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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 4 Chemical Science and Technology Laboratory
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 PANEL MEMBERS Arlene A. Garrison, University of Tennessee, Chair James W. Serum, Viaken Systems, Inc., Vice Chair Thomas M. Baer, Arcturus Engineering, Inc. Alan Campion, University of Texas at Austin Pablo G. Debenedetti, Princeton University Robert R. Dorsch, DuPont Life Sciences Robert E. Ellefson, Leybold Inficon, Inc. Daniel L. Flamm, The Microtechnology Analysis Group Walter W. Henslee, Dow Chemical Company E. William Kaiser, Ford Motor Company Roy S. Lyon, Eurofins Scientific, Inc. James D. Olson, Union Carbide Corporation Frank K. Schweighardt, Air Products and Chemicals, Inc. Jay M. Short, Diversa, Inc. Christine S. Sloane, General Motors Corporation Anne L. Testoni, KLA-Tencor Corporation Edward S. Yeung, Iowa State University Submitted for the panel by its Chair, Arlene A. Garrison, and its Vice Chair, James W. Serum, this assessment of the fiscal year 2000 activities of the Chemical Science and Technology Laboratory is based on site visits by individual panel members, a formal meeting of the panel on February 29-March 1, 2000, in Gaithersburg, Md., and documents provided by the laboratory.1 1 U.S. Department of Commerce, Technology Administration, National Institute of Standards and Technology, Chemical Science and Technology Laboratory: 1999 Technical Activities Report, NISTIR 6445, National Institute of Standards and Technology, Gaithersburg, Md., 2000.
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 LABORATORY-LEVEL REVIEW Laboratory Mission According to laboratory documentation, the mission of the Chemical Science and Technology Laboratory (CSTL) is to provide the chemical measurement infrastructure to enhance U.S. industry's productivity and competitiveness, ensure equity in trade, and improve public health, safety, and environmental quality. CSTL carries out its mission by providing U.S. industry with engineering measurements, data, models, and reference standards in order to enhance U.S. industrial competitiveness in the world market. The mission of the Chemical Science and Technology Laboratory fully reflects the mission of NIST to strengthen the U.S. economy and improve the quality of life by working with industry to develop and apply technology, measurements, and standards. The CSTL staff are dedicated to providing standards that strengthen the vertical traceability structure of measurement in the United States. For example, during fiscal year 1999, CSTL provided 53 percent of NIST's Standard Reference Materials (SRMs) units and 17 percent of the calibration services. CSTL is also committed to leading in global standards organizations for chemical and physical measurements. In addition, CSTL maintains numerous programs to anticipate and address the next generation of measurement needs in chemistry and chemical engineering and, ultimately, to maintain a competitive position for U.S. industry in the future. Technical Merit and Appropriateness of Work The quality of the technical programs across the divisions of CSTL and the level of collaborations between the divisions have exceeded the panel's expectations. The technical work across all divisions was found to be of high quality, and in several areas it is world-class. This is further demonstrated by recent benchmarking activities undertaken by CSTL, comparing CSTL's capabilities in several measurement areas against those of other international laboratories realizing SI (International System of Units) and SI-derived units. This exercise showed CSTL to be world-class to best-in-class in these areas. The divisional reports below provide more detailed assessments of the technical merit of ongoing programs. Some highlights are cited here to give the reader evidence of the breadth of CSTL programs. An excellent example of a well-targeted program is the continuing development of cavity ring-down spectroscopy (CRDS) for use in sensing low-level gaseous contaminants in manufacturing processes. The level of precision measurements obtained with this method puts the detection sensitivity very close to the International Technology Roadmap for Semiconductors (ITRS)2 2001 target for measuring water vapor in semiconductor fabrication lines. The CRDS project originated as a Competence program and matured to a regular program this year. A second example of note is the development of nuclear magnetic resonance (NMR) and fluorescence spectroscopy methods to screen the binding of ligands to RNA. This is of significance since protein-nucleic acid complexes provide new targets to regulate or inhibit gene expression and viral and bacterial infection. The CSTL has developed a general method for screening and optimizing inhibitors of such nucleic acid-protein complexes. Another program of outstanding technical merit and significant importance is work to develop better screening procedures for cloth swipe samples obtained in International Atomic Energy Agency (IAEA) inspections of ura 2 Semiconductor Industry Association, International Technology Roadmap for Semiconductors, Semiconductor Industry Association, San Jose, Calif., 1999.
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 nium enrichment plants. CSTL researchers aim to improve the efficiency and reliability of current methods and improve the detectability of uranium-235 (235U). Such measurements are a critical component of verification called for by current and proposed arms control treaties. Another internationally important effort is CSTL work with international groups developing and promulgating refrigerant standards. As ozone-depleting chlorofluorocarbon and hydrochlorofluorocarbon refrigerants are phased out, it is important that international standards for thermodynamic and transport properties of refrigerants are in place to allow U.S. manufacturers to sell their products globally. CSTL efforts in measurement technologies for combinatorial chemistry techniques, such as microfluidic measurement technology and gas sensing with microhotplate sensor arrays, are good examples of interdivisional collaboration. These efforts also have potential high payoff as microchip combinatorial methods become more and more practical for widespread use. CSTL is playing a leading role in both national and international standards intercomparisons. For example, CSTL and the Bureau International des Poids et Mésures have prototyped a database with data from key and supplementary international comparisons of measurements and standards. This database is searchable by area of metrology and country of participation (<http://icdb.nist.gov>). Such easy access to information will further drive information exchange, and the implementation of this database was one of the key action items in a mutual recognition agreement (MRA) signed by the national measurement institutes (NMIs) of 38 nations. Successful implementation of this MRA facilitates acceptance of U.S. measurements and standards in foreign markets. CSTL is also an active participant in the assessment of chemical measurement comparability by the Comit é Consultatif pour la Quantité de Matière (the Consultative Committee for the Amount of Substance). The Analytical Chemistry Division has provided much of the leadership on this effort; additional information on these activities can be found in the divisional reports below. The CSTL has made significant progress in developing and utilizing planning processes to make decisions on the continuation of existing programs and the choice of new ones. The programs going on overall are strategically chosen to address scientific areas relevant to the NIST mission. The CSTL evaluates each proposed and ongoing project against the criteria of (1) industrial need, (2) match to division and CSTL missions, (3) ability of CSTL to make a difference in the field, (4) anticipated nature and size of CSTL impact, and (5) anticipated timeliness and quality of CSTL work. The laboratory continues to work hard to ensure it balances work in traditional measurement science with new technical opportunities that may be of importance for future industries. Most importantly, the laboratory has begun putting in place measurable goals and objectives for the quality and appropriateness of its work. The panel applauds this effort and acknowledges that it is difficult to assign goals and objectives to long-term research. However, such research can benefit from the organization and forward thinking provided by tools such as metrics, time lines, and technical roadmaps with quantitative milestones. Impact of Programs The CSTL has done an impressive job of disseminating its results to a wide scientific audience in industry, government, and academia. Laboratory staff utilized publications, conferences, workshops, and the Internet to disseminate their results. In 1999, CSTL staff authored 417 peer-reviewed publications. Citation analysis shows that CSTL publications are extensively referenced by other scientists, a strong indication of the significance of the work. Although CSTL continues to broaden the means by which it disseminates its results (especially increasing its use of the Internet), further efforts in this direction could be fruitful. The impact of the laboratory's work on industry is also reflected in numbers of reference materials and databases sold, Web site hits, and calibrations performed. In 1999, approxi
