueger, C.L.; Sharp, P.; McKibben, J.C.; Rockwell International 04/92-03/93 Langhorst, S.M., Engineering, Chemistry Rocketdyne Division and MURR Program Support of the Rockwell $519,312 International TRUMP-S Project (273,487)*
Storvick, T.S.; Viswanath, D.S.; Krueger, C.L.; Rockwell International 01/90-03/92 Sharp, P.; McKibben, J.C.; Langhorst, S.M.; Rocketdyne Division Retzloff, D.G., Engineering, Chemistry $1,383,367 and MURR Program Support of the Rockwell (928,597)*- . International TRUMP-S Project Taub, H., Phase Transitions in Surface Films, NATO 11/89-08/91 NATO Advanced Study Institute Erice, Italy $60,890 Taub, IL, Studies of the Structure, Phase, Transitions NSF 09/90-02/94 and Dynamics of Adsorbed Films $258,500 Taub, IL; Hansen, F.Y., Molecular Dynamics 200 Service Units 04/91-04/92 Simulations of Hydrocarbon Molecules Adsorbed Pittsburgh Super-on a Graphite Substrate computing Center
~
Taub, H.; Schmidt, P.W., Acquisition of a High- NSF Materials 09/90-01/93 Intensity X-Ray Diffractometer Research Instrumentation Program
$152,700 Troutner, D.E.; Schlemper, E.O.; Ketring, A.R., DOE 06/89-06/93 Bifunctional Chelates of"$RH and 8"Au as $573,285 Potential Radiotherapeutic Agent i Volkert, W.A.; Ketring, A.R.; Kuntz, R.R.; Feldbush, DOE 07/89-10/92 T.L; Mitchel, E., Production of Radiolabeled $532,974 Monoclonal Antibody Conjugates by Photoafnnity Labeling Werner, S.A.; Kaiser, H., Neutron Interferometry NSF, Physics 01/89-05/95 and Neutron Schrudinger Wave Optics Division
$816,000 Winholtz, R.A.; Krawitz, A.D., Characterization of Babcock & Wilcox - 05/92-10/92 Residual Stresses in a Subscale Cylinder of the $90,337.66 Advanced Solid Rocket Motor
- O is amount to MURR 190 t
E GRANTS AND CONTRACTS PRINCIPAL INVESTIGATORS, TITLE AGENCY / AMOUNT PERIOD Winholtz, R.A., Single Crystal and Grain Interaction NSF 0&92-05/95 Stresses Measured with Neutror. Diffraction $94,041 Winholtz, R.A., Summer Research Fellowship MU Research 06/92-08/92 Council
$3,779--declined Yelon, W.B., Neutron Scattering of Titanium- McDonnell Douglas 02/91-02/92 Aluminum Alloys $30,000 Yelon, W.B., Neutron Supermirrors Ovonic Sy,thetic 12/90-06/92 Materials Company, Inc.
