An Assessment of the National Institute of Standards and Technology Programs: Fiscal Year 1993 (1994)

John P. O'Connell, University of Virginia, Chair

Barry G. Willis, Hewlett-Packard Company, Vice Chair

John L. Anderson, Carnegie Mellon University

Joseph D. Andrade, University of Utah

H. Frederick Dylla, Continuous Electron Beam Accelerator Facility

Steven M. George, University of Colorado

Philip K. Hopke, Clarkson University

Lynn W. Jelinski, Cornell University

Charles E. Kolb, Jr., Aerodyne Research, Inc.

Uzi Landman, Georgia Institute of Technology

Douglas E. Leng, The Dow Chemical Company

Kenneth O. MacFadden, W.R. Grace & Co.

David W. H. Roth, Jr., Allied-Signal, Inc.

C. Thomas Sciance, Du Pont Experimental Station

Robert E. Sievers, University of Colorado

William B. Streett, Cornell University

Isiah M. Warner, Louisiana State University

James D. Winefordner, University of Florida

Submitted for the panel by its Chair, John P. O'Connell, this assessment of the fiscal year 1993 activities of the Chemical Science and Technology Laboratory is based on Gaithersburg, Maryland, and Boulder, Colorado, site visits, the panel meeting on May 25-26, 1993, and the 1992 annual report of the laboratory.

The Chemical Science and Technology Laboratory (CSTL; Figure 6.1) provides measurements, reference materials, data, and scientific research (1) to improve measurement reliability and quality control; (2) to increase the rate of innovation and commercialization; (3) to allow for the design and control of competitive and energy-efficient manufacturing facilities; (4) to enhance health, safety, and environmental quality; and (5) to aid competitiveness in the marketplace for the chemical, energy, health care, biotechnology, electronics, instrumentation, and materials processing industries.

The Chemical Science and Technology Laboratory's mission statement is appropriately ambitious and comprehensive but too general to stand alone. It must be coupled to more specific strategies and operational plans. As CSTL continues to integrate activities acquired from other parts of NIST, to respond to NIST 's new vision and strategies, and to adopt the federal

government's evolving technology policy, further refinement of focus and relationships to other technical and scientific institutions both internal and external to NIST will be in order.

CSTL emphasizes chemical and physical characterization, laboratory automation and expert systems, process modeling and simulation, sensors and instrumentation, separation science, and surface and interface science. The matrix of cross-cutting science and technology areas (interdisciplinary technologies) versus strategic thrusts (technical expertise) used to select projects takes full advantage of CSTL' s broad range of skills in addressing new applications, developing novel techniques, and exploring alternative opportunities.

CSTL's limitation on the implementation strategies will come more from a lack of buy-in by research personnel than from a lack of concepts or goals. For example, individual CSTL programs often seem driven more by the availability of internal capabilities than by external needs. As NIST's extramural programs, e.g., the Advanced Technology Program (ATP), mature, CSTL's strategies will need to place more weight on external needs, and in particular, the needs of ATP-generated external partners.

In fiscal year 1992, CSTL had 295 full-time permanent staff members, 90 part-time and temporary employees, and 235 industrial research associates and guest researcher staff members. CSTL received $43.5 million for research and technical services, of which 41 percent was base support (STRS) directly from Congress, 30 percent was from other-agency (OA) contracts, 7 percent was from the NIST director 's fund for competence building, 17 percent was from reimbursements for services, and 5 percent was from a variety of nonbase research and miscellaneous reimbursements.

CSTL's mix of base and reimbursable funds is appropriate but is not uniform across CSTL divisions and groups, causing financial stress in some organizational entities. The balance (not shown) between CSTL's expenses for equipment and facilities relative to staff-related costs seems about right. Research support seemed appropriate, and staff seemed satisfied with their equipment.

The delivery costs incurred in providing standards and calibration services appear to be the only costs recovered. If so, the significant cost of necessary technical improvements, customer relations, and the quality control of services is ignored.

When a CSTL activity is highly dependent (more than 40 percent) on external, OA support, it becomes vulnerable to

termination based on criteria other than its importance to the CSTL mission. Several CSTL activities are vulnerable.

In recent years, NIST has instituted a number of innovative funding mechanisms to encourage new initiatives and thrusts, competence building, greater entrepreneurial spirit and outreach, and extensive collaboration and interaction with industry, which help maintain CSTL's quality and productivity. However, CSTL's current static level of resources is now causing major discontinuities in CSTL projects, particularly those that are reaching the end of competence funding or support under the Director's Reserve. Such uncertainty of support engenders insecurity and morale problems among laboratory personnel that could be alleviated should the anticipated out-year budget increases be realized.

CSTL's research staff indicate that research proposals are submitted on the basis of what is likely to be funded.

• The Chemical Science and Technology Laboratory's strategic planning should involve an expert advisory board or steering committee from industry, academia, and other government agencies. Initially, such a board should recommend directions and priorities. Later, it should emphasize technology transfer. A pilot program, such as the one on chemical waste elimination, would be useful in evaluating the feasibility and desirability of involving an advisory board in strategic planning.

• The Chemical Science and Technology Laboratory should price its services so that clients do not pay less than the clients' internal billing would be for comparable work. CSTL's superior expertise and facilities should be sufficient incentive for buying CSTL's standards and calibration services. CSTL's hourly charge should be comparable to charges assessed for full cost recovery in standard commercial facilities. In addition, there is merit to obtaining more direct customer feedback and actively marketing databases, calibrations, and standard reference materials.