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 mately 17,000 chemistry-related SRMs and 683 Standard Reference Databases (SRDs) were sold and 910 calibrations performed by CSTL. Of course, such output numbers do not by themselves give a sufficient measure of the impact of CSTL programs. The laboratory recognizes this and seeks to measure the success of its programs in various ways. In fiscal year 1999, CSTL commissioned an economic impact study of its SRM for sulfur in fossil fuels. This study showed positive impact on production efficiency, environment, and health. It concluded that a conservative benefit-to-cost ratio for this program was 113 and the social rate of return was 1,056 percent.3 This and previous economic impact studies demonstrate quantitatively the effectiveness of a sample of CSTL programs and their impact on the U.S. economy. CSTL should continue to utilize the tool of economic impact analysis as part of its process of continuous evaluation and improvement of effectiveness. Globalization of industry means that various sectors have increased need for measurement traceability to NIST. These sectors include electronics, automotive, and aerospace and involve measurements impacting such factors as environment, health, and safety. The NIST Traceable Reference Materials (NTRM) Program is a CSTL response to the need to provide traceable references to a broad and growing number of customers through a network of NIST traceable secondary standard suppliers. The success of this program will require continued proactive management of planning and implementation of program activities. The evolution of industries and their products makes it vital that CSTL continue efforts in developing new and advanced reference materials in order to lead worldwide efforts to ensure traceability of product and service quality and safety. The laboratory's leadership role in driving global standards has a huge impact on U.S. industrial competitiveness. The importance of this work is well recognized by management and staff. However, there are insufficient resources to dedicate the necessary personnel to this critical task while maintaining other standards responsibilities. The CSTL has a number of research collaborations with industrial partners, and this is one good indication of the potential impact of its work. The laboratory should consider that the metrics for assessment of industrial relevance change as a function of time and maturity of work in any area. For example, the relevance of programs in the earliest stage of development can be gauged from attendance at workshops on the topic—both quality and quantity of attendees (i.e., which and how many companies and individuals attend). Midstage programs can be gauged by listing and describing briefly all of the significant interactions with external clients. (A good example of such a list was provided by the Physical and Chemical Properties Division.) Late-stage or completed programs that are major successes are subject to economic impact evaluation, a good but expensive tool whose use should continue. A less exhaustive and expensive evaluation mechanism is needed for all completed programs, perhaps an extended form of the suggested midstage evaluation. Laboratory Resources Funding sources for the Chemical Science and Technology Laboratory are shown in Table 4.1. As of January 2000, staffing for the Chemical Science and Technology Laboratory included 275 full-time permanent positions, of which 235 were for technical professionals. There were also 117 nonpermanent and supplemental personnel, such as postdoctoral research associates and part-time workers. 3 National Institute of Standards and Technology, 00-1 Planning Report: Economic Impact of Standard Reference Materials for Sulfur in Fossil Fuels, February 2000, available at <http://www.nist.gov/director/prog-ofc/report00-1.pdf>.
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 TABLE 4.1 Sources of Funding for the Chemical Science and Technology Laboratory (in millions of dollars), FY 1997 to FY 2000 Source of Funding Fiscal Year 1997 (actual) Fiscal Year 1998 (actual) Fiscal Year 1999 (actual) Fiscal Year 2000 (estimated) NIST-STRS, excluding Competence 37.0 37.8 37.9 37.4 Competence 1.9 2.0 2.4 2.3 ATP 2.0 3.0 3.0 2.8 Measurement Services (SRM production) 2.3 2.3 2.4 3.2 OA/NFG/CRADA 10.0 9.6 10.9 10.9 Other Reimbursable 2.8 3.0 3.4 3.1 Total 56.0 57.7 60.0 59.7 Full-time permanent staff (total)a 281 280 276 275 NOTE: Funding for the NIST Measurement and Standards Laboratories comes from a variety of sources. The laboratories receive appropriations from Congress, known as Scientific and Technical Research and Services (STRS) funding. Competence funding also comes from NIST's congressional appropriations but is allocated by the NIST director's office in multiyear grants for projects that advance NIST's capabilities in new and emerging areas of measurement science. Advanced Technology Program (ATP) funding reflects support from NIST's ATP for work done at the NIST laboratories in collaboration with or in support of ATP projects. Funding to support production of Standard Reference Materials (SRMs) is tied to the use of such products and is classified as Measurement Services. NIST laboratories also receive funding through grants or contracts from other government agencies (OA), from nonfederal government (NFG) agencies, and from industry in the form of Cooperative Research and Development Agreements (CRADAs). All other laboratory funding, including that for Calibration Services, is grouped under “Other Reimbursable.” a The number of full-time permanent staff is as of January of that fiscal year. CSTL's ability to do world-class measurements is clearly affected by the caliber of the facilities, equipment, and human resources allocated to its projects. In 1999, the Analytical Chemistry and Biotechnology Divisions relocated into the new Advanced Chemical Sciences Laboratory. This move had significant positive impact, which is discussed in the divisional reports. Facilities improvement continues to be a major issue for the other three divisions. Construction of the planned Advanced Measurement Laboratory (AML) is essential to maintaining the best-in-class outputs of the calibration laboratories in CSTL. Construction is scheduled to begin in the fall of 2000, and the anticipated completion date is expected to be a minimum of 4 years away. As discussed in the fiscal year 1999 report, the panel is concerned about short- and midrange planning to deal with the inadequacies of the current building. It is critical that CSTL implement a facility plan to address the interim period prior to completion of the AML. Laboratory space utilized by CSTL in Boulder is particularly below standard. Impacts of the facilities on ongoing programs are detailed in the divisional reports below. The panel identified some concerns regarding capital equipment funding for specific programs. The current operational lifetime of scientific hardware is highly limited, and funding must be monitored carefully to ensure that needed funds are being appropriated to key areas to maximize CSTL's impact on U.S. industry. The panel noted the need for a capital equipment plan in its 1999 report and reiterates the importance of such a plan. Specific capital equipment concerns are discussed in the divisional reports. The quality of CSTL staff is superb. This is CSTL's greatest resource. The panel also acknowledges the leadership of the CSTL director, who is keenly attuned to the measurement needs of the
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 laboratory's constituents and who works tirelessly and creatively to direct CSTL to meet these needs. His recent election to the National Academy of Engineering underscores the excellence of his work. The panel is particularly pleased that CSTL researchers are involved in several interlaboratory projects. It is also pleased to note that these projects were supported by the appropriate division and laboratory resources and did not seem to require additional incentives to encourage this activity. An internal NIST Web site listing staff expertise throughout the laboratories appears to be an excellent tool for enabling collaborations and is used by many CSTL staff. Specific examples of collaborations are mentioned in the divisional assessments. DIVISIONAL REVIEWS Biotechnology Division Division Mission According to division documentation, the mission of the Biotechnology Division is to provide the measurement infrastructure necessary to advance the commercialization of biotechnology. It seeks to do this by developing a scientific and engineering technical base and reliable measurement techniques and data to enable U.S. industry to produce biochemical products quickly, economically, and with appropriate quality control. The division's current programs address its mission as defined. This mission is particularly challenging in light of the rapid growth of biotechnology. Technical Merit and Appropriateness of Work The Biotechnology Division continues many well-targeted and high-quality programs in the areas of DNA technologies, bioprocess engineering, structural biology, biomolecular materials, and bioinformatics. The division participates in the CSTL planning process and utilizes the CSTL criteria when considering program initiation, continuation, and termination. The DNA Technologies Group continues to play a pivotal role supplying SRMs for application in areas related to the detection and characterization of DNA. Its support of the nation's crime laboratories with DNA standards for forensics provides an excellent example of relevant and highly valuable standards developments. In fiscal year 1999, the group issued a new SRM for mitochondrial DNA sequencing, which is widely used in forensics work but also has applications in medical diagnostics. In collaboration with the National Institute of Justice, the group has begun automating matrix-assisted laser desorption ionization (MALDI)-Time of Flight (TOF) mass spectrometry for rapid DNA testing and identification of human alleles. It has recently updated its forensic database for short tandem repeats (<http://www.cstl.nist.gov/biotech/strbase>) to include new information on rare variant alleles. Use of short tandem repeats is rapidly becoming the preferred forensic method of human identification worldwide. The Bioprocess Engineering Group focuses on the development of measurement methods, databases, and generic technologies related to the use of biomolecules and biomaterials in manufacturing. Measurement methods and data are under development in protein biospectroscopy to apply spectroscopic and electrochemical techniques to characterize energy-transfer processes in biomolecules. Recent work has aimed at developing enzyme-coated electrodes that might lead to biosensors for detecting and remediating contaminated bodies of water. The group has also been actively soliciting industrial input concerning the development of fluorescent standards for biomedical and biochemical research.