$20,000 Yelon, W.B.; Farmer, J.W.; Cowan, D.L.; Ross, F.K., Midwest Supercon- 07/90-07/92 l Neutron Diffraction and Defect Studies of ductivity Consortium High T, Superconductors (MISCON)
$249,417 Yelon, W.B.; Popovici, M., Optimized Optics for Heat- Argonne National 10/91-09/92 l Loaded Double Monochromators Laboratory Advanced Photo Source
$26,294 i
! Yelon, W.B.; Schupp, G., Inelastic Scattering in DOE 03/91-12/92 l Condensed Matter with High Intensity M6ssbauer $138,694 f Radiation t Yelon, W.B.; Schupp, G., Multi-Beam Mussbauer DOE 10/91-09/93 Scattering Facility $74,065 ( Zinn, K.R., Drug Evaluation Study, Phases I-IV Oread Laboratories 07/89-12/92
$79,000 l
- O is amount to MURR 191
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T' i l' PROFESSIONAL SERVICE ACTIVITIES - National and International Committee Participation DOE Nuclear Medicine Project Review, Review Team, May,1992, Bethesda, MD, G.J. Ehrhardt, i member Co-Moderator for Scientific Paper Session #84, Radiopharmaceutical Chemistry: Proteins / Antibodies III,39th Annual Society of Nuclear Medicine meeting, les Angeles, CA, June 9-12, ! 1992, A.R. Ketring, member: Scientific Program Committee, Protems/ Antibodies Category, l member Executive Committee-American Nuclear Society, Central-Eastern Missouri Section, K. Kutikkad, , member : American Board of Health Physics, Panel of Examiners (Part 2), Susan M. Langhorst, member IAEA Technical Committee Meeting on Research Reactor Problems of the 1990s, Dhaka, Bangladesh, June 22-26,1992, J.C. McKibben, member, the USA representative International Group of Research Reactors (IGORR) Organizing Committee, J.C. McKibben, j member Test, Research, and Training Reactors (TRTR) National Organization Executive Committee, J.C. t McKibben, chair (1991-1992), member Professional Engineering Examination Committee, American Nuclear Society, W.H. Miller, member Accreditation Board for Engineering and Technology, Ad Hoc Visitor for American Nuclear Society, W.II. Miller
~
Scientific Committee Ieuis Neel Laboratory, C.N.R.S., Grenoble, France, J.J. Rhyne, member Advisory Committee,Ims Alamos Neutron Scattering Cater, J.J. Rhyne, member Journal of Magnetism and Magnetic Materials, J.J. Rhyne, Advisory Editor Neutron Special Interest Group (of the American Crystallographic Association), F.K. Ross, Chairman,1989, member 1 192
PROFESSIONAL SERVICE ACTIVITIES Chemistry Participating Research Team at the High Flux Beam Reactor, Brookhaven National . .; Laboratory, H. Taub, member Executive Committee Midwest Analytical Team for Reseach Instrumentation ofX-Rays, H. Taub, member Executive Committee Midwest Universities Group to establish a Collaborative Access Team at the Advanced Photon Source, Argonne National Laboratory, H. Taub, member National Science Foundation New Young Investigator Award Selection Panel, H. Taub, member Board of Assessment., Physica Laboratory, National Institute of Standards and Tecimology, S.A. Werner, member Intermag '92 (St. Louis, MO, april 13-16,1992), Publication Committee, W.B. Yelon, choir; Program Committee, member; Steering Committee, member Magnetism and Magnetic Materials Conference, Publication Comnuttea, W.B. Yelon, chair, Steering Committee, member University Standing Committee Participation UM Central Radiation Safety Committee, G.J. Ehrhardt, J.S. Morris, and J.J. Rhyne, members , University Award Committees-Chancellor's Award Committee for Outstanding Faculty Research .. and Creative Activity, Spring 1992, M.D. Glascock, member ; MU Honorary Degrees Committee, A.D. Krawitz, member ! MU MAE Promotion and Tenure Committee, A.D. Krawitz, chair : MU Graduate Faculty &r.ac Procedures Committee, S.M. Langharst, chair '( UM Research Board, S.A. Werner, member -[ 1 193 -l s . k l
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s PROFESSIONAL SERVICE ACTIVITIES MURR Standing Committees MURR Reactor Advisory Committee, A.E. Bolon (UMR), chair; G.J. Ehrhardt, D.T. Gordon, J.F. Kunze, S.M. Langhorst, P.K. Lee, J.C. McKibben, R.D. Murphj (UMKC), T.S. Storvick, D.L. Worcester, members; J.J. Rhyne, J.D. Sheridan, ex officio members MURR Reactor Advisory Subcommittees Gemstone License Subcommittee, J.S. Morris, chair; R.R. Berliner, S.M. Langhorst, L.H. Manson, O.B. Oladiran, J.R. Schuh, members; M.D. Glascock, J.P. Ernst, S.L. Gunn, CA Fairfax, alternates I Isotope Use Subcommittee, G.J. Ehrhardt, chair; S.L. Gunn, H. Kaiser, S.M. Langhorst, C.B. McCracken, W.A. Meyer, J.G. Shotts, K.R. Zinn, members i 1 I Procedures Review Subcommittee, Manager-Reactor Health Physics, chair, Associate Director, Reactor Operations Engineer, Reactor Manager, Chief Machinist, Chief Electronics Technician, ' Shift Supervisor, Manager-Facilities Operations (this committee is represented by position, not - ; by name) i Reactor Action Subcommittee, P.K. Lee, chair; J.F. Kunze, C.W. Tompson, members
]j Reactor Research Advisory Subcommittee, J.C. McKibben, chair; G.J. Ehrhardt, W. Folk, S.K.