• The Chemical Science and Technology Laboratory should tax its contracts for solving national problems at a rate that will help support the development of the technical underpinning for the contracts and the laboratory's traditional services.

• The Chemical Science and Technology Laboratory must attempt to ensure that funding mechanisms have appropriate phase-in and phase-out funding formulas.

• The Chemical Science and Technology Laboratory's managers should ensure that probabilities for support as perceived by the staff are accurate before committing resources.

The Chemical Science and Technology Laboratory responded commendably to those of the panel's fiscal year 1992 concerns that could be dealt with directly by CSTL management. CSTL had few options in dealing with static NIST resources and with NIST's diversion of emphasis from traditional services and fundamental research.

The panel expressed concern in its fiscal year 1992 report (pp. 118-119) that CSTL's increasing emphasis on technology development and industrial competitiveness would detract from CSTL's unique role in providing standard data and reference materials (see Attachment 1 below for further discussion). CSTL management reported that data and reference material activities continued to produce impressive results during fiscal year 1992; however, the panel perceived that many CSTL staff suspect that data and standards programs are not highly valued by NIST management. For example, NIST's data and standards programs must rely on sales income and outside agencies for financial support, and the organizational level of the Standard Reference Data and Standard Reference Materials programs has been lowered.

Responses by CSTL's divisions to specific 1992 panel recommendations are addressed in detail in the following section.

The Chemical Science and Technology Laboratory and its Biotechnology Division are relatively new organizational entities resulting from major NIST organizational restructuring during the past several years. Biotechnology is one of the few product areas in which the United States still has a significant scientific and technological lead and which has yet to reach its full industrial promise.

The Biotechnology Division consists of the Biochemical Measurements Group, the Biophysical Measurements Group, the Center for Advanced Research in Biotechnology (CARB), and the Biosensor Technology Group.

• The Biotechnology Division should be fully cognizant of and a full participant in initiatives of the Food and Drug Administration (FDA). There has been considerable discussion within FDA about establishing a national biomaterials database activity. The National Heart, Lung, and Blood Institute of the National Institutes of Health (NIH) has sponsored activities within the past few years to establish standard reference

materials for evaluation of biocompatibility and blood compatibility.

• The Biotechnology Division should work closely with counterparts in the National Library of Medicine, the Advanced Research Projects Agency, and other groups within the government and in the private sector to ensure readily accessible databases and communication resources. As the nation moves to establish highly efficient, effective, high-volume, and rapid communications networks for data and images, it is imperative that federal agencies meet their responsibilities for providing information through these modern communication tools. For example, NIST has a major health-related technology initiative in the fiscal year 1995 budget for which the Chemical Science and Technology Laboratory is expected to play a major role. To be effective, the CSTL must be well informed about health care technology initiatives in other agencies, including the NIH, the National Science Foundation, the Advanced Research Projects Agency, and the FDA.

• The Biotechnology Division should consider a broader biomaterials effort, possibly in collaboration with the Food and Drug Administration and the National Institutes of Health.

• The Biochemical Measurements Group expanded its efforts into polynucleotide separation standards and databases, and, apparently, deemphasized its work in protein separation and development of protein databases. This group's premier activity in high-resolution protein separation and protein database development should not be deemphasized.

• The Biophysical Measurements Group would benefit from more extensive interactions with the Advanced Research in Biotechnology Group and with the Biosensor Technology Group. The group is aware of this need and is developing programs and mechanisms to facilitate such interaction.

• The high-speed computer resources of the Center for Advanced Research in Biotechnology (CARB) are crucial to the center's structural biology research and therefore should be continually upgraded. CARB staff should also interact more frequently with other groups in the Biotechnology Division.

• The Biosensor Technology Group needs additional fundamental and theoretical input, including various aspects of molecular modeling and simulation. Individuals from the Biophysical Measurements Group and the Advanced Research in Biotechnology Group could put the activities in biosensor technology on a firmer scientific footing. Regarding the industrial consortium (Center for Advanced Biosensors) being established, the panel fears that the Biosensor Technology Group is not fully aware of many relevant developments and innovations, especially in the minimization of nonspecific binding, a topic chosen by the consortium as its major collaborative activity.

• The Biosensor Technology Group should use advisors for planning an expansion of biomolecular devices and bioelectronics projects.

• The Biosensor Technology Group should have additional interaction with the Center for Advanced Research in Biotechnology and the Biophysical Measurements Group. The group's reliance on fiber-optic-based methods for biosensor development may have been premature, thereby complicating the group's understanding of basic interfacial processes that need to be developed and controlled. Some of these processes can be more effectively studied using the instrumentation and techniques of the Biophysical Measurements Group.

The Chemical Kinetics and Thermodynamics Division has historically concentrated on problems relating to energy sources, the environment, microelectronics fabrication, advanced materials, and chemical process technology. The division provides modern, computerized standard databases.

Stabilization of the senior personnel base and effective use of nonpermanent staff have enabled the Chemical Kinetics and Thermodynamics Division to continue its excellent research and produce an enviable quantity of research publications and standard reference data products.

The division relies heavily on OA funding, which to date, along with reimbursements from the division's data products, has provided stable support for the division's personnel. However, there is little support for planning, long-term research, and data programs.

The division anticipates adding two permanent professionals to replace competence lost by a recent retirement and a retrenchment.

The Experimental Chemical Kinetics Group is well focused and productive, as evidenced by the high level of support from outside agencies. The Kinetics Data Center is innovative and productive, having spearheaded NIST's efforts to produce modern and comprehensive computerized databases. The Chemical Thermodynamics Group's programs are appropriately balanced between experimental properties measurement, theoretical data estimation, and data compilation and evaluation activities. The group and the data center are understaffed and undersupported, given the needs of U.S. industry.