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 Several collaborative research projects are under way in biocatalytic systems. These projects use a variety of techniques—chromatography, microcalorimetry, site-directed mutagenesis, 15N NMR, x-ray crystallography, and computational techniques—to characterize structure and thermodynamics of enzymatic transformations. These techniques are being used to address potentially industrially important biotransformation problems such as those found in hydroxylation and aromatic amino acid metabolic pathways. For example, calorimetric studies carried out in 1999 and planned for 2000 should complete data collection on the full thermodynamics of the chorismate metabolic pathway. This pathway has potential importance as a process for the chemical, agricultural, and pharmaceutical industries. This is part of an effort at the joint NIST-University of Maryland Center for Advanced Research in Biotechnology that will provide one of the first examples of an integrated analysis of a metabolic pathway: from gene sequence to protein sequence to thermodynamic analysis of the chemical reactions. In fiscal year 1999, the Research Collaboratory of Structural Bioinformatics, a collaboration between the NIST Biotechnology Division, Rutgers University, and the University of California at San Diego Supercomputing Center, assumed responsibility for the Protein Data Bank (PDB). The PDB is the most comprehensive international repository for processing and distribution of three-dimensional structural data for biological macromolecules. This Web-based tool (<http://nist.rcsb.org/pdb/>) was recognized by the publication Genetic Engineering News as one of the top 50 influential Web sites in biotechnology. Currently, up to 75 new structures are entered per week, and the site has more than a million hits per month. This activity is a marriage of NIST 's traditional strength in data and databases with the emerging area of biotechnology and is a very appropriate project for this division. Impact of Programs The Biotechnology Division continues to disseminate its work via publications, research seminars, and industrial contacts. The division 's publications increased from 96 in 1998 to 118 in 1999. The division presented more than 250 talks at seminars, conferences, and other venues in 1999. It has also maintained a number of Internet databases such as the Short Tandem Repeat (STR) DNA Database and the Biological Macromolecule Crystallization Database (BMCD), which receive significant numbers of hits, and it cross-referenced the BMCD with the Nucleic Acid Database. The efforts in these areas are excellent and the division is encouraged to continue such dissemination efforts. It is clear to the panel that this division will have a significant impact on the biotechnology industry. As one example, the Bioinformatics Group has the potential for achieving significant economic impact through its sequence, functional, and structural data analysis. However, the division is challenged by the speed with which this industry is developing and is limited by its small size. Biotechnology's influence is rapidly expanding into practically every sector of industry as biological systems are integrated into materials processes, sensors, agricultural chemicals, and other products. Therefore, the panel believes that additional resources are necessary to fully realize the mission of the Biotechnology Division. Division Resources Funding sources for the Biotechnology Division are shown in Table 4.2. As of January 2000, staffing for the Biotechnology Division included 35 full-time permanent positions, of which 31 were for
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 TABLE 4.2 Sources of Funding for the Biotechnology Division (in millions of dollars), FY 1997 to FY 2000 Source of Funding Fiscal Year 1997 (actual) Fiscal Year 1998 (actual) Fiscal Year 1999 (actual) Fiscal Year 2000 (estimated) NIST-STRS, excluding Competence 6.9 6.6 6.5 6.5 Competence 0.5 0.9 0.8 0.7 ATP 1.3 1.9 1.7 1.7 Measurement Services (SRM production) 0.1 0.0 0.1 0.0 OA/NFG/CRADA 0.8 0.9 1.7 2.1 Other Reimbursable 0.1 0.0 0.1 0.2 Total 9.6 10.3 10.9 11.2 Full-time permanent staff (total)a 31 35 37 35 NOTE: Sources of funding are as described in the note accompanying Table 4.1. a The number of full-time permanent staff is as of January of that fiscal year. technical professionals. There were also 33 nonpermanent and supplemental personnel, such as postdoctoral research associates and part-time workers. The division's facilities in the new Advanced Chemical Sciences Laboratory have greatly increased productivity and improved morale. The importance of such facilities for attracting top scientific talent should not be underestimated. Despite the quality of NIST researchers and the steady flow of guest researchers, the division has a shortfall of trained microbiologists. The dynamic nature of biotechnology-based industries requires an evolving Biotechnology Division that continues to explore new areas and continuously reassesses older programs against desired objectives and continued relevance. Entirely new approaches in biotechnology can be invented, commercialized, and become obsolete in less than 5 years. Biotechnology is experiencing unprecedented advances and growth, at a pace similar to information technology and electronic commerce. NIST has recently made substantial investments in these areas, and the panel believes that NIST must make greater efforts in biotechnology to adequately serve the needs of this developing area of U.S. industry. Process Measurements Division Division Mission According to division documentation, the mission of the Process Measurements Division is to develop and provide measurement standards and services, measurement techniques, recommended practices, sensing technology, instrumentation, and mathematical models required for analysis, control, and optimization of industrial processes. The division's research seeks fundamental understanding of chemical process technology and generates pertinent critical data in support of this goal. These efforts include the development and validation of predictive computational tools and correlations, computer simulations of processing operations, and the acquisition and critical evaluation of chemical, physical, and engineering data.
