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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

4

Chemical Science and Technology Laboratory

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

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.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

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.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

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

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

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>.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

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

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

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.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

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

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

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.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

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

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

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

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

a measurement method would replace an artifact), and low-concentration water vapor standards. The Thermometry Group leader was expected to retire in March 2000; the division designated a successor from within the group who started to assume these duties in good time and provide continuity.

The Pressure and Vacuum Group continues to provide pressure gauge calibrations from high vacuum to very high pressure to U.S. industries. This same group also provides flowmeter calibrations. The high quality of the NIST calibrations is attested to by the low uncertainties noted during international standards comparisons. This year the group participated in six International Committee for Weights and Measures key comparisons and 2 SIM comparisons, in addition to national round-robin standards exchanges with U.S. secondary calibration standards laboratories. Many staff are involved with directing these comparisons, and the group staff serve on national technical committees in their field.

The Pressure and Vacuum Group has also been proactive in the development of new standards and techniques. One fine example is the development of a low-drag spinning rotor gauge to extend quality vacuum measurements to pressures lower by at least an order of magnitude. A new leak-into-atmosphere standard is under development, and work on measurement of gaseous impurities by CRDS is progressing. Efforts to support the semiconductor industry continue with real-time residual gas analyzer measurements of the effluent from tungsten deposition processes in a chemical vapor deposition (CVD) reactor at the University of Maryland. Additional measurements are planned with CRDS interfaced to the reactor. At the time of the panel's visit, a workshop was planned for May 2000 as part of an important initiative to interface with the mass flow controller industry. NIST personnel planned to discuss issues in linear flow elements, calibration methods, and new thermophysical property-based models for improving the calibration of flowmeters for reactive and hazardous gases. The panel encourages such workshops as a forum to define broad industrial issues for strategic planning and looks forward to hearing the results of this workshop at its next meeting.

The Thermal and Reactive Processes Group has completed a first version of the Benchmark for Database Multiphase Combustion Models. This database was released to 200 industrial and academic collaborators for use in validating multiphase combustion models. The database contains statistically evaluated combustion parameters from the NIST combustion facility that are needed for testing model variability. Thirty-four modelers from chemical, power, and energy industries and software developers attended a workshop to review the data, express their needs for further assistance, and define goals for future measurements. The panel encourages the planned follow-up solicitation of additional needs from workshop and Internet respondents. NIST should continue to cultivate partnerships in combustion measurement. A related effort to provide benchmark data for fire models should attract postdoctoral research associates and thus partially relieve a staffing shortage.

The group successfully identified three stable glass compositions that have now been qualified as candidate laser Raman fluorescence standards. The group will direct a round-robin intercomparison of these artifacts with instrument manufacturers and academic members of the American Society for Testing and Materials (ASTM) E13.08.

Efforts continue to develop models for microcontamination in CVD semiconductor manufacturing processes. Preliminary experiments with a rotating-disk CVD reactor show qualitative evidence for thin layers of aerosol particles, in accord with a numerical transport model developed in the division. Some results were published, and further work on aerosol measurements is planned. Particulate and aerosol contamination during CVD and plasma-etch processing are well-known issues that have been studied for many years. Formation of unwanted particulate depends on many variables, such as deposition chemistry, reactor design, and processing conditions. Although the division 's current work has some relevance, the panel encourages it to develop a concrete strategy to directly benefit mainline equipment manufacturers or to improve process chemistries for CVD reactor users.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

The transfer of the Fluid Science Group to the Process Measurements Division is logical. The expertise of the Fluid Science Group is complementary to that of the other groups in the division, and its presence should enhance collaborations. Advances in acoustic resonator thermometry will be facilitated by closer ties to the Fluid Science Group, and the Pressure Vacuum Group's metering work should help coordinate the thermophysical properties measurements of semiconductor and other industrial process gases within the Fluid Science Group.

A new Competence project to develop a pressure standard (0.5 to 5 MPa) based on the dielectric constant of helium (He) shows promise. If the methodology and techniques can be developed into a robust practical standard, an electrical measurement would replace dead weight pressure standards with a reference based on fundamental physical parameters rather than mass, piston area, and gravity. Better values for physical properties will allow manufacturers of many types of equipment, especially flow-meters, to improve calibrations involving both actual and surrogate gases.