Experimental Chemical Kinetics Group. This group concentrates on relevant environmental measurements and energy and chemical processes. Kinetic rate parameters and photochemical cross sections important in determining the atmospheric lifetimes of chemicals affecting stratospheric and tropospheric ozone remain a major area of concentration and success. A particularly fruitful collaboration with a former divisional postdoctoral associate, now at Ford Research, demonstrates the effectiveness of NIST's Postdoctoral Research Program in promoting technology transfer.

Important work is also being carried out in the photochemistry of outer planetary atmospheres. The atmospheric kinetics projects are supported by seven contracts from outside NIST.

Other kinetics work with energy, environmental, and process industry applications includes pioneering studies of radical reactions in aqueous and nonaqueous solvents. Unique kinetic mass spectroscopy studies of ion and molecule reactions relevant to energy and industrial processes also continue to produce valuable results. In addition, shock tube kinetic studies of hydrocarbon and chlorocarbon pyrolysis and oxidation reactions important to combustion and waste incineration continue to yield valuable data. These studies receive direct external support.

Resonance enhanced multiphoton ionization spectroscopy is being developed as a key diagnostic tool for gas-phase and gas/surface chemical kinetic and materials processing studies. The NIST Resonance Enhanced Multiphoton Ionization Group has done pioneering work in detecting and characterizing many radical species of critical importance to combustion, chemical vapor deposition, and plasma deposition and etching processes. Such radical species are difficult to monitor, and resonance enhanced multiphoton ionization spectroscopy may allow evaluation of their role in important industrial processes. This work has received ATP funding and Director's Reserve funding during fiscal year 1993.

The division's permanent senior staff are all recognized on the national and international level and successfully direct the work of many guest workers and postdoctoral fellows. The staff's work currently depends on OA funding; however, current ATP-related initiatives proposed in environmental technology and microelectronics may provide additional support.

Kinetics Data Center. The Kinetics Data Center leads the world in rate and chemical property data compilation and evaluation. A combination of permanent staff, guest workers, part-time employees, and students accomplishes much on OA funding and reimbursement for their products.

The division's work in experimental chemical kinetics also contributes directly to the division's outstanding data programs. The data activities in the Kinetics Data Center cover not only rate parameters, but also related topics in atomic and molecular structure and spectroscopy. Many members of the Experimental

Chemical Kinetics Group also contribute directly to data compilation and evaluation activities.

Major accomplishments since the panel's fiscal year 1992 assessment included the issuance of updated versions of the NIST-Environmental Protection Agency-NIH Mass Spectrometry Data Center Mass Spectral Database and the NIST Chemical Kinetics Database, along with a new NIST Vapor-Phase Infrared Database. New data for both the revised Mass Spectral Database and the new Vapor-Phase Infrared Database were taken by division personnel on an instrument that simultaneously measures the infrared and mass spectra of target compounds.

The Mass Spectral and Chemical Kinetics databases led NIST's sales of database products. Other significant Kinetics Data Center activities included the preparation and publication of specialized evaluated data compilations for propellant combustion, atmospheric chemistry, and plasma etching. The center's Ion Energetics and Chemical Properties Database is being upgraded.

Chemical Thermodynamics Group. Over the past few years, retirements, reorganizations, and reductions in staff have pared this group to a barely adequate level of five permanent senior staff members. A sorely needed permanent scientific staff member will be added before the end of fiscal year 1993. The group's activities are divided between research, standard reference data, and standard reference materials. The group earns significant reimbursement from the Standard Reference Data and Standard Reference Materials programs but has little OA support.

The group is a world leader in fluorine and oxygen combustion bomb calorimetry. Studies with fluorine yield highly accurate and precise enthalpies of formation for inorganic compounds, while studies with oxygen yield similar data for organic and organophosphorus compounds. An innovative low-temperature adiabatic heat capacity calorimeter is also being developed. This will provide entropy data that can be combined with the group's enthalpy measurements to yield free energy data and allow the computation of equilibrium constants for chemical reactions.

In reference materials and information, the group recertified the important benzoic acid standard as well as two sulfur-in-coal reference material standards. Updates were issued of the Thermodynamic Data Estimation Program and Design Institute for Physical Properties Research Database, a thermodynamic properties database maintained in cooperation with the American Institute of Chemical Engineers. Pioneering work in developing new and upgraded data estimation methods was continued, with significant experimental effort aimed at obtaining benchmark data for validation of estimation methods. Pioneering work on techniques for estimating thermodynamic data for hydrocarbon and substituted/heteroatom hydrocarbon species has recently been published in the Journal of Physical and Chemical Reference Data.

• The Chemical Kinetics and Thermodynamics Division's programs for the evaluation and processing of data need additional planning, management, and financial support. A division objective in support of NIST's industrial competitiveness programs should be to expand its data programs.

• The Kinetics Data Center should prepare computerized databases for on-line service on future “electronic highway networks” and develop efficient data estimation algorithms for on-line prediction of data when no measured or calculated data are available.

The Inorganic Analytical Research Division improves the accuracy of inorganic analyses and certifies standard reference materials. The division's 5-year plan includes the development of automated analyses, dissolution techniques, method-dependent analysis, chemometrics, methods of analyzing low-atomic-number elements, documentation, and pure materials.

Outstanding research is being conducted in neutron focusing, laser-based analysis and ultraviolet Fourier transform spectrometry, standard laboratory modules for automated analyses, and depth profiling of light elements.