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 The panel believes that the division's goals and projects are generally consistent with this mission statement and also contribute to the NIST mission by meeting the needs of U.S. industry and the public within the division's disciplines. Technical Merit and Appropriateness of Work The Process Measurements Division continues to make a significant contribution to the promotion of U.S. economic growth by engaging in partnerships with industry; by sustaining and developing an impressive array of international standards, benchmarks, and cooperative programs; and by holding timely workshops in important technical areas. The panel sees evidence that ongoing projects and resource allocations are reviewed and that projects are brought to timely and productive completion. Examples are completion of SRM 1750, which is a calibrated capsule standard platinum resistance thermometer for 13.8 to 430 K; completion of heat transfer measurements near the critical point of carbon dioxide (CO2); suspension of a project to build a 300-mm reactor for plasma processing measurements; and successful completion of the CRDS Competence project. A new Competence project on developing an atomic standard for pressure is also appropriate. Division leadership has committed itself to strategic planning within the division by establishing and training a five-member team to begin the analysis and planning. Further evidence of continuing review of projects and resource allocation was seen in the redeployment of staff, with good matches between skills and newly assigned tasks. The Fluid Science Group was reassigned to the Process Measurements Division from the Physical and Chemical Properties Division. Fluid Science Group research competence in temperature measurement and fluid flow has significant synergy with the competencies of the Thermometry Group, the Pressure and Vacuum Group, and the Fluid Flow Group. Housing these four groups in the same division has resulted in improved collaboration among these researchers. Widespread demand for the division's calibration services in pressure, humidity, vacuum, temperature, and flow continues to be a positive index of the quality of its work. The division continues to pursue the automation of calibrations where appropriate in order to service this workload while engaging in research and development. The Thermometry, Pressure and Vacuum, and Fluid Flow Groups are leaders in conducting international standards comparisons. This is a high-priority activity within the groups, and those involved seem passionately committed to ensuring world-class accuracy and the highest-quality references for international commerce. The operational priorities of groups directly involved in standards are (1) calibration services and international comparisons, followed by (2) research and development aimed at overcoming measurement limitations in industry, and (3) advancing the state of the art. The panel finds that those involved in measurement technology and process modeling have priorities that are consonant with industrial interests and do quality modeling and measurements. Some specific illustrations and current activities are noted in the following paragraphs. The Fluid Flow Group defines key comparisons for flow in international commerce. It has completed scheduled measurements for nine international comparisons. The incorporation of corrections for vibrational relaxation in CO2 flow-through in critical nozzles used in flowmeters is a significant advance in flowmeter research. Telecalibration of gas flowmeters continues to spread as an important productivity-enhancing technique, and a report on this work garnered the best paper award at the 1999 Measurement Science Conference. Telecalibrations between Boulder and Gaithersburg continue, and industrial interest exists in providing flow calibration services over the Internet. Automation of flow testing has improved throughput for this service and allowed unattended operation with better efficiency and safety. Hydrocarbon flow calibrations are also candidates for automation, but this work would require an additional engineer and funding beyond the current level. The panel encourages the planned expansion
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 of automation to relieve labor-intensive calibrations. This improves productivity and partly compensates for a shortage of personnel. The Fluid Flow Group continues to make strong contributions to process measurements of fluid flows. The new leader of the Fluid Flow Group was promoted from within the group after the former leader filled the newly created position of deputy chief of the Process Measurements Division. The transition appears to have been seamless, and the deputy chief is still active in fluid flow standards as chair of the new international Working Group for Flow in the Consultative Committee for Mass and Related Quantities. The group leader provides leadership for the Working Group for Flow in the Sistemo Interamericano Metrologia (Interamerican System for Metrology, or SIM). The panel appreciates the vision, focus, and enthusiasm of group staff and applauds the fact that 45 percent of the staff in this group are currently enrolled in degree-granting institutions to further their education. A Competence award for the new Microanalytical Laboratory project was won by the Process Sensing Group, and a new staff member was added to the group to reinforce microhotplate sensor self-assembling monolayer (SAM) biosensor efforts. The panel is pleased with this development. Microfluidics, an essential technology for developing the microscale analytical laboratory, is being developed in an internal collaboration with Analytical Chemistry Division and Electronics and Electrical Engineering Laboratory experts in structure fabrication. The group's extensive collaborations with universities, the Department of Energy, and industry provide fabrication capabilities and accelerate these projects on many fronts. Basic surface science studies are also helping to advance NIST's own ability to create more specific, accurate, and precise microsensors. Microstructure technology (MST) is an emerging field that is beginning to show exponential growth and is expected to have effects on the national infrastructure—perhaps equal to or greater than those of the integrated circuit (IC). Even at this early stage, advances in gas sensing are progressing because of the availability of better microhotplates and the incorporation of various metal oxides as sensor surfaces. There are many collaborations with industrial research and development facilities and universities. Such work is vital to the NIST mission because it will dramatically benefit the whole U.S. infrastructure of biotechnology, pharmaceutical, and chemical industries. Another process-sensing project addresses monitoring of ion currents in plasma etching and plasma chamber cleaning systems. Noninvasive current and voltage measurement studies were initiated this year in collaboration with the plasma processing tool manufacturers Fusion and Novellus. NIST is also studying the use of laser-induced fluorescence measurements to profile plasma densities in the high-density, inductively coupled plasmas commonly used for IC manufacture. Developing these technologies and disseminating them in the semiconductor industry is an appropriate activity that builds on the group's research. The Thermometry Group continues to provide important services and technology to the U.S. chemical process industries. Extensive effort in fiscal year 1999 was directed at international comparisons of temperature standards and scale realizations. NIST coordinated the exchange of artifacts and data reports for two of four key comparisons. Similarly, Thermometry Group staff were actively involved in developing an international standard for humidity. NIST solicits participation and encourages leadership in these comparisons; however, there is a shortfall in the budget to build and characterize artifacts. Temperature calibration services for industry enjoy a steady workload with turn-around times that are reasonable and accepted by customers. The group's project to instrument silicon wafers for rapid thermal anneal temperature profiling, along with the accompanying radiometry measurements, reflects appropriate involvement and interchange with semiconductor equipment suppliers, support industries, and end users. Other important areas of research under way on new fundamental approaches to thermometry and humidity include acoustic thermometry (with the Fluid Science Group), noise thermometry (where
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 may have industrial impact far beyond refrigeration applications since its results are pertinent to lubricant-surface interactions at any frictional contact. The Membrane Science and Technology project concerns research on membrane characterization techniques and provides fundamental data and models needed to design and/or select more efficient and robust materials for membrane-based separations. A unique attenuated total reflectance Fourier transform infrared spectroscopy technique has been developed and implemented to measure solubility and diffusion rates of multicomponent mixtures in commercial membranes using unique adhesion methods. Membranes are widely used in industrial and environmental applications, such as water purification, separation of gases, and purification of chemicals. This research fills a critical need for information on how separation membranes interact with chemical feedstock components, which will facilitate the design of optimal membrane separation systems. A method using field-flow fractionation and membrane characterization has been developed that provides understanding of the processes leading to plugging of membranes during water treatment. Plugging causes deterioration of the membrane, and this research will provide the critical data necessary to the design of practical membrane filtration systems having minimum degradation during use. State-of-the-art laboratory apparatus, not duplicated anywhere in the world, enables the Experimental Properties of Fluids Group to measure with high accuracy comprehensive thermophysical and transport property data on industrially important pure fluids and mixtures. These include hydrocarbons, organic and inorganic chemicals, refrigerants, and aqueous waste mixtures. Special equipment not available in industrial laboratories includes high-accuracy apparatus to measure very low vapor pressures (regulatory compliance data), critical properties, surface tension, and viscosity. This year, the Experimental Properties of Fluids Group helped issue a final report on the activities of International Energy Agency Annex 18 to establish international standards for refrigerant properties.6 Ongoing group work to facilitate the use of ozone-friendly alternative refrigerants includes the IUPAC project on halogenated organic compounds and further updates to the NIST refrigeration properties database, REFPROP. Currently, the group is also extending its measurement capability to include partially characterized systems such as lubricants and petroleum fractions. The Theory and Modeling of Fluids Group performs theoretical and computational research on the thermophysical properties of industrially important fluids and fluid mixtures and continues to provide comprehensive and evaluated Standard Reference Data and electronic databases for the properties of commercially important fluids and fluid mixtures. A new initiative on modeling of partially characterized systems of great technical significance, such as lubricants or petroleum fractions characterized only by American Petroleum Institute gravity and boiling-range data, has begun in close collaboration with laboratory work in the Experimental Properties of Fluids Group. A key milestone achieved in 1999 was the capability to input petroleum fractions into the NIST4 database on thermophysical properties of hydrocarbon mixtures, SUPERTRAPP. In addition, high-accuracy models for hydrogen-methane mixtures at high hydrogen concentration were developed for alternative fuel applications. A longer-range research program characterizes the structure and properties of gelling colloidal silica by neutron scattering and rheometry; these data are important for materials applications involving the use of complex and structured fluids. The Cryogenic Technologies Group develops improved measurement and modeling techniques for characterizing basic cryocooler components and processes and develops state-of-the-art prototype 6 M.O. McLinden and K. Watanabe, “International Collaboration on the Thermophysical Properties of Alternative Refrigerants: Results of IEA Annex 18,” 20th International Congress of Refrigeration, Sydney, Australia, September 19-24, 1999.