Loyalka, J.M. Meese, J.S. Morris, M.J. O'Brien, E.O. Schlemper, T.S. Storvick, R.A. Sunde, T.L. Veum, W.A. Volkert, SA Werner, W.B. Yelon, members; J.J. Rhyne, J.D. Sheridan, ex officio members I
- Reactor Safety Subcommittee, J.F. Kunze, chair; J.C. McKibben, W.A. Meyer, W.H. Miller, J.S.
Morris, T.L. Pitchford, W.F. Reilly, G. Schupp, T.S. Storvick, W.A. Volkert, members; K. Riggle, alternate, non-voting member ' Reactor Service Subcommittee, J.C. McKibben, chair; W A. Meyer, J.S. Morris, F.K. Ross, ? memlers .f l 194 I
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Governmental / Industrial Agencies COLLABORATORS Governmental Agencies Ames National Laboratory Foundation for Ancient Sandia National Laboratories Kramer, M. Research & Mormon Studies Bennett, P.C. Argonne National Laboratory Stocker, T. Smithsonian Institution f Bowman, M.K. Iowa Geological Survey Bishop, RL. t Crabtree, G.W. Anderson, RR. Blackman, MJ. Downey, J. Jet Propulslon Laboratory Hegmon, M. Dozier, W.D. Vandersande, J.W. Southern Research Institute Flesher, S. Museum of Northern Arizona Dismukes, E. Frischherz, M.C. Weigand, P.C. . Un!!ed States Army Hettinger, J. NationalInstitute of Standards Johnson, J.C. Katz, J.J. and Technology United States Geological Survey Kirk, M.A. Borchers, J.A. - Grauch, R.L Liu, J.Z. Casella, RC. VA Hospital, Columbia, MO Michal. ski, T.J. Copley, J. Corlija, M. Tmuw, F.R Erwin,R.W. CNRS Grenoble, France Vandervoort, RG. Gilinka, CJ. Fruchart, D. Vleck, RM. Mildner, D.F.R. Laboratory Leon Brillouin, Welp, U. Pierce, D.T. France Brookhaven National Prask, HJ. Coddens,G. !' Laboratory National Park Service Museo del Banco Central, - Ehrlich, S.N. Lynott, MJ. Ecuador i Larese, J.Z. Nebraska State Historical Salazar, E. -1 Cumberland Science Museum Society Nuclear Hesearch I.sstitute, Thieme, M.S. Bozell, J.R Czechoslovakia EG&G Energy Measurements Oak Ridge National Laboratory KoPi cka, K . James, C. Smith, H.G. Tatu Institute of Fundamental Naison, D. Spooner, S. Research, Colaba, India ! Van den Berg, L. Wignall, G. Malik, S.K ; Industrial Agencies .__ __._.