The Inorganic Mass Spectrometry Laboratory and Cold Neutron Research Facility are recognized as leading laboratories in their fields in the United States. The development of lead standards for paint, rhodium standards, and methods for autocatalyst characterization are important to national health and competitiveness.

Several young researchers are developing national reputations.

• The Inorganic Analytical Research Division's Electrochemistry Program should reconsider its objectives and direction or cut back to maintenance-level support.

• More intergroup and interdivision collaboration is desirable.

• As mentioned in the fiscal year 1992 assessment (p. 119), the Inorganic Analytical Research Division needs additional expertise in chemometrics.

• Publications from the division increased from 37 in fiscal year 1991 to 95 in fiscal year 1992. Over 50 came from the Nuclear Methods Group. Groups other than the Nuclear Methods Group should publish more to increase the visibility of the division and its people. Refereed articles in inductively

coupled plasma mass spectrometry and automation were fewer than the panel would expect. In the case of automation, it appears that publications were being sacrificed in order to manage a consortium.

• Among the emerging technologies in need of the division's metrology services are advanced batteries (e.g., conductivity for solid polymer electrolytes), direct analysis of solids by inductively coupled plasma (glow discharge, laser ablation), molecular spectroscopic techniques, and new laser-based analytical techniques.

The Organic Analytical Research Division's research and development in analytical sensors, measurement automation, gas metrology, mass spectrometry, and separations of organic pollutants develops a wide variety of measurement methodologies and standard reference materials used by its industrial and governmental clientele.

Morale seems high, perhaps because of anticipated major changes in NIST's role.

Equipment is, with exceptions as noted below, reasonably modern and adequate for cutting-edge research. However, the purchase of a needed $500,000 high-resolution magnetic sector mass spectrometer would cause serious budgetary problems.

The Analytical Sensors and Automation Group does cutting-edge research on (1) flow injection immunoassay for determining chemical warfare agents, pesticides, and estrogen hormones, (2) fiber-optic waveguide sensor development, (3) analytical supercritical fluid extraction, (4) laboratory robotics for automating clinical analyses, and (5) biomedical and forensic-related metrology. The group's research in capillary electrophoresis for fingerprinting gunpowder residue is also innovative and has probably generated more publicity for the Organic Analytical Research Division than any previous activity. Laboratory robotics and related chemometrics projects appear to be off to a good start.

The group is acquiring a new Fourier transform infrared/Fourier transform Raman spectrometer that should prove useful for fiber-optic research.

The Mass Spectrometry Group is (1) using electrospray mass spectrometry to characterize biomolecules, (2) developing a definitive method for characterizing serum triglycerides, (3) using capillary electrophoresis and microcolumn high-performance liquid chromatography to separate proteins, (4) developing a definitive or reference method for the analysis of serum thyroxine, (5) measuring and certifying several standard

reference materials for drugs in urine, serum glucose, and cholesterol, and (6) carrying out several small projects for other agencies.

The group's ability to do state-of-the-art research was demonstrated by the recent introduction of electrospray and ion trap technologies.

The Separations Science Group's breadth of competence is impressive. The group's improvements in biomolecule separation will affect the U.S. biotechnology industry.

• The Organic Analytical Research Division, along with CSTL's Thermophysics Division, should focus on the emerging supercritical fluids technology. Supercritical fluid extraction is an increasingly important technique for sample preparation and analysis because it is faster and generates fewer waste solvents than do technologies using conventional solvents. A better understanding of supercritical fluids may lead to commercial separations of various materials. Supercritical fluids are also becoming increasingly useful for waste treatment and cleanup. Physical properties of binary and ternary mixtures need to be examined, and chemical reactivities need to be studied. Several alternative refrigerants are supercritical fluids at moderate temperatures and pressures.

• The Analytical Sensors and Automation Group needs only to continue its current high level of performance.

• The Gas Metrology Group should satisfy the growing demand for more varied standards, particularly those for reactive and unstable materials. Recent federal legislation to improve air quality requires better standard reference material samples of sulfur- and nitrogen-containing compounds, as well as volatile organic compounds. The time pressure in creating new standards to meet demand is great, but some attention to innovations analogous to the type illustrated by permeation tubes may also be warranted.

• The Mass Spectrometry Group should upgrade its 18-year-old magnetic sector mass spectrometer.

• The Separation Science Group should develop capabilities to separate molecules based on chirality. Enantiomeric separations and measurement of ratios of isomers are important to the drug industry, to the study of climate change, and to the study of reaction mechanisms. Separation of optical isomers continues to be one of the most formidable challenges in separation science, although considerable progress has been made.

The Process Measurements Division's Fluid Flow Group has good support from its clients, appropriate expertise, and sound programs. The group has outstanding facilities and staff in Boulder, Colorado, and in Gaithersburg, Maryland, and commendable collaboration occurs. CSTL supervisors make frequent visits to both sites. The consortium programs (Intelligent Processing of Rapidly Solidified Metal Powders and Flow Meter Installation) are well conceived.

The High-Temperature Processes Group has unique facilities and capabilities. The Supercritical Water Oxidation Program is particularly noteworthy. The single-drop studies of the fundamentals of the interaction of focused laser beams with droplets to support optical diagnostics of spray combustion are of high quality. The research dealing with internal circulation within the drop has also been of particular technical interest.

The Reacting Flows Group cooperates with the High-Temperature Processes Group in research on supercritical water oxidation. The ab initio calculations of clustering of silicon atoms are an example of useful and appropriate research that can help explain observations of the sphericity of particles. This work should lead to confidence in calculations for other systems with chemical changes.