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 cryocoolers for specific applications under several ongoing CRADAs. It also provides measurement methods and standards for flow under cryogenic conditions and assists U.S. industry in the development of new and improved products utilizing cryogenic processes. This group provides the most direct engineering impact in the Physical and Chemical Properties Division. An example of this impact is the outstanding engineering research paper award given to group staff at the 1999 Cryogenic Engineering Conference. The development of novel cryocooler applications is facilitated by ongoing projects to improve basic cryocooler measurement and modeling techniques. This year, three joint patents were granted for cryogenic catheter treatment of heart arrhythmia and abnormal uterine bleeding. Also, the prototype pulse-tube Mars oxygen liquefier was delivered to NASA-Johnson Space Center. The panel was pleased to see new initiatives in the Cryogenic Technologies Group. These include a project to model high-frequency pulse-tube refrigerators to be used for detector cooling in remote locations at temperatures of 10 K for the National Radio Astronomy Observatory and a project to upgrade computerized data acquisition and load cell technology for the unique NIST cryogenic flow calibration facility. Although useful metrics exist within the division for assessing the level of activity and overall quality of the work (e.g., conference participation and number of invited lectures, publications, and editorships), the panel encourages division management to develop project-specific metrics. This could be done, for example, by using some of the activity metrics described above on the project level. It is important for the division to find ways of assessing the quality of completed work rather than just listing the activities completed. The panel encourages division management to develop systematic criteria and a process for the selection, periodic review, and phasing out of databases. Impact of Programs The Physical and Chemical Properties Division's groups are making a strong, well-directed effort to convey their results to the scientific and engineering communities. One example of this is the Chemistry WebBook, which is visited by between 6,000 and 12,000 users per week. A mechanism should be set up to provide for periodic review and updating of the division's Web site pages and links. During fiscal year 1999, the Physical and Chemical Properties Division published 116 papers (28 percent of CSTL output), delivered 86 talks (11 percent), and served on 103 committees (17 percent). The division works closely with industry to identify measurement and standards needs and to develop programs that will have impact. Significant evidence of the value of divisional programs is seen in industrial funding of a number of projects. The division wisely uses multiple approaches, including workshops and conferences, to maintain very close ties with industry. Examples of the division 's industrial interactions and responses to industry problems include alternative solvent characterization (with Dow and Dow-Corning); the design of mixtures to obscure IR radiation (with Bechtel Corporation); property measurement for high-pressure gas separations (with the Gas Processors Association); thermophysical property measurement and model formulation for hydrofluorocarbons (HFCs) that have zero ozone depletion potential (with DuPont, Honeywell, Elf Atochem, ICI, Solvay, and Carrier); extensions to algorithms for mass spectral searching (CRADA under development with Finnigan); and the development of cryogenic catheters for the treatment of heart arrhythmia and abnormal uterine bleeding (CryoGen). The division's databases are disseminated through NIST Technology Services. The division is well served through these interactions, although the speed of the database review process could be improved. However, a recent reduction in the level of division funding for databases from Technology Services could adversely affect division programs.
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 Division Resources Funding sources for the Physical and Chemical Properties Division are shown in Table 4.5. As of January 2000, staffing for the Physical and Chemical Properties Division included 64 full-time permanent positions, of which 53 were for technical professionals. There were also 21 nonpermanent and supplemental personnel, such as postdoctoral research associates and part-time workers. The NIST staff are split approximately equally between Gaithersburg and Boulder. The panel is concerned that the division's budget has been essentially flat over the past 5 years. This creates significant pressure to obtain additional resources and to reallocate existing resources to maximize impact. In the long run, this will necessarily have a negative impact on the quality of the division 's work. The panel is encouraged that the percentage of other agency (OA) funding has decreased from 30 percent, but the reliance on OA funding remains a problem. Division management would prefer the level of OA funds to be closer to the CSTL average of 18 percent. Although currently most externally supported projects are consistent with the division's mission, this may not always be the case. Nevertheless, competing for grants and other funds is a healthy process that ensures the division scientists and engineers remain at the forefront of their fields. Division staff in Gaithersburg are generally satisfied with the physical facilities, although some problems were noted by the panel. In some laboratories, air cleanliness, dust control, and air filtration are insufficient; the quality, capacity, and reliability of the power supply are problematic; and the exhaust and ventilation systems are inadequate. Laser-based optical studies planned for the future will require cleaner rooms and better vibration control. However, the current quality of the laboratories at Gaithersburg is generally comparable with that of facilities at research universities. In Boulder, the division's laboratory space in Building 2 is generally of adequate quality but is severely overcrowded. Laboratory space in Building 3 is totally inadequate. Problems associated with Building 3 include extremely minimal temperature control (no cooling, only ventilation); extremely poor air cleanliness, dust control, and air filtration; unreliable, low-quality, low-capacity power; poor lighting; and a leaky exterior shell. The situation is expected to improve as National Oceanic and Atmospheric Administration (NOAA) personnel vacate space in Building 1, but the additional space has TABLE 4.5 Sources of Funding for the Physical and Chemical Properties Division (in millions of dollars), FY 1997 to FY 2000 Source of Funding Fiscal Year 1997 (actual) Fiscal Year 1998 (actual) Fiscal Year 1999 (actual) Fiscal Year 2000 (estimated) NIST-STRS, excluding Competence 8.6 8.7 9.1 9.1 Competence 0.1 0.1 0.1 0.4 ATP 0.1 0.4 0.4 0.3 OA/NFG/CRADA 4.2 4.0 3.5 2.6 Other Reimbursable 0.0 0.1 0.3 0.1 Total 13.0 13.3 13.4 12.5 Full-time permanent staff (total)a 65 68 65 64 NOTE: Sources of funding are as described in the note accompanying Table 4.1. a The number of full-time permanent staff is as of January of that fiscal year.