___. _ . _ . _ . Ceramen! Corpontisn f.8. T=krodt Medical,Inc. Union Electric TofTe, A. Brodack,J. Graham, C. Crucible Research Deutsch, E. Stretch, D. Kim, A. Deutsch, K Welty, T. Dow Chemical Company Pipes, D. West, L. Carni, J. Thomas-Miller, B. Central Research Institute of Fordyce, W.A. McDonnell Douglas Electric Power industry Garlich, J. Lederich, RJ. (CRIEPI), Japan Goeckeler, W.F. Sastry, S.M.L. Miyashiro, H. McMillan, K Schwartz, D.S. Eakamura, Y. NeoRx Corporation Ecole Polytechnique - Montreal, Simm, J. Simon, J. Fritzberg, A.R. Cane.da E I du Pont Su,F-M. Yelon, A. Flattery, D.K Vanderheyden, J.L IBM, Munich, Germany General Motors Ovonic Synthetic Materials Binnig, G. Fuerst, C. Keem, J.E. ' Smith, D.P.E. Herbst, J. Wood, J. Phi!!ps Eindhoven, The Morelli, D. RockwellInternational Netherlands Jewish Hospital Grantham, L. Buschow, KHJ. Connett, J.M. Gnmmett, D.L. Guo, LW. Roy, JJ. Philpott, G.W. 195 p i .__
COLLABORATORS Universities Arizona State U John Carroll U Tulane U Allison, J.R. Trivisonno, J. Andrews, E.W. Calvache, M.LL. Johns Hopkins U Braswell, G.E. Carr, C- Chien, C.L. U of Arizona Heller, L. Childress, J.R Clark, C. Irscinsky, D. IlofTman, S. Fish, P.R. Schaefer, S.J. Lincoln U Fish, S.K. Siebe, C. Gilliam, D.L Whittlesey, S. Loras College U of California-Davis Williams, S. Gr ss, J.B. Meares, C.F. Yo R . . California Tech assachsens Insh of U d CamorniaNne . Etti, C. Technology Ericson, J.E. Johnson, W.L. Davison, A. U of Ca!!fornia-Los Angeles - Krill III, C.E. Missouri Baptist College - Biskowski, M. Li, J2 Guimon, R.K. U of California-Santa Barbara Samwer, K. Missouri valley College Bove, F.J. Carnegie Mellon Symes, S. Ford, A. Pararian, F. Northeast Missouri State U U of Cincinnati Central College Bormann, L. Boolchand, P.- Hosch, M.D. Northwestern U Bresser, W. j Central Metnodist College Kim,J. Maxon, H. Noren, E. ober!!n College U of Connecticut Central Missouri State U Welch, P.D. Lizee, J.M. Bequette, J.M. Purdue U U of Delaware ~ l Billings, B.J. Bullard, B.R. Hadjipanayis, G.C. College of Charleston Mullen, J.G. Singleton, E.W. Coglan. M.W. Wagoner, R.A. Tang, Z.X. - Southeast Missouri State U ' Wang, Y.Z.
""""*' Johnson, T.N. U of Florida Dartmouth College .<
Allen, T. St uis U Aspacher,B. Carlson-Fosez, V.L. Cmok, A.G.- Coldwell, R. _, Franklin and Marshall College Stephens College Haywood, S. Shawkey, E. Anderson, H.D. . Rester, A.C. Indiana State U Benton, T. U of Hawaii-Gomez, B. Hodges, S. LeMarchand, L. Iowa State U Syracuse U U of Houston Goldman, A.I. Kumar, A. Backe, H. Jia, H. Meyer, W. Bechtold, J. Seifert,, K.E. Tennessee Technical U Buskirk, F.R. Shinar, J. Hindi, M.M. Chu,C.W. Shinar, R. Kozub, R.L . Connors, S.M. Stassis, C* Thomas Jefferson U Her, P.H.
' Windom, K.E. Thakur,M. Huang, Z.J.