Because most of its funding comes from internal sources, including competence building funds, the Process Sensing Group has the flexibility to pursue fundamental programs, e.g., using multiple-sensor arrays to improve neural network analyzers. Building specific arrays of self-assembled monolayers on surfaces offers the possibility of building unique sensors, especially biosensors. Understanding the fundamentals and potential applications of such structures is a worthy objective.

The Thermometry Group has completed much of its current research in the temperature range from 0.65 to about 85 K. After this research is completed, the group's focus will likely shift primarily to calibration. Although the calibration service will be self-supporting, the facility will need to be subsidized.

The Fluid Systems Group's capability in cryogenics and research in flow metering are commendable.

• The Process Measurements Division should emphasize the use of commercial software rather than special user-friendly programs for the transfer of its modeling developments. Also, computational fluid dynamics technology could be transferred more efficiently through collaboration with small user teams rather than with individuals. The panel's experience indicates that a

critical mass of users is needed for the ready adoption of this kind of technology.

• The division should join with the Environmental Protection Agency and the Department of Energy (e.g., through the National Renewable Energy Laboratory) in sharing modeling programs. Modeling of chemical processes offers ways to minimize the waste from, and hazards in, operating chemical processes. Existing simulation programs are deficient in areas involving solids, polymers, multiphase systems, and nonideal systems. Some CSTL programs, such as the examination of incineration products while studying flame characteristics, have been deemphasized or dropped from the division because of lack of outside support.

• Total quality management should be incorporated into the management of all of the Process Measurements Division's programs.

• Outside funding, such as participation in Advanced Technology Program projects, should be incorporated strategically rather than on an ad hoc basis.

• The Fluid Flow Group should expand its applications of computational fluid dynamics, e.g., in the flow meter installation program, the vortex-shedding meter program, and the meter programs at NIST in Boulder. Commercially available codes should be used whenever they can serve the needs of the problem. Emphasis on applications permits researchers to focus on the problem rather than the means to solve the problem and eases the transfer of results to the customer. The group needs to define a new role for itself through dialogue with the Gas Research Institute, Southwest Research Institute, and other potential clients. (The Gas Research Institute has ended its support for the group and now sponsors a facility at the Southwest Research Institute.)

• The High-Temperature Processes Group should concentrate on the fundamentals of the chemistry and flow of supercritical water oxidation, rather than on shorter-term metrology such as corrosion and process verification, even though the shorter-term measurement problems are important to the commercialization of the technology.

• The Process Sensing Group has a major opportunity to contribute to the sensing of low concentrations of toxic substances in waste-gas streams. The group's success will depend on gaining a fundamental understanding of component-surface interactions.

• Under no circumstances should the Thermometry Group decrease its emphasis on research in support of its technology base and calibration capability.

• Cryogenics research in the Fluid Systems Group should be enhanced. The new application will probably be in multiphase flow.

The Surface and Microanalysis Science Division's Atmospheric Chemistry Group's funding for standard reference materials and its OA support have decreased slightly since the panel's fiscal year 1992 assessment but remain at reasonable levels. The level of chemometrical activity has increased within this division and within CSTL. The group has developed an exceptional facility for separating carbon species and preparing them for accelerator mass spectrometry, has applied total quality management concepts to the accelerator mass spectrometry project, and has substantially improved the precision of accelerator mass spectrometry-based isotopic composition measurements through collaboration in the World Ocean Circulation Experiment at the Woods Hole Oceanographic Institution.

The skills of the Microanalysis Group match the new directions facing NIST and CSTL. This group is used to working on practical and applied problems. A nice balance exists between standards, fundamentals, and applied work. The group has developed true state-of-the-art methods in mapping and profiling with ions and electrons.

The Surface Dynamical Processes Group has made significant contributions in surface dynamics. Results from experiments of CO vibrational relaxation on Pt (III) are crucial to understanding energy transfer at surfaces and constitute a major achievement in the field. Laser photochemistry experiments provide an underpinning for surface laser processing. The Fourier transform infrared results of Mo (CO) ₆ on Si (III) 7 × 7 are state of the art and the first example of single-reflection infrared spectroscopy on semiconductor surfaces. These spectroscopic studies are important as technique development, apart from their significance in photochemistry studies. The planned experiments on radical surface interactions are a logical extension of the group 's research.

The Surface Spectroscopies and Thin Films Group has some functional difficulties. Almost all aspects of materials science can be viewed from a surface science or interface perspective. The group's most successful effort, that on magnetic films, may not be able to succeed for lack of personnel. The work on ion interactions with surfaces and x-ray analysis of surfaces is good but seems to be done in isolation. Theoretical work on hot electrons and their role in surface photochemistry is essential to interpreting the related experiments. This work is definitely related to that of other groups but has yet to be fully connected with that work.

The Atmospheric Chemistry Group has a good balance of funding from other agencies, Congress (STRS), and NIST's Standard Reference Materials Program. The group has acquired a mass spectrometer to provide stable isotopic ratio measurements to complement existing radiocarbon capabilities and is beginning to use its new mass spectrometric capability to measure the isotopic compositions of tropospheric CO and CH₄. These measurements are important to understanding possible global climate changes due to anthropogenic activities as well as possible biogenic contributions to urban ozone problems and have led to the start of an international program for developing natural gas isotopic standards.

The group uses accelerator mass spectrometry to determine ¹⁴C in samples of airborne particles to distinguish between carbon masses produced by fossil fuel combustion and those produced by sources such as wood burning. This research is done in conjunction with the Environmental Protection Agency and the academic research community. Continuing efforts are being made to improve the chemical and isotopic analysis of volatile organic compounds. The calibration facility provided by the reference ozone photometer continues to be critically important in studying the significant national and international air quality problems of urban and regional ozone.