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 yet to be turned over to the division. Activities currently housed in Building 3 must be moved to adequate facilities. A firm date for such a move should be set. These problems have a strong negative effect on the division's work. For example, efforts to measure phase equilibrium for aqueous systems have been seriously hampered by the lack of temperature control in Building 3. During the summer months, measurements in the laboratory are very inefficient because the ambient temperature may rise by as much as 20 °F during the work day. By arriving early in the morning before the steep temperature rise sets in, the research group can measure a single phase equilibrium point per work day. This dismal rate of progress makes it impossible to finish work in a timely manner. Measurements of vapor-liquid equilibrium, coexisting phase densities, and interfacial tensions are hampered by poor ventilation and noisy, surging power in Building 3. These measurements are a key part of the natural gas systems program for the Gas Processors Association. Poor laboratory ventilation has forced the temporary abandonment of measurements at temperatures greater than 340 K, which is the point at which vapor begins to escape the confines of the stirred liquid bath into the laboratory atmosphere. The escaping vapor, which has low toxicity, is an eye and respiratory irritant whose level would rise continuously due to poor lab ventilation. Until the ventilation problem is mitigated, measurements between 340 and 425 K must be postponed. In addition, a power surge recently shut down the vapor-liquid equilibrium experiment by burning out a high-capacity uninterruptible power source and the personal computer that operates the instruments. The impact would have been much worse if not for power surge protection on all the instruments. The division's activities include several collaborations with other NIST laboratories. Examples include work on fire suppression, refrigerant properties, firefighting agents, effects of lubricants on R134a pool boiling, and clay nanocomposite fire retardants (interactions with the Building and Fire Research Laboratory); research on the computational prediction of molecular electron impact ionization cross sections; methods for chemical structure prediction; long-range interactions in alkali diatomics associated with atom-atom collisions at low temperatures; and vibrational spectroscopy of reactive intermediates (interactions with the Physics Laboratory); investigations on statistical comparisons of enthalpy of adsorption data; use of the ANSYS for computational fluid dynamics, and work on the latest release of the REFPROP database program (interactions with the Information Technology Laboratory); and research on lubricant characterization, behavior of torsionally vibrating transducers; and effect of solvent quality on the dispersability of clay (interactions with the Electronics and Electrical Engineering Laboratory). The panel is not aware of any mechanisms or processes that are in place to support or encourage such interlaboratory collaborations or of any factors that inhibit their occurrence. The Next-Generation Kinetics Database is eagerly anticipated by chemical kineticists both in industry and in academia. The current database, which was developed in the Chemical Reference Data and Modeling Group and sold to individuals, has had only one update in the past 5 years and provides simply a compilation of existing data. Although this database is of great use to gas kineticists, a more efficient method is needed to keep the database current. The Next-Generation Kinetics Database provides such a mechanism. It will be Web-based and can be updated frequently. The development of the new Web database should be made to proceed as quickly and efficiently as possible. This may require additional funding to staff the project at an optimal level. The panel also urges that updates of the current database be offered to previous customers during the development of this new project if a delay of a year or more is anticipated in the first offering of the Next-Generation Database. The Computational Chemistry Group benefits from the able leadership and technical insight of the group leader, who has also been appointed deputy division chief. The panel is concerned that his double duties may lead him to step down from his group leader position in the future. Should this occur, that position must be filled to maintain sufficient staffing and leadership for the group.
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 Analytical Chemistry Division Division Mission According to division documentation, the mission of the Analytical Chemistry Division is to serve as the nation's reference laboratory for chemical measurements and standards to enhance U.S. industry 's productivity and competitiveness; ensure equity in trade; and provide quality assurance for chemical measurements used for assessing and improving public health, safety, and the environment. The division is the fundamental chemical metrology component of CSTL and NIST. Divisional programs provide measurement standards, accurate and reliable compositional data, and research in measurement science that are critical to the overall success of CSTL and NIST. The division 's programs continue to be well managed and serve the fundamental role of maintaining U.S. standards and standard methodology for analytical chemistry. The projects currently under way are well positioned relative to the mission and are critical for supporting the U.S. measurement infrastructure. The development of new measurement technologies allows the division to develop SRMs previously thought impossible while improving existing standards with faster, more accurate measurements. Nonetheless, it remains necessary for the division to maintain a balance between developing new measurement technology, supplying new SRMs, and defining the need for existing SRMs. The division continues to review research and service projects on an annual basis using a formal system to assess relevance and to prioritize programs and projects. The panel again notes that this process must be revisited continually to ensure that the projects with the greatest impact on U.S. industry are supported. Where the division has determined it cannot be the best in class, it should ensure that U.S. industry has access to best-in-class capability through strategic partnerships or other mechanisms. Technical Merit and Appropriateness of Work Overall, the technical merit of the work in the Analytical Chemistry Division continues to be outstanding. The scientific results and products (i.e., SRMs) of the division are of vital importance to U.S. industry because they directly impact the measure of trade, purity, or value to the world economy. All staff are dedicated to a quality process that drives most of their activities. Research activities in the division focus on chemical measurements made by high-performance analytical tools and techniques such as mass spectrometry, microsampling or detection technologies, state-of-the-art separation methods, classical analytical methods, gas metrology, nuclear analytical methods, organic analytical methods, and spectrochemical measurement methods. These programs are carried out within five groups: the Spectrochemical Methods Group, the Organic Analytical Methods Group, the Gas Metrology and Classical Methods Group, the Molecular Spectrometry and Microfluidic Methods Group, and the Nuclear Methods Group. The Spectrochemical Methods Group focuses on the development, critical evaluation, and application of methods for the identification and measurement of inorganic chemical species using x-ray, optical, and mass spectrometry. This group continues to expand the application of high-performance, inductively coupled plasma-optical emission spectrometry (HP-ICP-OES) methodology. HP-ICP-OES is capable of fulfilling industry's need for faster, highly accurate techniques for elemental analysis. The HP-ICP-OES approach has matured from spectrometric solution certification to the capability to solve real-world applications involving complex matrices. The division's efforts to promote the use of this technology are most appropriate. The group assumed responsibility for the related spectrometric solu-