Impact of Programs

The Process Measurement Division's strong program in standards and calibration services for pressure, temperature, flow rate, and humidity provides a needed service to industry. The division actively researches new methods and realizations of the standards to advance the accuracy and usability of the standards for international commerce. Additionally, groups actively develop partnerships or collaborations with industry through publications, workshops, their Web sites, direct agreements, and technical discussions, as described elsewhere in this report. The panel views as very good the collective efforts of the division to disseminate information and collaborate with industry. The panel supports the plans for a workshop on mass flow controllers and meetings with industrial collaborators and encourages all researchers to maintain dialogue with industry as a way to assess key areas for NIST involvement.

Division Resources

Funding sources for the Process Measurements Division are shown in Table 4.3. As of January 2000, staffing for the Process Measurements Division included 57 full-time permanent positions, of

TABLE 4.3 Sources of Funding for the Process Measurements 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

8.0

8.1

7.9

8.6

Competence

0.9

0.6

0.8

0.5

ATP

0.2

0.3

0.4

0.3

Measurement Services (SRM production)

0.1

0.1

0.0

0.0

OA/NFG/CRADA

0.3

0.4

0.8

1.0

Other Reimbursable

1.2

1.2

1.2

1.2

Total

10.7

10.7

11.1

11.6

Full-time permanent staff (total)a

65

59

59

57

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.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

which 50 were for technical professionals. There were also 14 nonpermanent and supplemental personnel, such as postdoctoral research associates and part-time workers.

The Process Measurement Division has encouraged and established cross-group and cross-divisional collaborations within CSTL and NIST and with industry, other government agencies, and academia. There are many examples of staff moving between groups in response to specific projects or by redeployment as projects are completed. An excellent example of collaborative work between groups is the continuing development of CRDS. From its beginnings as a water vapor measurement Competence project in the Pressure and Vacuum Group, CRDS is now being incorporated for validation in the low-concentration water vapor standard. The Thermometry Group took this technology and miniaturized it to create a CRDS optical cavity that can detect and quantify small amounts of materials in contact with or absorbed on a surface. Researchers are now exploring its potential as a miniature detector for the Process Sensor Group's new lab-on-a-chip. Extension of CRDS to semiconductor process monitoring collaborations at the University of Maryland explores yet another use of this technology. The Microscale Analytical Laboratory project is a cross-divisional and cross-laboratory effort involving the Chemical Science and Technology Laboratory, the Manufacturing Engineering Laboratory, and the Electronics and Electrical Engineering Laboratory. Another example of cooperative work is the development of laser Raman fluorescence standards by staff from three CSTL divisions with extensive outside collaboration.

Most groups are concerned that vacancies left by retiring researchers and term postdoctoral research associates have become difficult to fill. A major factor appears to be intense competition from high-technology industry and attractive salaries in the current full-employment economy. The panel believes that these issues and their potential solutions should be evaluated promptly to avoid a potentially serious problem in the near future.

The general-purpose laboratory equipment available to the Process Measurement Division is comparable to that in industrial laboratories, but the specialized equipment is significantly better in most areas. However, specific needs—some urgent—do exist.

In the area of process sensor development there is need for a small-scale, state-of-the-art rapid nanostructure fabrication facility. This is necessary core infrastructure to support and advance MST technology for biochips, chemical and SAM sensor development, new microchannel flow and optical measurement techniques, and more. The panel sees this facility as the 21st-century “semiconductor-MEMS (microelectromechanical systems) machine shop” that will enable the development of prototype structures.

The panel sees the problem of aging facilities as an important matter that should be addressed even before the AML is completed. Systematic renovation of the existing physical plant should be integral to maintaining a productive work environment. In the Fluid Flow Building, a center where flow measurement techniques are developed and shared with visitors, there are many failed lightbulbs, leaky faucets, and a dysfunctional hot-water loop. The interior has reportedly not been painted since 1967. In other buildings, makeshift filtering of the air supply in laboratories and secondary enclosures reflects researchers' attempts to protect experiments and to continue working. More difficult problems also exist with too-frequent power outages. The panel is aware that these problems have been investigated and a long-term remediation of ducting and air supply is planned; however, the panel shares staff concerns that nearer-term solutions are sorely needed. The panel is pleased that $300,000 worth of equipment is being installed to restore temperature control to the pressure standards calibration laboratory, which requires ±0.2 °C room temperature control for calibrations to be within specification. Temperature excursions as high as ±1.5 °C occur, disqualifying calibrations and requiring their restart. The direct cost of such failures cannot and should not be recovered from fees. Lost-time delays extended a 3-day

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

calibration into 1 month, and a key comparison study that was allotted 2 months took 3 months to complete due to the unpredictable temperature excursions. The panel recommends that CSTL record air and power failure occurrences and duration, measure deviations from acceptable conditions, and estimate the financial impact to aid in prioritizing remediation.