The expanded effort in statistical analysis of chemical data (chemometrics) has continued. As part of the chemometrics initiative, the Atmospheric Chemistry Group has begun work on developing standard test data for chromatography that would provide the analytical community with data sets to test and validate new chemometrical methods. The group has assisted in the statistical questions involved in DNA fingerprinting in forensic problems, and it is becoming increasingly involved in other activities in CSTL as problems of instrument optimization and data analysis increase. The group has a good record of publication and information dissemination.

The Microanalysis Group's leader is piloting excellent staff scientists who are excited about their work. The molecular mapping with secondary ion mass spectrometry is particularly impressive. This molecular method is complemented by the secondary ion mass spectrometry-depth profiling with focused ion beams and the elemental mapping with field-emitted electrons. These first-rate techniques are being applied to practical problems and are establishing important metrology standards.

The Surface Dynamical Processes Group is clearly the world's leader in surface energy transfer. The most recent experiments on energy transfer between electron-hole pairs and surface adsorbates are extremely important to a basic understanding of surface dynamics. The group is doing excellent science and is positioning its research for continued success.

The experimental and theoretical research in the Surface Spectroscopies and Thin Films Group is first-rate.

Development of a scanning scattering microscope for diagnosing surface roughness should have been pursued vigorously but was not because of a lack of resources.

• Core microelectronics processing competence and nanofabrication facilities should be developed to support NIST's semiconductor processing and nanostructured materials initiatives.

• The Surface and Microanalysis Science Division should acquire access to scanning tunneling and atomic-force microscopy instrumentation in order to participate in NIST's nanostructured materials initiative. Even though such instrumentation is available in other NIST laboratories, CSTL should consider the merits of having the instrumentation within the Surface and Microanalysis Science Division.

• The Microanalysis Group should expand into nanofabrication (e.g., ion milling) and scanning tunneling microscopy/atomic-force microscopy surface analysis.

• There should be no downsizing in the Surface Dynamical Processes Group, whose planned studies of surface reactions could make significant technological contributions. The group's current noteworthy research equipment originated in or is shared with the Physics Laboratory; therefore, further relocation of the group's staff and facilities should retain the Surface Energy Transfer Laboratories in close proximity to counterparts in the Physics Laboratory.

• The Surface Spectroscopies and Thin Films Group should consider adjusting its mix of expertise to consolidate an excellent working team. The addition of a surface kineticist to this group would help to fortify the surface processing theme and balance the predominantly physics work with more chemical expertise. Such a team could tackle numerous questions associated with surface processing with a unique combination of expertise.

Two Thermophysics Division groups are located in Boulder, Colorado, and three are located in Gaithersburg, Maryland; however, the activities and goals of these five groups are well coordinated. The close working relationship between the Properties of Fluids Group (Boulder) and the Fluid Science Group (Gaithersburg) is especially important and effective.

A reorganization was completed almost 6 months ago in which (1) the Subsecond Thermophysics Group was eliminated; (2) a Process Separations Group was formed, with some of its staff

coming from the defunct Chemical Engineering Group; and (3) several members of the Properties of Fluids Group were assigned to a new Process Separations Group.

The Thermophysics Division's budget is less than 50 percent base funding. Most proposals to outside agencies are team-oriented rather than based on a single principal investigator. Very little funding for research and determination of physical properties comes directly from single companies. Rather, industrial grants are from trade associations, such as the Gas Research Institute (natural gas properties), the Air Conditioning and Refrigeration Technology Institute, and the Electric Power Research Institute (alternative refrigerants). Primary sources for other federal agency funding are the Department of Energy, the Department of Defense, the National Aeronautics and Space Administration, and the Environmental Protection Agency. The low percentage of base funding threatens the operation, stability, and morale of the division, especially the Boulder groups.

The division has an interest in patents and intellectual property, but as yet, a coherent strategic plan for technology development and licensing in partnership with industry is not evident.

The Process Separations Group is developing robust computer modeling software to solve convective-diffusion transport problems with chemical reaction and complicated flow geometries. Applications to metal-organic chemical vapor deposition and electrochemical deposition have been achieved.

The Properties of Fluids Group has maintained excellence in thermophysical property measurements. The work done through experiment, theory, empirical correlation, and computer simulation is well integrated and is an excellent example of how these activities can be combined to produce high-quality standard reference data and to address industrial needs for design data. The combination of range, accuracy, and precision of the experimental work done at Boulder, including pressure-volume temperature, heat capacity, phase equilibrium, speed of sound, and thermal conductivity, is unique in the world. The data produced find widespread use in the gas, petroleum, and chemical industries, and contacts with industry ensure that measurements are attuned to current needs. Together with the Fluid Science Group, the Properties of Fluids Group has taken the national leadership role in the collection, evaluation, correlation, and publication of thermophysical property data for alternative refrigerants.

Work in the Fluid Science Group on the investigation of supercritical water oxidation of hazardous chemicals can be combined with other NIST activities in supercritical flow technologies to develop a new competency in response to recognized environmental problems.

The Vacuum Group was very productive in fiscal year 1993 with three complex research and development projects generating the group's first results. A transition flow standard was completed to give NIST the capability of providing pressure calibrations over a continuous range from ultrahigh vacuum (< 10^-7 Pa) to high pressures (600 MPa). A low-density water vapor standard was fabricated and characterized. Measuring low gas densities using a resonant multiphoton ionization technique was demonstrated.