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 tion SRM Program. It reengineered the production systems for these SRMs to achieve improved accuracy, focusing on providing traceability standards to support a planned NTRM Program. The development of such a program is progressing. Increased emphasis on NTRM Program implementation will enable the spectrochemical group to expand its efforts in the development of new SRMs. Also within the Spectrochemical Methods Group, the X-Ray Fluorescence project has progressed significantly. The amount of SRM work done by this group includes the certification of three cement SRMs that support an important segment of the U.S. construction industry. The group has also developed a lubricant SRM. The group recently installed its fifth ICP-mass spectrometer in its facility at the new Marine Environment Health Research Laboratory in Charleston, South Carolina. This laboratory is a cooperative effort between NIST, NOAA, the South Carolina Department of Natural Resources, and the University of Charleston. A NIST researcher has also relocated to work full-time at this facility. This new endeavor will benefit greatly from the on-site presence of additional NIST inorganic analysis expertise, and the collaboration offers the division additional stimulus for the development of useful new techniques and analytical methods. The Organic Analytical Methods Group develops a variety of methods and standards to characterize organic molecules in the many types of matrices in which they are found. These matrices include environmental, clinical, and food samples. For example, new stationary phases developed by the group for liquid chromatography (LC) provide shape-selective separations to distinguish among closely related environmental pollutants. Solid-phase extraction is employed in conjunction with LC and GC for pesticide analysis at low concentrations. A micronutrient measurement quality assurance program was developed to standardize the vitamin and carotenoid content of biological fluids. The feasibility of using chiral compounds extracted from hair as markers for drug use is being evaluated. For potential clinical applications, effort continues in mass spectrometry to assay troponin I for heart disease diagnosis. These are just a few of the group's ongoing efforts. One particularly noteworthy program uses the unique advantages of isotope-depleted protein standards for calibration of mass spectrometers. Calibration of mass spectrometers used for high-molecular-weight species is relatively difficult. The Organic Analytical Methods Group is developing calibration standards consisting of proteins produced by bacteria grown in 13C- and 18O-depleted conditions. These proteins will have simple isotope clusters and should be useful for calibrations in MALDI and electrospray mass spectrometry of biomolecules. The Gas Metrology and Classical Methods Group leads NIST and the global standards-setting community in identification of the need for, and development and distribution of, SRMs and NTRMs. The current programs are in direct line with the objectives of NIST and goals of the sponsoring agencies. In fiscal year 1999, 170 gas SRMs were recertified for 15 corporations and 66 NTRM batches were certified for 7 specialty gas vendors. The Gas NTRM Program has set the basis for production of more than 400,000 NIST traceable standards. To maintain this technology lead, the group is active in gas metrology, classical wet chemical methods such as gravimetry and titrimetry, coulometry, ion chromatography, and spectroscopy (IR, ultraviolet (UV), visible, Raman) and has primary responsibility for maintenance of the theoretical infrastructure for pH and conductivity measurements. The Gas Metrology and Classical Methods Group's standards serve one of the broadest commercial markets in the world, the $19 billion specialty and bulk gas producers. Such gas- and liquid-phase standards are second only to the gram in their impact on U.S. regulatory and international trade agreements. The most significant of these are standards for environmental control (e.g., EPA protocol gases) and standards to assess product purity, which impact food and drug manufacture and trade. During
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 fiscal year 1999, the group completed the implementation of an infrared database (NIST SRD 79). Available on the Web and on CD-ROM, this database allows direct, consistent, and cost-effective calibration of instruments for quantification of EPA hazardous air pollutants. In fiscal year 1999, group leadership also developed a plan to work more directly with specialty gas producers in the manufacture and certification of NTRMs in order to eliminate shortages of critical gas standards. Another project to develop low-concentration nitric oxide gas standards for the next generation of automotive emission regulations will encompass an international effort with the Netherlands and the United Kingdom. This is an outstanding example of the kind of cooperative work needed by the group and NIST to leverage its resources to meet the needs of U.S. manufacturers in the global marketplace. The Molecular Spectrometry and Microfluidic Methods Group has a focus that is both appropriate and timely as the use of microanalysis becomes more widespread. This group's efforts in SRMs include optical filter SRMs for spectrometric calibration and SRMs to provide near-IR wavelength and absorbance standards, where substantially higher accuracies have been enabled by a new approach to spectral fitting. In addition, a new UV solution standard SRM is being developed in response to requests from users. Two efforts of particular note are fluorescence standards for flow cytometry and capillary electrophoresis analysis of single-residue particles of gunpowder for forensic applications. The division sponsored a workshop to examine candidate materials for fluorescence standards for luminescence spectrometry. Attendance included representatives from five NMIs that examined more than 60 candidate materials. In collaboration with the Biotechnology Division, the Molecular Spectroscopy and Microfluidic Methods Group is developing a fluorescein solution SRM to be used to characterize the moles of equivalent soluble fluorophore scale used in flow cytometry. Through the NIST Office of Law Enforcement Standards, the group is also developing a quantitative extraction and analysis method for the recovery of gunpowder additives from physical evidence. This will allow comparison of residue to unfired gunpowder for purposes of identification. The group is also working on an SRM for additives in smokeless gunpowder. A relatively new direction in the group is the study of microfluidics, the result of a successful NIST Competence award proposal. This program aims to develop methods for monitoring and characterizing microchannels and microfluid flows on integrated chips. The group's fabrication of unique reaction and mixing regions in the chip can lead to future standardization of such microscale measurements. This effort is timely and has good potential for future impact, and the panel encourages such efforts. The Analytical Chemistry Division should try to identify at least one such additional new core competency area in 2000. The Nuclear Analytical Methods Group continues to provide a comprehensive array of nuclear analytical techniques supporting a variety of U.S. industries and other government agencies. The techniques include neutron activation analysis, prompt gamma activation analysis, and neutron depth profiling. They complement the Spectrochemical Methods Group by providing a powerful alternative reference technique for SRM development as well as the ability to make measurements where sensitivity and sample dissolution issues arise in other methods. Continued research into neutron focusing technology will push the technique to even better sensitivity and will enhance spatial resolution. The NIST Center for Neutron Research is arguably the best facility in the world for many areas of neutron production and use, and it supports cutting-edge research by NIST and guest researchers. The group was very active in collaborative research and organized the Tenth International Conference on Modern Trends in Activation Analysis. This meeting brings together researchers from around the world to assess nuclear analytical techniques and their applications. Hosting this conference at NIST further enhances NIST's reputation in the international scientific community.