An equipment accident on the large-flow (16-inch diameter) water flow calibrator has halted all large-flow flowmeter calibrations in the United States. Three customers had already been turned away at the time of the panel's visit. Currently, only $100,000 of the estimated $250,000 cost of restoration and repair is available. Other calibration equipment is too small (8-inch diameter) for these calibrations; thus, rebuilding the damaged facility is urgent.

Surface and Microanalysis Science Division
Division Mission

According to division documentation, the mission of the Surface and Microanalysis Science Division is to promote U.S. economic growth, safety, health, and environmental quality by working with industry, other government agencies, and standards organizations to develop and apply key technologies, measurements, and standards for spatially and temporally resolved chemical characterization.

Because it is very general, the mission statement of the Surface and Microanalysis Science Division is not inconsistent with the CSTL and NIST missions. However, it has lost useful specificity that was present in previous versions. All chemical measurements are in some way spatially and temporally resolved. The unique capabilities of this division are in developing and applying new technologies with nanoscale resolution and compositional sensitivity. Also, the panel believes that the importance of the division's work to support national and international security should be mentioned more directly in the mission or vision statements—safety is not the same as security.

The division plans its activities using the CSTL evaluation criteria, evaluating each project for industrial need, match to division and CSTL missions, ability to make a difference in the field, nature and size of impact, and timeliness and quality of work. The panel believes that the Surface and Microanalysis Science Division does a very effective job of assessing and modifying its projects to match rapidly changing needs. It has used the CSTL reprogramming process to provide an orderly end to projects and the rapid initiation of new work. For example, work was stopped in developing isotopics for industrial use and zeolite characterization to allow new work to begin in combinatorial methods, airborne particles less than 2.5 µm in diameter (PM2.5), and polymer characterization.

The division also uses a variety of formal and informal external roadmaps (such as the ITRS and Technology Vision 20204) and interactions (e.g., with SEMATECH, ASTM, the North American Research Strategy for Tropospheric Ozone, the Environmental Protection Agency (EPA), the Air Force Technical Applications Center, and IAEA) to ensure that its mission and work are focused on the most important needs of its industrial and government customers. The panel recognizes in particular the effort that the division has made over the last year to strengthen the Atmospheric Chemistry Group and encourages growth in its interactions with the EPA.

As in past years, the panel notes that division projects would benefit from specific, measurable goals or a roadmap of technical development. The panel acknowledges that it is difficult to assign time lines to long-term research. However, long-term research can benefit from the organization and forward

4  

American Chemical Society, Technology Vision 2020: The U.S. Chemical Industry, American Chemical Society, Washington, D.C., 1996.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

thinking provided by a time line and technical roadmap with quantitative milestones. Also, a significant portion of the division's work is of shorter and therefore measurable duration. The panel encourages the division to continue to tie quantitative goals to staff development plans.

Technical Merit and Appropriateness of Work

The Surface and Microanalysis Science Division continues to perform world-class research on the spatial and temporal distribution of chemical species in a wide variety of heterogeneous systems. The division remains the foremost national laboratory in the world in surface and microanalysis. The Surface and Microanalysis Science Division's work is divided among four groups: Analytical Microscopy, Atmospheric Chemistry, Microanalysis Research, and Surface Dynamical Processes, which conduct research in seven programs. In addition to these four groups, the division also has three very active NIST Fellows. This section discusses highlights and issues relating to the programs under way in these groups.

The Surface Dynamical Processes Group conducts state-of-the-art research in surface physics and chemistry. The focus of the work has shifted over the past several years from gas-surface dynamics to the development of nondestructive optical probes for imaging and chemical analysis of nanoscale structures. The panel believes that this change in emphasis is appropriate because it better meets emerging technological needs of U.S. industry and draws clearly on the available scientific talents. Complementary efforts will benefit catalysis, semiconductor, and biotechnology research and development.

The panel endorses the group's work to develop high-throughput screening and analysis for combinatorial chemistry, in particular the development of Raman and infrared (IR) imaging techniques. This is a potentially powerful new approach for which the group's expertise is perhaps unique. The advantage of this approach is that it will provide molecular characterization of species without requiring fluorescent tags. The initial project, the development of a microwave technique for the measurement of dielectric constants (k) of new high-k materials, is especially novel and potentially very important to the semiconductor industry. This is a collaboration with the members of the Analytical Microscopy Group, whose expertise in Raman and IR will benefit these projects. The Surface Dynamical Processes Group's effort to develop sum-frequency generation (SFG) techniques pushes the leading edge of interface characterization. Applications range from understanding the chemical mechanisms and issues of copper electroplating to studying biomimetic interfaces that model living cells. The panel is less certain about the role of the group's work on theoretical aspects of dynamics and condensed matter physics. The panel recommends that the theoretical effort be redirected to better support the current experimental work of the group.