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Universities COLLABORATORS Hungerford, E.V. U of Mississippi Technical U'of Denmark ' Maruyama, X.R Sisson, E.B.' Hansen, F.Y. ; Snyder, D.D. Sisson, P.R. Technical U of Vienna Xue, Y.Y. U of Nebraska Rauch, H. U of Houston-Clear Lake Holen, S.R. . Steiner, W.- Hodge, M.G. Jaswal, S.S. W61witsch, H. U of Illinois Champaign-Urbana U of Nebraska-Lincoln Technische Universitat Beach, R.S. Sellmeyer, D.J. Munchen, Germany Carlson, K E. U of North Carolina 4hapel Hill Petruva-Koch, V. ! DiZio, J.P. Steponaitis, V.P. The RoyalInfirmary, Glasgow ' Du, R.R. U of Notre Dame Anderson, J.H. Flynn, C.P. Furdyna, J.K. Bessent, R.G. Katzenellenbogen, J.A. Giebultowicz, T.M. Cooke, T.G. Matheny, A. Klosowski, P. Goldberg, J.A. Nieuwenhuys, G.J. Luo,H. McArdle, C.S. Salamon, M.B. Samarth, N. McKillop, J.H, Simmcas, R.O. Scott, J. U of Alberta, Edmonton Tsui, F. U of Pennsylvania Cavell, R.G. U of Indiana McGovern, P.E. U of Edinburgh, Scotland Lee,L Vanderbilt U Torbet, J. Ripley, E. Medrano, S. U of G5ttingen, Germany Shaffer, N. Washburn U Egert, E. Taib, I. Nagy, H.J. Rietzel, M. U of Kentucky Washington U Roesky, H.W. Sandefer, E. Anderson, C). U of Grenoble, France Arsenault., R.J. Bell, BJ. Isnard, O. Shi, N. Diederichs, J. U of loannina, Greece Walters, D.B. Kelton, K. Moukarika, A. . U of Michigan Libbert, J. Papaefthymiou, V. Hayashida, F.M. Rocque, P.A. U of Liege - Belgium King,J. Schilling, J.J. Grandjean, F. Luginsland, J. Schwarz, S.W. U of Melbourne, Australia Minc, L.D. Welch, M.J. Allman, B.E. > Parsons, J. Academia Sinica, People's Cimmino, A. Riley, K.J. Republic of China Klein, A.G. Seman, D.J. Nansheng, C. Opat, G.I. ; Summerfield, G. Ciudad Universitaria, Mexico U of Munich, Germany U of Minnesota de Arcehavaleta,D.S. Allgier, C. Dahlberg, E.D. Glasgow U Neumeier, J. Prohaska, J.R. Kerr, D.J. U of San Carlos, Guatemala , Saini-Eidukat, B. Instituto Nacional de Lou,B. Weiblen, P. Antropologia e Historia, Merico Cobean, R.H. t 197 P k
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J l COLLABORATORS University of Missouri System Adams, C.G. Greenfield, M.C. Llorens, A.S. Schmidt, P.W. Agarwal, S.R. Greenlief, C.M. Loeppky, R.N. Schupp, G. Angot, T. Greenwood, S. Iong, G.J. Sellers, S.D. Arif, M. Griffin Jr, J.L Love,J. Shar p, P.R. Auman, L. Gulati, P. Loyalka, S.K. Singh, P. Bahadori, D. IIakimi, N.M. Lu,J. Slane, K.W. Banerji, S.K. Hamacher, K.A. Lubensky, E.H. Smith, D. Barnes, C.L Hassan, N. Ma, D. Smith, LF. Bames, K.J. Hayes, W.W. Manahan, S. Sorrell, D. Bartlett, B.R. Hilburn, D.N. Mann, J.T. Stammeyer, M.M. Benfer, RA Hillman, L. Manning, G. Stephens, L.S. Bennett, PA Hinderks, BA Marasinghe, G.K. Stich, T.A. Bentley, RL. Hines, A.L. Mattheis, B. Stith, B.K. Biere, N.N. Hinkebein, K.W. Mcdonald, GA Stith, P.S. Boley, M.S. Hirtz, G.J. McIntyre, A.L. Stoops, D. Bradford, D. Hoard, R.J. McNally, M.G. Storvick, T.S. Brewer, M.D. Hogan, C.S. Messmer, J.P. Stryker, KS. Broadway, S. Holmes, RA Miller, W.H. Stuck, J.T. Brown, RF. Hu, Z. Mills, D.S. Su, Z.M. Brugger,R.M. Iyer,R.R Mobley, R. Sunde,R. Buckley, J.E. Jalbuena, R. Mously, K Tang, Y.Y. Chandrasekhar, M. James, W.J. Murowchick, J.B. Taub,H. Chao,W-W. Janedi, T. Nabelek, P.I. Temenak, J. Cheng, K-Y. Jean, Y.C. Nel, M. Thomas, B.L j Clieng, T-P. Jia, W. Nurrenbern, J. Thomas, D.C.T. Clothier, R Jimenez, H.N. O'Brien, M. Tones, KK