The Pressure Group has a reputation for world-class research in the fundamental effects of viscosity on gauge operation and gauge characterization.

One-third of the Process Separations Group's effort pertains to membranes, including facilitated-transport membranes for H₂S separation in fuel gas and modification of ultrafiltration membranes with adsorbed polymers to avoid fouling. Ten to twenty percent of the effort focuses on supercritical fluids for extractive separations and analytical chromatography. A large project on detecting polychlorinated biphenyls in natural gas pipelines is supported by an industrial consortium.

Using its own and data from other sources, the Properties of Fluids Group has developed a wide array of databases and empirical and theoretical correlations to support activities in custody transfer, process design, improved energy efficiency, and environmental safety. The group' s efforts are further supported by fundamental research with neutron scattering experiments and computer simulations. A vapor-liquid equilibrium project designed to address systems of importance to the gas industry is well organized and highly productive. It includes carefully prepared plans to combine measurements of phase compositions, phase densities, and interfacial tension.

High-quality precise measurements of the thermal conductivity and diffusivity of fluids are being made using a heated-wire technique. Special problems associated with the polar nature of alternative refrigerants are understood and have been corrected. The heat capacity measurements are a fine example of state-of-the-art experiments in measuring properties of fluids. The dual sinker densimeter is an ambitious project designed to extend the state of the art in experimental measurements of fluid densities. In keeping with its traditions, the Boulder group remains at the forefront of experimental techniques for property measurements.

Activities of the Fluid Science Group in alternative refrigerants and supercritical water oxidation, as well as fundamental constants and properties, are excellent and responsive to national need.

The Vacuum Group's work on transition flow standards and water standards is useful for materials processing applications. This work, along with continuing activities in the group to improve the accuracy of total pressure, partial pressure, and flow measurements in vacuum environments, can be combined successfully with other activities within the CSTL that support process measurement technology for the semiconductor industry (such as the fluid flow metrology in the Process Measurements Division).

Optical density measurements have been demonstrated for CO partial pressures over a wide dynamic range. When this technique is extended to other active gases (such as O₂, H₂O, and H₂), there are significant applications for density measurements in systems when gas temperatures are indeterminate, such as cold bore tube particle accelerators (e.g., the Continuous Electron Beam Accelerator Facility).

The group provided its clientele with a significant volume of calibration services in fiscal year 1993 for the complete range of vacuum and flow instrumentation.

To augment its fundamental work, the Pressure Group is developing collaborations with industry. One Cooperative Research and Development Agreement is in progress; another is under negotiation.

• The Thermophysics Division should continue to emphasize precision measurements of physical properties rather than the development of generic technology.

• The computer modelers in the Process Separations Group should become more involved in the projects of the Properties of Fluids and Fluid Science groups. Apparently, such collaboration is contemplated in the division's proposed initiative for developing technology for eliminating environmental pollutants.

• The Fluid Mixtures Data Center should investigate the data needs of chemical process simulators used in computer-aided design software. Theory and modeling by the Fluid Mixtures Data Center should be better coordinated with other efforts in the division.

• The potential impact of supercritical fluids projects should be evaluated.

• External support, especially from industry, is important to the Thermophysics Division's mission; however, base funding should be at least 60 percent.

• The neutron scattering metrology of the Properties of Fluids Group also might be used for measuring molecular solutes adsorbed on the surface of minerals such as clay and be useful for environmental cleanup monitoring.

• The Vacuum Group should further automate measurements in order to eliminate the current 3-month backlog in delivering vacuum calibrations.

• The Pressure Group should identify new opportunities for standards development and related research. A possible area of investigation is the analysis of pressure sensors used in chemical processing, particularly those based on silicon.

In early 1993, NIST requested evaluation of three NIST-wide issues (see Appendix D for definitions and details) that apply particularly to CSTL.

The inadequacy of NIST's support of CSTL's Standard Reference Data and Standard Reference Materials programs was a major panel concern in its fiscal year 1992 assessment (p. 118). In this fiscal year 1993 assessment, the panel again finds the attention, visibility, and resources given to CSTL's development of standard reference materials, standard reference data, and databases to be inadequate. Although the importance of these efforts to industry and the scientific and engineering communities does not make daily headlines, their significance should neither be underestimated nor given lower priority than the more glamorous precommercial or emerging technology research and development. The panel believes that NIST 's evaluated data and related measurement services have proved their merit and are probably the most valuable service that NIST can provide to enhance the competitiveness of U.S. industry. To be even more effective in this vital endeavor, CSTL need only be more proactive in meeting the database and calibration needs of U.S. technical and industrial communities. CSTL's visionary leadership and experience are invaluable in this critical infrastructure function.

• Issue: Is there proper balance between meeting short-term customer data needs (that also bring sales income to the data program) and longer-term customer needs, particularly those of industry?

  Panel Assessment. The current practice of using revenue from sales of evaluated data as the primary funding mechanism for ongoing data program activities guarantees that CSTL will focus

on short-term needs. CSTL divisions active in data compilation and evaluation activities do not have sufficient core funding to make longer-term investments in data program activities, and the Standard Reference Data Program does not have significant resources to invest in longer-term activities either. The net result is an unbalanced focus on short-term needs.

• Issue: Since industry's needs are extremely large in scale and scope compared to NIST's resources, what should NIST's niche be in producing industrially important data?

  Panel Assessment and Recommendation. Commercial sources of data can often meet industry's immediate needs for specific data. The CSTL should focus on more comprehensive data compilations and evaluations aimed at intermediate and longer-term needs. This is not likely to happen, however, since CSTL has only taken resources for maintaining data program activities. An advisory panel of industrial and other non-NIST scientists and engineers should be established to confirm NIST's assessment of longer-term industrial data requirements and to design responsive data programs.

• Issue: What should be the balance between NIST's data programs and other research and services?

  Panel Assessment and Recommendation. While CSTL should maintain an appropriate balance among standards development, generic technology development, fundamental research, and data programs, the panel wishes to emphasize that CSTL has a unique capability in the standard reference data area. No other U.S. laboratory is going to provide the level of compilation and evaluation of numerical chemical data that CSTL currently provides. Many CSTL staff members, particularly those leading data program activities, perceive that evaluated data efforts are not highly regarded by current NIST management. However, such programs are highly valued by the panel as one of CSTL's most successful technology transfer activities. NIST and CSTL need to upgrade the perceived and real status of the data programs by assuring that the data programs have priority at least equal to other research and technology development activities.

• Issue: Are CSTL's data programs focused on the right things (e.g., the customers' highest-priority data needs)? How does CSTL assure itself (and others) of this?

  Panel Assessment. Most of the CSTL data program activity is funded by data product sales revenue or other federal agency funding. In each case, the funding mechanism pressures CSTL data staff to be responsive to the customer's concerns, either by developing upgrades and updates to popular products or by fulfilling the funding sponsor's work statement. However, longer-term customer needs are sacrificed by focusing on immediate customer needs. (See also discussion above.)

• Issue: Are there high-priority gaps or other needs that are not being addressed?

  Panel Assessment. The increasing efforts of U.S. industry to design and implement environmentally acceptable processes and products will require extensive databases on chemical thermodynamic, kinetic, and spectroscopic properties. Existing databases should be expanded and new databases initiated to meet industrial and governmental needs.

• Issue: What tools are being employed, and how effective are they, to strategically adjust the data programs to meet industry's emerging needs?

  Panel Assessment. On the technical front, future databases will largely be on-line products subject to continuous update. Recent CSTL activities have moved NIST from printed text to computer disk formats. Attention now needs to be paid to on-line distribution in conjunction with the federal National Information Infrastructure initiative. Furthermore, increasingly agile theoretical algorithms should be incorporated into data programs to provide computed data where measured or previously computed data are not available. The on-line nature of future databases will enhance this built-in data estimation capability.

The CSTL panel strongly endorses NIST's development and maintenance of traditional and unique basic and secondary measurement standards, physical science data evaluations, reference sample materials, and fundamental constants. NIST's contributions to technology development are certainly worthwhile and cost-effective; however, at CSTL's current funding levels, too great an emphasis on generic technology development could adversely divert resources from research that leads to measurement and data services critical to U.S. industry. The panel's strong conviction is that there should be no further reduction in fundamental research and laboratory-based standards work.

CSTL's assistance to NIST's extramural programs has augmented CSTL's funding, facilitated external connections, and stimulated new opportunities. The current level of CSTL's support of NIST's extramural programs is manageable. However, there appears to be some confusion among CSTL's research staff about the availability of the 10 percent of Advanced Technology Program funds that NIST is authorized to allocate to the intramural programs. Also, if the size of the extramural programs increases, CSTL could become too involved in them, causing significant management problems because CSTL's

professional staff is spread too thin already. The specificity and short time frames of the individual extramural projects could easily divert too much of CSTL's attention and resources from CSTL's statutory mission if the volume of extramural requests for assistance increases.

The CSTL director asked the panel to address several specific issues in its fiscal year 1993 assessment. Brief summaries of the panel 's findings follow:

• Is CSTL maturing as a unit? Are collaborations and communications developing appropriately?

  Panel Response. Significant progress is being made. A number of promising cooperative activities are under way in which the researchers are very enthusiastic about the work. The staff are generally positive about laboratory management. Some individuals still have not achieved a desirable degree of involvement; however, such difficulties exist in all organizations. Continuation of the current level of communication and collaboration will, in time, thoroughly integrate CSTL's strengths.

• Have the proper course and strategic thrusts been set?

  Panel Response. Yes. The principal remaining task is to ensure that the research staff fully understands the broad goals as well as the specifics of the strategy and develops responsive tactics at their particular levels.

• Are there needs for emerging technologies not being addressed that should be?

  Panel Response. Some important emerging technologies have been identified by CSTL, and others are suggested by the panel in this report. The principal concern of the panel is that CSTL's resources are inadequate to provide the level of support for emerging technologies that Congress intends.

• Are there needs for standard reference data, standard reference materials, and calibration services that are not being addressed?

  Panel Response. As described in the fiscal year 1992 report and elsewhere in this report, the panel is concerned about CSTL's current lack of support for these traditional functions. CSTL must give this NIST-wide issue higher priority if CSTL is to meet extensive diverse customer base needs.

• How should longer-term data program activities be funded?

  Panel Assessment. Up to 10 percent of the funds of the Advanced Technology Program can be allocated for NIST's internal support of ATP activities. NIST 's data programs are of great value to U.S. industry; therefore, at least 5 percent of these internal ATP funds (or 0.5 percent of all ATP funds) should be allocated to relevant data program activities.

• Are short-term projects an acceptable expedient for dealing with inadequate funding?

  Panel Assessment. The necessity of responding to marginally significant technological requests and a diminished opportunity to plan or make commitments are real dangers to CSTL, as are the complex demands on management and stresses on researchers. CSTL's major strengths are scientific sophistication and vision. These strengths should not be sacrificed for survival or for services that could be provided by others.