The Analytical Microscopy Group performs cutting-edge work on ion and photon microprobe analysis. It continues to be an internationally recognized leader in the development and application of advanced ion beam analytical methods, most importantly, secondary ion mass spectrometry (SIMS). The group has an impressive array of instrumentation to support its mission. In addition to activities in all variations of SIMS (dynamic, static, and time of flight), the Analytical Microscopy Group has active projects in the development of Raman spectroscopy standards and in the advanced application of Raman spectroscopy, x-ray diffraction, and laser microprobe mass spectrometry to particle and thin film characterization. The panel encourages the group to continue work on development of reference materials for SIMS to support new implant species in the semiconductor industry. The panel notes that the SEMATECH laboratory managers' council recently cited a need for standards to verify and calibrate analysis techniques applied to chemical identification of particle contaminants. Further, the panel

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

encourages the group to continue work on laser microprobe mass analysis, for the benefit of combustion product identification. Recently, the Analytical Microscopy Group has performed interesting work in the characterization of diesel soot.

It is important to highlight the work of the Analytical Microscopy Group in support of international nuclear security. The group's scientists are the leading international authorities in methods to characterize International Atomic Energy Agency swipe samples. They have used their expertise in isotopic analysis by SIMS to develop procedures that improve the detectability and reliability of screening measurements for enriched uranium. These are critical measurements for the verification of compliance with the Nuclear Non-proliferation Treaty. Analytical Microscopy Group scientists have performed onsite consulting and training at international laboratories and have had a major impact on improving international safety and security.

In addition to applying state-of-the-art methods, the Analytical Microscopy Group has projects to advance the state of the art in instrumentation. Work to understand and control depth resolution in SIMS by researching cluster ion sources will advance analytical capabilities for a wide variety of industrial applications. The use of C1− to C8− primary ions, alone and with cesium (Cs), will allow high-depth-resolution profiling of implants in silicon (Si) and III-V substrates used in the semiconductor industry and will enable much finer discrimination between surface and near-surface regions of organic polymer films. In partnership with Peabody Scientific, the group expects to develop these sources for commercial application, as it did with its earlier sulfur hexafluoride (SF6) source. These sources are designed for use with today's ion beam instrumentation, so the large base of currently installed equipment in industry can benefit from the new technology.

The work of the Atmospheric Chemistry Group focuses on advanced isotope metrology and chemical measurement processes needed to develop and enforce U.S. environmental policy. U.S. policy is implemented through National Ambient Air Quality Standards and emission restrictions aimed at achievement of these standards. Key to this approach is the ability to measure markers of ambient air quality and associated emissions, and it is here that NIST contributes. The most confounding aspect of particulate matter is carbonaceous material, which results from airborne transformations of emissions from multiple sources. The Atmospheric Chemistry Group has developed a unique capability to specify the biogenic or fossil origin of carbon emissions, a critical key to deciphering emission sources. It is extending this capability by developing techniques for isotopic profiling of organic and elemental fractions using microanalysis of particles, multi-isotopic speciation via gas chromatography (GC) and accelerator mass spectrometry (MS), and compound-specific infrared and mass spectrometry. Isotopic profiling of organic and elemental fractions, used in conjunction with other trace analyses, offers the potential to add another analysis to distinguish sources of fossil fuel emission, such as differentiating between emissions from the transportation and the power-generation sectors. The panel is concerned that the group is undersized to handle the scope of this research. Because its unique expertise is complementary to the broad spectrum of atmospheric aerosol measurements, to have significant impact the group must collaborate with the existing community of atmospheric scientists.

The Atmospheric Chemistry Group has also identified and created needed reference materials to provide traceability for environmental measurements. Its new isotopic CO2 reference materials provide for calibrations that are free of the confounding effects of preparing samples from carbonate reference standards. The Urban Dust SRM provides a much-needed calibration reference for ambient PM2.5 measurements of organic and elemental carbonaceous fractions and inorganics. The panel is concerned that the relatively small quantity of standard dust that was collected to produce this SRM will not meet the long-term needs of NIST customers and recommends continued planning for additional collections. Finally, the standardization of the thermal-optical-kinetic technique and its application to a Greenland

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

aerosol sample provide a much-needed standardization of that measurement technique for low-level black carbon. The group's proposals to the EPA for development of additional particulate reference materials are on target. Indeed, collaboration with EPA on the development of measurement techniques and calibration standards is key to enabling meaningful evaluation of compliance with National Ambient Air Quality Standards.

The Microanalysis Research Group performs state-of-the-art research in electron and x-ray beam microanalysis. A significant achievement this year was the completion of an order for a new Auger electron spectrometry (AES) system. The panel is pleased to see that this very popular analytical method will now be available within the group. The new AES system and the transfer of a slightly older AES system from another NIST laboratory will allow the group and the division Fellows to perform research and practical analysis in support of U.S. industry, government, and academic partners. NIST researchers are already recognized as international leaders in the calculation and evaluation of fundamental data for quantitation of electron spectroscopy (AES and x-ray photoelectron spectroscopy) data. It is critical that they have access to the latest scientific equipment to support their work.

Researchers in the Microanalysis Research Group continue to drive the commercialization of new x-ray detectors for materials microanalysis. The new silicon drift detectors, whose development is being supported and encouraged by the group, will allow unprecedented high-count-rate x-ray detection. The semiconductor industry eagerly awaits the availability of commercial instrumentation, first for laboratory analysis applications, then eventually for online defect identification and classification. Other U.S. industries that require high-spatial-resolution analyses, including thin films and coatings, metals, ceramics, and catalysts, will benefit from both of these new detector technologies.

The Microanalysis Research Group has been forwarding the use of electron backscatter diffraction (EBSD; also known as Kikuchi pattern analysis) for the phase identification of individual crystalline particles. EBSD is emerging as an important commercially available crystallographic tool that complements scanning electron microscopy. This fundamental work by NIST researchers to understand the limits in particle size, background interference, and sample preparation methods will benefit any industry that needs to accurately identify small particles and structures.

The panel recognizes the important role that the Microanalysis Research Group plays in the certification and recertification of laboratories performing commercial analysis of asbestos using transmission electron microscopy. Given the serious health risks of asbestos, it is essential that commercial laboratories perform accurate analysis, yet these laboratories are under severe cost and time restrictions. The Microanalysis Research Group serves the nation by providing the technical expertise to ensure that these laboratories are providing accurate data to industrial and government customers.

Finally, the panel would like to specifically highlight the active work of the Surface and Microanalysis Science Division's NIST Fellows. The panel recognizes the major contribution that they make to the technical progress and international prestige of the division. Examples of their projects include the commercialization of microcalorimeter and silicon drift detectors for high-sensitivity and high-resolution x-ray spectroscopy; development of new visualization standard reference data for the practical measurement and development of spectral curve-fitting methods; and accurate isotopic and chemical measurements of particulate carbon.

Overall, the panel continues to be impressed with the technical achievements of the Surface and Microanalysis Science Division. The work is of the highest quality, and strong efforts are made to ensure that it addresses major customer needs. There are strong intra-CSTL and intra-NIST collaborations and extensive interactions with U.S. industry and government agencies. The panel encourages the division to continue to seek out collaborations to maximize the impact of its human and equipment resources.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
Impact of Programs

There are many examples of the impact of the Surface and Microanalysis Science Division's work; several are given here. The development of methods to analyze IAEA swipes for uranium enrichment is essential to national and international security. The development of a new urban dust standard on filters will allow rapid calibration during EPA filter analysis. The projects to aid in the commercialization of new x-ray detectors will revolutionize all aspects of materials microanalysis. All of the division's work in particle characterization will benefit a wide range of U.S. industries, including the automotive, petroleum, catalysis, semiconductor, biotechnology, optical coatings, and general chemical sectors.

The Surface and Microanalysis Science Division is a role model for collaborative research work. Joint research programs exist with all of the CSTL divisions. Within NIST, division researchers partner with the Materials Science and Engineering Laboratory (in combinatorial methods and ceramic coatings), the Electronics and Electrical Engineering Laboratory (in new analysis methods and standards for semiconductors), the Physics Laboratory (in SFG of biomimetic membranes and characterization of thin film dielectrics), and the Advanced Technology Program (in catalysts and engineered powders). The panel believes that these intra- and interlaboratory collaborations maximize the impact of the division on the broader NIST mission to support U.S. industry.

Strong external collaborations exist as well. The division has had long-standing relationships with the chemical (DuPont, Dow, Mitsui Chemical, 3M), semiconductor (SEMATECH, Lucent Technologies), and analytical instrumentation or service (Charles Evans & Associates, McCrone Associates, Noran, Peabody Scientific, Visteon, XOS) industries. Guest researchers continue to both receive and provide the technical support and new expertise within the division. The panel encourages the division to consider placing one or more of its staff on an industrial assignment to see firsthand the short- and long-term demands on their industrial counterparts. Division researchers also remained active in a variety of standards organizations, such as the International Organization for Standardization (ISO), ASTM, the Versailles Project on Advanced Materials and Standards (VAMAS), IAEA, and the International Union for Pure and Applied Chemistry (IUPAC). The staff are encouraged to participate in these activities, increasing NIST's position as a world leader in standard reference methods, data, and materials development.

The panel recognizes that the division has worked to establish a closer collaboration with the EPA on the development of standards and methods for air quality. NIST should be the primary source of standard methods and data for this important government agency, to ensure that the regulations imposed on U.S. industry are appropriate and fair.

The panel encourages the Surface and Microanalysis Science Division to further strengthen its efforts to make concrete assessments of the impact of all aspects of its work. It is recommended that at least one project in each of the four groups be selected for a more careful evaluation of the short- and long-term effects on U.S. industry or national security. Given the breadth of division collaborations, direct feedback from industrial and government partners should be obtainable. Perhaps one of the projects could be used as the next case study for a CSTL economic impact analysis. The panel believes that the work of the Surface and Microanalysis Science Division has a strong impact on U.S. industry and national security and that it is important to document this impact each year.

Finally, as noted last year, the impact of the Surface and Microanalysis Science Division would be expanded if its Web site were improved. The current Web site is only informational; it lists the division 's research areas but does not show many results. The results that are posted are not easy to find. For example, a user must move through 10 screens to see the status of the near-field scanning optical microscopy project. It should be easier to move between the research project descriptions and the

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

available databases that have resulted from the work. A Web site that has been designed for easy navigation by customers rather than for visual presence would greatly expand the dissemination of division and CSTL activities. In addition, the panel believes that the planned Web version of the mean-free-path databases is the correct direction to take for future reference data publication.

Division Resources

Funding sources for the Surface and Microanalysis Science Division are shown in Table 4.4. As of January 2000, staffing for the Surface and Microanalysis Science Division included 36 full-time permanent positions, of which 33 were for technical professionals. There were also 15 nonpermanent and supplemental personnel, such as postdoctoral research associates and part-time workers.

The quality of the division staff is outstanding. Three recent additions to the professional staff came from postdoctoral and NIST-CSTL graduate fellowship programs. One of these is the first CSTL graduate fellow to obtain a doctorate through this program. The panel is pleased with CSTL's use of these two programs to obtain technical talent.

The division continues to rely heavily on other government agency (OA) funding, especially from the Department of Defense, for capital equipment. External support accounted for a major portion of the division's budget increase in fiscal year 1999. This is appropriate, since it allows the division to fulfill its broader mission. With the addition of two Auger electron spectrometers, one newly purchased (due in 2000) and one transferred from the Physics Laboratory, the division will have a broad and now complete set of state-of-the-art analytical instrumentation.

The division is to be applauded for acting within limited resources to address the facilities issue by renovating space as it consolidates into contiguous space. However, progress is small compared with the serious nature of the facilities problem that was cited in last year 's report. Investments in basic building systems (heating, ventilation, air conditioning, electricity, air quality, vibration, water, and safety) must be made in the near future. More importantly, a comprehensive plan for addressing the ongoing needs of the existing laboratory space must be developed and executed annually. Waiting

TABLE 4.4 Sources of Funding for the Surface and Microanalysis Science 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

4.4

4.5

4.6

4.9

Competence

0.4

0.4

0.4

0.4

ATP

0.2

0.4

0.4

0.3

Measurement Services (SRM production)

0.1

0.0

0.1

0.1

OA/NFG/CRADA

2.9

2.1

2.9

3.3

Other Reimbursable

0.4

0.3

0.3

0.1

Total

8.3

7.7

8.7

9.1

Full-time permanent staff (total)a

37

37

36

36

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.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

indefinitely for the AML is not a sufficient plan—it could be 10 years before full occupancy is achieved. New instrumentation is arriving in the next 12 months (AES, SIMS) that requires state-of-the-art laboratory space to reach its full analytical capabilities. Furthermore, new equipment that is temporarily housed in substandard space may become too dirty to move into the AML's tightly controlled environment.

The unresolved issue of the final location of the Atmospheric Chemistry Group as it separates from the rest of the division remains a concern. Further, the continuing air quality problems constrain this group 's technical progress. For example, the 10 µg lower limit on carbon (14C) isotope sample measurements does not result from technological limits; it is imposed solely by air quality in the NIST laboratory. This measurement limit is unfortunately higher than levels in clean Arctic samples. The importance of the Arctic as an early warning system for global environmental change cannot be overstated, yet the current and future ability of CSTL to address these important issues is precluded by the air quality in CSTL facilities.

Indeed, project delays and quality detriments due to laboratory air quality are not rare. For example, in the preparation of the urban dust PM2.5 reference material, variations in laboratory air quality (both particulate matter and humidity) affected chemical fidelity and resuspension properties. The result was increased variability in carbon content and mass on the reference filter blanks. Construction of temporary facilities in borrowed space to get around these difficulties caused delays and unknown compromises to the project. The cost of construction and time delays represents an unrecognized additional overhead drain on the technical project. The panel encourages CSTL management to improve laboratory space, especially for the Atmospheric Chemistry Group, as soon as possible.

Physical and Chemical Properties Division
Division Mission

According to division documentation, the mission of the Physical and Chemical Properties Division is to promote U.S. economic growth by providing measurements, standards, data, and models for the thermochemical and thermophysical properties of gases, liquids, and solids, both as pure materials and as mixtures; rates and mechanisms of chemical reactions in the gas and liquid phases; and fluid-based physical processes and systems, including separations and low-temperature refrigeration and heat transfer. The Physical and Chemical Properties Division serves as the nation's reference laboratory for measurements, standards, data, and models in the areas of thermophysics, thermochemistry, and chemical kinetics.

The programs of this division comply with the NIST mission to strengthen the U.S. economy and improve the quality of life by working with industry to develop and apply technology, measurements, and standards. Each group in the division has ties to appropriate industries. The division maintains a desirable balance between research directed toward supporting shorter-term industrial needs and longer-term national science and technology needs.

Priority-setting processes and input mechanisms are in place that allow the division's management to forecast industry needs systematically. These include participation in professional societies and standards organizations (e.g., the American Institute of Chemical Engineers, Design Institute for Physical Properties Research steering committees, ASTM E-37 Committee), participation in conferences and symposia (e.g., the International Association for Properties of Water and Steam Working Group on Thermophysical Properties of Steam), trade organizations (e.g., the American Society of Heating,

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

Refrigerating, and Air-conditioning Engineers), industry roadmaps (e.g., the ITRS and Vision 20205), contact with guest researchers and NIST industry fellows, and direct customer contacts. Information from these sources is examined and used to select and to continue projects by taking into consideration the magnitude and time frame of the industrial need, the degree of correspondence between a particular need and the division's mission, the opportunity for division participation to make a major difference, the nature and size of the anticipated impact resulting from NIST participation, the division's ability to respond in a timely fashion with a high-quality solution, and the nature of opportunities afforded by recent advances in science and technology. The current program portfolio indicates that these mechanisms provide effective input to priority setting and to project selection and continuation.

Technical Merit and Appropriateness of Work

The Physical and Chemical Properties Division conducts work of unsurpassed quality in making fundamental measurements of thermophysical and thermochemical properties. The research skill level of the scientists and engineers in the division continues to be unsurpassed. In several areas the laboratory is clearly the best in the world. The large number of fiscal year 1999 publications from the division—116, nearly all of which are in peer-reviewed journals—and the participation of division personnel in lead editorships (including International Journal of Chemical Kinetics, International Journal of Thermophysics, Journal of Chemical Thermodynamics, and Journal of Physical and Chemical Reference Data) also indicate the technical and scientific quality of these researchers and the regard of the scientific community for their work. The division 's programs are highly relevant to industrial needs for accurate measurements, standards, data, and models in the areas of thermophysics, thermochemistry, and kinetics. The division's program plans are the result of extensive external input mechanisms that ensure adequate consideration of future industrial needs and emerging scientific areas. Highlights of the technical program follow.

The division is a unique national resource that bridges the gap between research directed at addressing the often short-range goals of industry and the long-range, open-ended inquiry commonly pursued in universities. Maintaining this balance is difficult, yet several projects within the division illustrate how this can be done successfully, as discussed below.

The Chemical Reference Data and Modeling Group compiles, evaluates, correlates, and disseminates Standard Reference Data, and it develops and disseminates electronic databases and software for thermodynamics, mass spectroscopy (MS), and IR spectra. It maintains and continues to develop the NIST Chemistry WebBook, a vital resource for industrial, academic, and government agency research. This searchable compilation of thermochemical data and spectra, which is designed for Internet access, contains data for more than 31,800 chemicals in the current fifth edition. Between 6,000 and 12,000 users per week access the WebBook, an increase of about 25 percent since 1998. A key product of the Chemical Reference Data and Modeling Group is the NIST-EPA-National Institutes of Health Mass Spectral Library, which is used in more than 65 percent of mass spectrometers manufactured in the United States. The addition of a new library component, the Automated MS Deconvolution and Identification System, has now been completed, thus allowing more systematic evaluation of mass spectra. In addition, during the past year, a new experimental program was initiated to measure selected gas chromatographic spectra and relate these to the Mass Spectral Library. This program will provide technical leadership for the emerging area of gas chromatography (GC)-MS applications.

5  

American Chemical Society, Technology Vision 2020: The U.S. Chemical Industry, American Chemical Society, Washington, D.C., 1996.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

The Computational Chemistry Group develops and applies computational methods, theories, and models for estimating and predicting chemical and physical properties of industrially and environmentally important molecules, rate constants of chemical reactions, and thermochemical properties of compounds. The group has successfully passed the start-up phase to become a well-run and productive part of the division. The work on the experimental and theoretical determination of mechanisms, kinetics, and thermochemistry of chlorinated species illustrates the very effective way in which this group's activities complement and enhance existing capabilities. The development of an online Computational Chemistry Comparison and Benchmark Database serves the needs of industry for accurate thermophysical property data by allowing users to compare experimental data and recommended computational prediction methods for the thermochemical properties of more than 500 compounds. Supported from the CSTL Director's Reserve, group scientists have developed the highly original and novel isopotential mapping computational method for the discovery of reaction paths.

The Experimental Kinetics and Thermodynamics Group develops and uses state-of-the-art measurement techniques to obtain kinetic and thermodynamic properties of industrially and environmentally important chemical species and materials and to determine the rates and mechanisms of chemical reactions in the gas and liquid phases. Three world-class activities are summarized here:

  1. The Next-Generation Kinetics Database is a new project, which includes critical evaluation of existing chemical kinetic data and application of computational tools to predict unmeasured rates. This Web-based database, unique in the world, will be a critical resource in the simulation of practical processes such as environmental processes, chemical synthesis in industry, waste incineration, and power generation with minimum pollutant formation. The panel eagerly awaits its completion.

  2. A unique reactor for studying the kinetics of reactions in supercritical water has been constructed and is now operational. Treatment of waste in supercritical water reactors is expensive but may provide the only efficient method available for very hazardous materials. These experiments, unavailable at any other research institution, will facilitate the design of improved treatment methods for disposal of such waste products in supercritical media.

  3. The experimental chemical kinetics of chlorinated species is being examined to provide critical rate data necessary to model incineration of chlorinated waste organic materials and to validate ab initio calculations of reaction rates that are impossible to measure accurately. Incineration of chlorinated species can form very toxic by-products, and a detailed knowledge of the chemistry of these reactions is critical to minimize this occurrence. This project is an example of the world-class gas-phase chemistry performed by this group. It also exemplifies the close collaboration that exists with the Computational Chemistry Group, which provides the ab initio calculations. This collaboration exemplifies the efficient use of scarce funding and is to be commended.

The Process Separations Group has been divided into two projects: (1) Properties for Process Separations and (2) Membrane Science and Technology. The Properties for Process Separations project provides critically evaluated data and models on a variety of industrially important fluid-based separation processes including distillation, adsorption, and supercritical fluid extraction. A novel method for measuring the enthalpy of adsorption of organic compounds on clay has been developed using a clay-coated capillary GC column. This technique allows study of the interaction of clays with organic substances. Absorption of organics on clay is a key process in practical applications ranging from pollution remediation to the manufacture of cosmetics and pharmaceuticals. Therefore, results from this project will have a very significant impact on both industry and the environment. A new project, funded from the CSTL Director's Reserve, has been initiated to characterize lubricant degradation at load-bearing surfaces of refrigerant compressors using spectroscopic and GC-MS techniques. The research

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

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.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

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.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

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.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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-

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

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

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

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.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

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.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×

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.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
  • 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.

Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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×
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×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
×
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×
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Suggested Citation:"Chemical Science and Technology Laboratory." National Research Council. 2000. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2000. Washington, DC: The National Academies Press. doi: 10.17226/9979.
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