Cogswell, J.W. Johnson, J.C. O' Dell, B. Troutner, D.E. Condra, C.W. Jokerst, S. Olaughlin, J. Vetter, B. Cooper, J. Jung,H. Pellet, L. Volkert, E.W. CoveneyJr RM. Jurisson, S. Peluso, M. Volkert, W.A. Cowan, D.L. Katti, K. Piechowski, M.F. Wald, MA Cruz, J. Khanna,V. Price, J. Wallman, A.T. 1 Curtis, RL. Kruessel, T.M. Pring!e, O.A. Wang, M. { Dai, P-C. Kulasekere, K.C. Quesenberry, J.T. Wang, N. k Dai, W. Kulasekere, R Radke,D.L Wang, S-K Date, S.V. Kuntz, RR RatlifT, V. Warren, B.D. Day, D.E. Kunze, J.F. Rautman, M. Watring, T.S. Dennison, J.R Lai, C,J. Reams, C.L Werner, SA Ding, X. Lane, D.G. RetzlofT, D.G. White, H.J. Dinger, R Lang,L Riggle, RJ. White, J. Elam, J.M. Lattimer, J.C. Roberts, C.J. Williams, M.L. Elwell, W.S. Law,H-M.R Rong,X Winslow, N.A. Eubanks,W A Lee, W-T.H. Ross, G. Witte, DA Gazaway, T.L Ire, Y. Rutan, J. Woods-Bowen, K.Y. German, G.E. Liang, Q. Salem, J.D. Worcester, D.L. Ghosh, T.K. Lin,1,T. Salib, M.SAR Wu, G.W. Gordon, D.E. Lindemuth, L.C. Santee, J.L. Wu, Z. Gottschalk, S.E. Littlefield, K. Satpathy, S. Xie, H. Liu, H.B. Schlemper, E.O. Yim, H. [ 198
[ RECIPIENTS OF RADIOISOTOPES AND ANALYSES Alpha Omega Purdue University L Amersham International R/A Services Inc. j Argonne National Laboratory Radiation Safety & Nuclear Prod. Aubum University Rads S L., Inc. . l } Battelle Memorial Institute Rosewell Park MemorialInstitute i Best Industries Inc. RTS Technology,Inc_ b Block Drug Company San Jose State University ! Brigham and Women's Hospital South West Research Institute Brookhaven National Laboratory Texas A&M University Buffalo Materials Research Center, SUNY Theragenics Corporation California Institute of Technology Thomas Jefferson University California State University University Hospital of Cincinnati Ceramed Corporation University of Arizona Chesebrough-Pond's Inc. University of Arkansas Children's Hospital Medical Center University of California Lawrence p Dow Chemical Company Berkeley Lab E.I. Dupont Products University ofCalifornia-Davis I Eastman Kodak Research Lab University ofCalifornia-LANL j Florida Atlantic University University of California-San Diego Franklin & Marshall College University of Chicago j , Fred Hutchinson Cancer Research Center University of Hawaii i ICN Biomedicals,Inc. University of Houston ) Indiana University Medical Center University ofIllinois
) ! Isotope Products Laboratories University of Kentucky 1 Mallinckrodt Medical University ofMassachusetts I Mallinckrodt,Inc. University ofMichigan :
Medical College of Wisconsin University of Missouri-Columbia ! Missouri Analytical Laboratory University ofMissouri-KC ! Monsanto Company University ofMissour: ' hila ! Montreal General Hospital University ofNorth C .ina NASA University of Oklahonu ; f' NASA / Johnson Space Center University of Rochester Medical Center !' NationalInstitute of Health University of South Florida { NeoRx Corporation University of Southern California :i I Neutron Products University of Texas M.D. Anderson New Mexico Institute Cancer Center Nordion International Inc. University of Utah j
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i Northwestern Memorial Hospital Univers;ty ofVirginia f Nuclear Sources & Services,Inc University of Washington Oak Ridge National Laboratory Utah State University Omnitron International,Inc. Vanderbilt University Med Center Oregon State University Washington University Princeton University 7,ynaxis Cell Science Inc. Protechnics International Inc. 199
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