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 Impact of Programs By far the most easily quantifiable of the Analytical Chemistry Division 's impacts on industry is seen in its development and dissemination of SRMs and NTRMs. NIST provides nearly 1,400 different types of SRMs and in fiscal year 1999 sold 33,000 SRM units to approximately 6,650 separate customers. Roughly 18,000 of these units were from the 850 different types of materials certified for chemical composition by the Analytical Chemistry Division. In addition, the division certified 66 batches of NTRMs for specialty gas companies. The combined number of types of SRM and NTRMs available from the division has increased from 216 to 308; the number of SRMs this year nearly doubled. Currently, each technical group within the division manages its respective SRM and NTRM standards programs and spends valuable resources that are not fully recovered from the sales of the reference materials. Recertification of optical filters and cylinder gas standards also remains a significant activity. The panel was encouraged by the division's success in reducing SRM backlog, increasing the ratio of new SRMs to restocked SRMs produced, and developing a new quality classification document for its SRM value assignment process. The panel recognizes the NTRM program as critical to a broad base of global industries. As noted in the fiscal year 1999 report, changes are still needed in the current work process to develop and provide SRM certification and NTRM products to a world market. The technical teams, especially group leadership, should carefully consider better balancing each team's scientific roles and increasing the management of commercial producers to better prepare, certify, and maintain inventory of NTRMs. The more effective use and monthly review of agreed-upon business metrics tied to technical performance metrics in program planning and execution should be considered. By these means, the panel believes, technical group leaders could reduce the time of SRM development and NTRM implementation by 25 percent. The division's industrial interactions are substantial. The division entered five CRADA agreements in 1999, the same number as in 1998. Although such formal agreements are useful, the panel supports the division's approach of also promoting informal partnerships with industry. For example, the division has made progress in establishing NTRM ties with several manufacturers of optical filters. It served as a pilot laboratory for 10 strategic international comparisons conducted under the auspices of BIPM and SIM and organized a Raman wavelength intercomparison in collaboration with ASTM and a gunpowder analysis round-robin for the Department of Justice. It formed collaborations with industrial companies in microfluidic devices. Partnering was also initiated with the Electronics and Electrical Engineering Laboratory and with the Biotechnology Division. The division's publication record is excellent and makes strong contributions to the peer-reviewed literature. Publications and presentations increased to 366 in 1999, up 40 percent from 1998. The project on international comparability of chemical measurements provides worldwide leadership in the development of SRMs, NTRMs, proficiency testing programs, and international intercomparisons. The panel is particularly pleased by this division's international work, since intercomparisons become more vital as trade becomes more global. Staff scientists and leadership in the division should put more effort into publicizing their work based on its impact on commercial markets and on sponsoring agencies. This effort can begin at the program-planning phase with the definition and quantification of business and technology metrics. Selected commercial public relations presentations, papers, and meetings may well enhance the group's ability to compete successfully for future funding. One prime example of the positive impact of participation in international activities occurred in the area of pH measurements. Division participation in IUPAC activities ensured the acceptance of a convention maintaining pH traceability based on thermodynamic principles and defining recommended
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 values of uncertainty in measurement. NIST's 3-year effort to defend the established scale from the simplified but nontraceable scale proposed by some IUPAC participants saved U.S. industry the cost of converting its measurements to a new scale. NIST has a goal of playing a leadership role in intercomparability programs among national and regional standards laboratories to facilitate international trade. The division's activities remain the basis for formal establishment of equivalence among primary methods and standards important for global commerce. The panel applauds the division's leadership in this area. However, although the division is well situated in the international reference material community, it lacks a coordinated effort that could have an impact on international measurement science. The division should focus more on international application-based groups to get a better understanding of emerging standards and measurement issues. The international application groups adopt many of the standards from the ISO, ASTM, and others, but the selection and evaluation of standards are outside the realm of expertise of current U.S. delegations. The division is encouraged to prioritize and consolidate current activities to accommodate such activities. The division should evaluate its participation in all international committees and refocus efforts to maximize impact. Many of the international activities are unfunded, squeezing the division's tight resources. Special funding for participation in these activities should be available if NIST is truly committed to leadership on intercomparability of measurements and to maintaining the competitiveness of U.S. industries abroad. Division Resources Funding sources for the Analytical Chemistry Division are shown in Table 4.6. As of January 2000, staffing for the Analytical Chemistry Division included 68 full-time permanent positions, of which 62 were for technical professionals. There were also 33 nonpermanent and supplemental personnel, such as postdoctoral research associates and part-time workers. The involvement of students and postdoctoral associates in the Analytical Chemistry Division is beneficial to achieving the goal of developing novel technologies and broadening public outreach. TABLE 4.6 Sources of Funding for the Analytical Chemistry Division (in millions of dollars), FY 1997 to FY 2000 Source of Funding Fiscal Year 1997 (actual) Fiscal Year 1998 (actual) Fiscal Year 1999 (actual) Fiscal Year 2000 (estimated) NIST-STRS, excluding Competence 7.3 8.1 8.5 7.2 Competence 0.0 0.0 0.3 0.3 ATP 0.2 0.0 0.1 0.2 Measurement Services (SRM production) 2.1 2.2 2.2 3.1 OA/NFG/CRADA 1.9 2.2 2.0 1.9 Other Reimbursable 1.1 1.4 1.5 1.5 Total 12.5 13.9 14.6 14.2 Full-time permanent staff (total)a 68 67 66 68 NOTE: Sources of funding are as described in the note accompanying Table 4.1. a The number of full-time permanent staff is as of January of that fiscal year.
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 Other-agency funding continues to shrink compared with the total budget. The reduced reliance on OA funding allows independence in the division's implementation of strategic measurement science research programs. The panel encourages the division to maintain this independence; however, the division needs to seek specific funding that supports its research programs. The current division technical staff make a responsive team fully capable of addressing the development and implementation of new measurement standards to serve the ever-changing world economy in emerging areas such as pharmaceuticals, foodstuffs, and microelectronic fabrication. Peer recognition of staff scientists is high from both within and outside NIST. In today's highly commercial environment, technical success must be tied to and directly quantified in terms of its impact on the cost of a process, product, or market. An active part of each program's plan must be justified at the start with business and technical metrics. The end result of any new SRM, NTRM, or measurement technology should be an ongoing quantifiable return to the commercial stakeholders. Such impact arguments need to be developed by researchers and widely publicized by division and CSTL leadership to best gain recognition from funding sources. NIST management should also recognize that the demand for new SRMs and advanced technologies will continue to increase as materials, biotechnology, and semiconductor industries grow. These complex samples require an increase in effort in the Analytical Chemistry Division that can come only with increased funding. The Analytical Chemistry Division moved into new facilities in the Advanced Chemical Sciences Laboratory (ACSL) in 1999. The quality of the new space is excellent. For example, the reduction of background in ICP-MS because of the clean room will allow the development of low-concentration SRMs that are critical to the semiconductor industry. Division management is encouraged to continue to maintain its 5-year capital plan to adequately address future needs and analytical capabilities. The panel is pleased to note that there was a smooth transition to the new space with very little disruption of ongoing activities. By bringing related efforts within close proximity to one another, work efficiency has been increased. Interactions among the scientists have also been enhanced. The relocation of most of the Biotechnology Division to the new ACSL should facilitate interdisciplinary efforts with analytical chemistry that will be vital to the generation of future SRMs. MAJOR OBSERVATIONS The panel presents the following major observations: The technical merit of the work in the Chemical Science and Technology Laboratory continues to be of a very high level and quality. The panel particularly observes enthusiastic staff and the outstanding leadership provided by the laboratory director. The panel is pleased with the receptiveness and responsiveness of CSTL to prior panel reports. International interactions are critical to the global economy. Within CSTL, two projects with major international impact deserve highlighting: work in the refrigeration working group and uranium swipe tests for international security. An increasing demand for resources to support the critical interactions in international horizontal intercomparability and standardization is beginning to impact other programs, and the panel recommends that this work be funded centrally rather than from the CSTL program budget. Extensive evidence of successful collaborative research was noted. An internal NIST Web site listing staff expertise appears to be an excellent tool to facilitate collaborations across NIST laboratories.
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An Assessment of the NATIONAL INSTITUTE OF STANDARDS AND TECHNOLOGY MEASUREMENT AND STANDARDS LABORATORIES: Fiscal Year 2000 The panel finds the work in CSTL to be highly relevant industrially. Metrics should include project-oriented interactions as well as workshops. Appropriate metrics will vary with the maturity of a particular program. Facility inadequacies, which prevent some state-of-the-art measurement work, are being addressed as funding permits. However, continuous improvement of facilities is needed to ensure that current and future work can be accomplished. A plan for renovation and for meeting facilities needs during the building of the Advanced Measurement Laboratory is still necessary to address major problems, especially in Building 3 in Boulder. The new space in ACSL is an excellent tool that has improved productivity. The panel is pleased to see that CSTL leadership continues to improve administration and management of the NTRM Program and urges that these efforts continue. Progress in CSTL's utilization of the Internet since last year is applauded. The NIST Web presence, however, needs an overall design and strategy with a customer focus. This is a major method of customer interaction and requires high-level attention. The panel notes that the biotechnology industry is working on a time line different from that of other industries serviced by CSTL. The panel recommends that NIST develop a cohesive strategy in biotechnology that addresses the rapid pace of change in this important industry.
Representative terms from entire chapter: