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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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4
Chemical Science and Technology Laboratory

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

PANEL MEMBERS

James W. Serum, SciTek Ventures, Chair

Alan Campion, University of Texas, Austin, Vice Chair

Ulrich Bonne, Honeywell Laboratories

Douglas C. Cameron, Cargill, Inc.

Robert E. Ellefson, Inficon, Inc.

E. William Kaiser, Ford Motor Company

John W. Kozarich, ActivX Biosciences, Inc.

Max G. Lagally, University of Wisconsin-Madison

R. Kenneth Marcus, Clemson University

James D. Olson, The Dow Chemical Company

Athanassios Z. Panagiotopoulos, Princeton University

Frank K. Schweighardt, Air Products and Chemicals, Inc.

Gary S. Selwyn, Los Alamos National Laboratory

Michael L. Shuler, Cornell University

Christine S. Sloane, General Motors Corporation

Anne L. Testoni, KLA-Tencor Corporation

Peter Wilding, University of Pennsylvania Medical Center

Submitted for the panel by its Chair, James W. Serum, and its Vice Chair, Alan Campion, this assessment of the fiscal year 2002 activities of the Chemical Science and Technology Laboratory is based on site visits by individual panel members, a formal meeting of the panel on March 12-13, 2002, 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: Annual Report FY2001, NISTIR 6856, National Institute of Standards and Technology, Gaithersburg, Md., February 2002.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

LABORATORY-LEVEL REVIEW

Technical Merit

The mission statement of the Chemical Science and Technology Laboratory (CSTL) is as follows: As the Nation’s Reference Laboratory for chemical measurements, CSTL provides the chemical measurement infrastructure to enhance U.S. industry’s productivity and competitiveness; assure equity in trade; and improve public health, safety, and environmental quality.

CSTL continues to carry out research of excellent technical merit overall. The panel wishes to draw attention here to several outstanding examples:

  • “Ionic liquids” are a class of organic compounds that have been proposed as environmentally friendly solvents for some important industrial processes. This past year, CSTL initiated a program to obtain and disseminate fundamental physical and chemical properties data for some of these compounds in order to facilitate industrial adaptation of these new solvents. The laboratory has anticipated industry need for these data—to the extent that the compounds are not yet available commercially and must be synthesized in-house for study.

  • The laboratory is also continuing work to control and characterize fluid flow in microfluidic devices. This work is noteworthy not only because of its world-class technical merit but also because of the strong industrial involvement in the program and its applicability across a broad spectrum of problems in chemistry, biology, and medicine.

  • Fluorescence spectroscopy is an old “workhorse” technique used in biochemical assays. Despite its long history of use, few standards exist for measuring the intensity of the fluorescent signal, making quantitative assays using this technique unreliable at best. Because of increased use of fluorescent techniques in clinical applications, CSTL is developing standards for these measurements, which will have a significant impact on the quality of clinical measurements made using this technique.

  • CSTL efforts to develop high-throughput characterization of particle properties is not only relevant to industries as diverse as paints and coatings manufacturers and semiconductor manufacturers but is noteworthy for its interlaboratory collaborations.

Several programs were noteworthy for the use and development of cutting-edge technologies. A new primary standard for pressure is under development; it determines pressure by measuring and calculating the dielectric constant of helium rather than by using the mechanical artifacts of existing pressure standards. CSTL work on characterizing degraded DNA samples is pushing forward the state of the art in mass spectroscopic techniques. In work aimed at characterizing “soft” surfaces such as biomaterials and polymers, the laboratory is developing new cluster-ion secondary ion mass spectrometry (SIMS) techniques.

The Chemical Science and Technology Laboratory is organized in five divisions: Biotechnology Division, Process Measurements Division, Surface and Microanalysis Science Division, Physical and Chemical Properties Division, and Analytical Chemistry Division (see Figure 4.1). These units are reviewed in turn under “Divisional Reviews” below in this chapter.

Program Relevance and Effectiveness

The panel found CSTL to be very proactive overall in identifying the customers of its work. In most cases, researchers have a good understanding of how their work meets the needs of those customers. In

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

FIGURE 4.1 Organizational structure of the Chemical Science and Technology Laboratory. Listed under each division are the division’s groups.

addition to their technical description, all projects presented to the panel had a concise statement of the anticipated industrial use. The panel was pleased to see an increased awareness of customer impact since its last assessment.

Particularly noteworthy for their relevance and effectiveness are the laboratory’s efforts in Standard Reference Materials (SRMs), Standard Reference Databases (SRDs), and international standards activities. These services and activities rarely garner headlines but have a large leverage effect in industry and underpin many critical measurements in the chemical, pharmaceutical, medical, and other industries. For example, the laboratory recently completed a series of SRMs for in vitro diagnostic testing. These SRMs will allow U.S. manufacturers to qualify their products for sale in the European Union. The panel anticipates that the positive impact for U.S. manufacturers will be substantial. NIST-Traceable Reference Materials (NTRMs), discussed in the Analytical Chemistry Division assessment below, have tremendous leverage in the chemical products industry and are also of value to National Laboratories, environmental laboratories, academic institutions, and other industries. Web-based databases are growing in size and number and are improving in quality. The panel is pleased with CSTL efforts in Web-based dissemination and finds that the laboratory’s Web-based dissemination continues to improve in utility and effectiveness. The laboratory has now hired a staff member dedicated to the effectiveness of Web usage and maintenance, which the panel applauds. However, funds are insufficient to maintain and update all of the laboratory’s Web-based tools. The panel is concerned about the utilization of these

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

databases if CSTL does not take advantage of the opportunity that the Web provides to continually update material. The laboratory needs to develop a strategy to determine how it will utilize its limited resources for Web-based dissemination.

Laboratory Resources

Funding sources for the Chemical Science and Technology Laboratory are shown in Table 4.1. As of January 2002, staffing for the laboratory included 270 full-time permanent positions, of which 232 were for technical professionals. There were also 92 nonpermanent or supplemental personnel, such as postdoctoral research associates and temporary or part-time workers.

The panel observed too many priority projects with subcritical resources devoted to them. It may be that CSTL needs to reexamine its prioritization, either to find additional resources for top priorities that are undersupported or to terminate efforts that cannot be supported effectively. CSTL has also targeted certain areas for strategic program growth. The panel cautions against implementing strategies in these areas too quickly, before the appropriate expertise is in place to launch efforts most effectively. For example, the CSTL program in tissue engineering does not seem to have the complete skill set necessary to meet its goals.

TABLE 4.1 Sources of Funding for the Chemical Science and Technology Laboratory (in millions of dollars), FY 1999 to FY 2002

Source of Funding

Fiscal Year 1999 (actual)

Fiscal Year 2000 (actual)

Fiscal Year 2001 (actual)

Fiscal Year 2002 (estimated)

NIST-STRS, excluding Competence

37.9

37.7

36.9

37.7

Competence

2.4

2.4

1.9

2.7

ATP

3.0

3.3

3.2

2.4

Measurement Services (SRM production)

2.4

2.2

1.9

1.9

OA/NFG/CRADA

10.9

14.2

14.3

15.4

Other Reimbursable

3.4

3.4

5.8

5.1

Total

60.0

63.2

64.0

65.2

Full-time permanent staff (total)a

276

275

264

270

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.”

aThe number of full-time permanent staff is as of January of that fiscal year.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

Strategic program goals must be coordinated with a plan for resources, including human resources, in order to ensure that resources are fully leveraged and programs have a sufficient critical mass to be effective. The panel is concerned that CSTL lacks a human resource plan, which would enable better personnel development, succession planning, and acquisition of new skills through hiring or retraining.

The panel recommends that the laboratory utilize a fellowship program for rapid development of the technical expertise needed for growth areas. A program in which NIST researchers spend a period of several months to a year in industry can greatly facilitate bringing new skills into the laboratory. All fellowships awarded must include a clear plan for how the new skills of the awardee will be used once he or she returns to NIST. The program must also be clearly tied to advancement, reward, and recognition to give employees an incentive to participate.

Midlevel managers in CSTL, especially group leaders, are being called on to exercise an increasing number of skills. They generally maintain an active research program while tending to personnel management, leadership of staff, and marketing of programs to industrial customers. Little training seems to be provided to support them in this work. The panel urges a proactive approach to training managers and prospective managers in these areas in order to enable their success. The result should pay off for the laboratory in terms of better coordination of programs, better communications to all levels of staff, and higher overall staff morale.

Facilities for CSTL research have improved greatly in the past 5 years, and the completion of the Advanced Measurement Laboratory (AML) will have a major positive impact. Equipment on hand is generally state of the art, although in some cases the equipment needed to meet goals is not in place. The panel believes that CSTL should clarify its thinking on an in-house microelectromechanical systems (MEMs) production facility. The panel did not see a clear rationale for a decision to procure that capacity in-house versus obtaining it off campus. Because of the high cost of maintaining such a facility, the panel recommends that CSTL and NIST be certain that any make/buy decision on MEMs production take into account the long-term costs of such a facility. The panel is pleased to see that the Hollings Marine Laboratory in Charleston, South Carolina, in which CSTL is a partner with NOAA and state agencies, is being appropriately equipped from the outset.

Laboratory Responsiveness

Clear examples of strong responsiveness to last year’s report2 exist. For example, in response to panel comments, time and funds were reprioritized to increase efforts in international activities and collaborations in analytical chemistry. Some divisions greatly enhanced the usability of their Web-based information, also in response to panel recommendations.

Responses in some areas were not as strong. For example, the panel has pointed out the lack of critical mass in program areas such as atmospheric chemistry. While recognizing that it is difficult to make decisions to redirect resources, some situations have been allowed to linger despite repeated comments from the panel. Such situations are having an increasingly negative impact on the morale of involved staff members.

In general, the panel is satisfied with the CSTL’s response to its 2001 report. It urges the laboratory to try harder to respond to the more difficult recommendations or to provide better explanations for why these recommendations were not acted upon.

2  

National Research Council, An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2001, National Academy Press, Washington, D.C., 2001.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

MAJOR OBSERVATIONS

The panel presents the following major observations:

  • Chemical Science and Technology Laboratory programs continue to have high technical merit overall.

  • Awareness of customer needs and customer impact is increasing at all levels of CSTL staff.

  • The panel is pleased with improvements made to CSTL use of the World Wide Web. Hiring a staff member devoted to Web utilization and Web-based dissemination is a positive step. A strategy is needed for Web-based dissemination, as databases currently exist that are not kept up to date.

  • CSTL needs a human resources plan that can be integrated with the CSTL strategic plan to account for the training, hiring, and succession planning needed to achieve laboratory goals and objectives.

  • CSTL should utilize industrial fellowships to learn more about its customers and to quickly gain skills necessary to achieve objectives in new and emerging areas. Any plan to place a staff member in industry for an extended period must include a plan for how that person will utilize new skills upon returning to NIST. In order to attract staff participation, industrial fellowships must be tied to advancement, reward, and recognition.

  • More proactive training of group leaders is required to help them achieve success in the multiple roles they are called on to fill in their positions.

  • CSTL should reexamine the rationale for its decision on building a microelectromechanical systems fabrication capacity in-house. If the decision is made to go forward with an on-campus facility, a long-term plan is necessary to provide for the cost of maintaining and utilizing it.

DIVISIONAL REVIEWS

Biotechnology Division

Technical Merit

According to division documentation, the mission of the Biotechnology Division is to advance the commercialization of biotechnology by developing the scientific and engineering technical base, reliable measurements, standards, data, and models to enable U.S. industry to quickly and economically produce biochemical products with appropriate quality control. The Biotechnology Division has four groups: DNA Technologies, Bioprocess Engineering, Biomolecular Materials, and Structural Biology. The division is also evolving a Bioinformatics Group from the Structural Biology Group. The division’s ongoing programs are appropriately aligned with its mission, and the scientific work is of high quality comparable with that at research-oriented universities and in leading industrial laboratories. The division’s challenge is to select those projects that are most critical and that will have the greatest impact on this rapidly growing and changing field.

The DNA Technologies Group carries out research to enhance measurement technologies and to provide SRMs for application in areas related to the detection and characterization of DNA. The group maintains a strong focus on standards development, nucleic acid characterization, and measurement development for the diagnostic and forensic communities. The group’s programs are quite wide ranging and are, in general, of outstanding quality.

The DNA Technologies Group is pioneering the development of SRMs for human identification

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

and is developing a critical database on short tandem repeats (STRs). The development of these methodologies for human identification is being carried out in collaboration with and with the support of the National Institute of Justice. This research is state of the art and continues to push the technology into new, productive, and high-impact areas. The development of new high-speed matrix-assisted laser desorption ionization (MALDI) time-of-flight mass spectrometric techniques with automated sample preparation is addressing the need for high-throughput analysis of genetic samples. Projects focusing on identification methodologies for the Y chromosome and mitochondrial DNA continue to make impressive progress. The development of Y-STR megaplex assays will greatly increase the acceptance of these identification techniques within the forsenic community. Genotyping of single nucleotide polymorphisms in the Y chromosome and the mitochondrial genome, the development of the prototype Y chromosome standard (SRM 2395), and the enhanced version of the human mitochrondrial DNA SRM 2392 have all progressed well in the past year.

The DNA Technologies Group has also successfully integrated state-of-the-art instrumentation into its programs. One CRADA with a biotechnology company led to the development of rapid capillary electrophoresis (CE) methods for mutation detection. Other work has focused on developing procedures for single-strand conformation polymorphism detection by CE. Another major program has centered on developing methods for detecting and quantifying DNA damage and repair in cancer detection and treatment. Methods have been developed to characterize DNA damage on a molecular scale at levels approaching one base per million using gas chromatography/mass spectrometry (GC/MS) techniques. These methods have been useful in the study of the kinetics and specificity of DNA repair by specific enzymes. Additional studies are concentrated on apoptosis, or programmed cell death, as well as detection of cellular responses to radiation. This work has potentially high-impact value.

The DNA Technologies Group also houses the NIST/National Cancer Institute (NCI) Biomarker Validation Laboratory (BVL), part of NCI’s Early Detection Research Network (EDRN). The BVL validates biomarkers of early cancer detection and cancer risk, supports the development and implementation of high-throughput biomarker analysis, and collaborates with Network Clinical and Epidemiology Centers (NCECs) in technology transfer. The panel was impressed with the accomplishments of the past year, including validation analysis of fluorescence in situ hybridization (FISH) for cancer risk analysis; technical improvements in polymerase chain reaction (PCR) DNA sequencing technology for analysis of mitochondrial DNA base mutations for lung cancer; and the development of capillary electrophoresis methods for analysis and quantification of telomerase. The work is cutting-edge and of high impact.

The Bioprocess Engineering Group develops measurement methods, databases, and generic technologies related to biomolecules and biomaterials in manufacturing. The group, which consists of 12 researchers, has activities in eight areas: (1) fluorescence intensity measurements, (2) biothermodynamics, (3) biotech grain testing, (4) quantitative PCR reference materials, (5) chorismate pathway enzymology, (6) biocatalytic hydroxylation/epoxidation, (7) bioelectrochemistry, and (8) DNA separations. The quality of the group’s work is high, and its activities and accomplishments are clearly presented in a useful and well-designed Web site.

The Structural Biology Group participates in the Center for Advanced Research in Biotechnology (CARB), a joint NIST/University of Maryland (UMD) research center located on the Shady Grove campus of UMD about 4 miles from NIST. Scientists at CARB develop and apply measurement methods, databases, and state-of-the-art modeling methods to advance the understanding of protein structure/function relationships. Current programs in x-ray crystallography, biomolecular nuclear magnetic resonance (NMR) spectroscopy, protein folding, computational chemistry and modeling, and mechanistic enzymology are outstanding. The NIST component of CARB has succeeded in attracting

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

several first-rate young investigators who have nicely blended their NIST-focused programs into the academic culture that they share with their UMD colleagues. The result is a stimulating research environment that maintains the mission-oriented flavor critical to NIST programs. Notable programs include research on the biothermodynamics of protein/protein and protein/nucleic acid interactions, single-molecule measurements, studies on computational molecular evolution, and the development of cell membrane hybrid bilayers for a high-throughput screening assay for membrane receptors. In addition, ongoing work on the x-ray and NMR structures of proteins and nucleic acid is of high quality.

The newly evolved Bioinformatics Group has four major projects: the Protein Data Bank (PDB), the Biomolecular Crystallization Database (BMCD), the Bioinformatics Software Resource (BISR), and the HIV Protease Structural Database (HIVDB). The PDB is a major national and international resource and a very visible success for NIST. The goal of the BISR is to create a database of commercial and noncommercial bioinformatics software. The panel was gratified to learn that the group has developed educational and outreach materials for high schools and has hired high school students to work in the laboratory. Overall, this group is making exceptional contributions to bioinformatics. Hiring and retention are continuing challenges for the group owing to a high demand for such skills in the biotechnology and pharmaceutical industries. The group currently consists of approximately 10 people.

The Biomolecular Materials Group builds on its skills in surface science, optics, biophysics, and chemistry to support research in protein structure/function relationships, biopolymer transport processes, biosensors, molecular recognition, protein/lipid and protein/protein interactions, mechanism of protein adsorption, and tissue engineering. The panel was very impressed that the group was awarded two NIST Competence programs with funding through FY 2007. The first, Single Molecule Manipulation and Measurement (SM3), is a collaboration between CSTL, EEEL, ITL, and PL. This program builds on the group’s historical strengths. Research planned in single-molecule force metrology and single-nanopore-based analyte sensors is particularly noteworthy. The second, Metrology for Tissue Engineering: Test Patterns and Cell Function Indicators, involves collaboration with MSEL. The tissue engineering effort is newer to this group. This program focuses on the use of indicator cells to evaluate cellular response to exposure to a new biomaterial. While most of the group’s efforts are understaffed in comparison with the potential of the research problems, the addition of more staff to the tissue engineering effort is particularly critical. At the time of the panel’s visit, a search was under way for a postdoctoral associate. Filling this position with an appropriately trained individual will be important to ensure rapid progress. The group is well situated to make contributions to these exciting and rapidly evolving research areas with its strong intellectual leadership and first-rate science and technology.

Program Relevance and Effectiveness

The Biotechnology Division has selected a wide range of exciting emerging research areas that will be critical to the nation’s future industrial competitiveness and safety. The division is well positioned to support efforts in genomics, proteomics and structural biology, tissue engineering, standards for genetically modified crops, and characterization and manipulation of single molecules such as DNA. As a whole, the division has selected a very appropriate set of research areas to which to apply its limited resources. The panel and the division both recognize that the range of potential issues in biotechnology is vast and that the potential number of customers for the division’s work is in the thousands. Since all of these issues and many potential customers cannot be served by a group of the division’s size, the prioritization of research problems is critical. The panel concurs with the priorities chosen by the division.

The division demonstrated its ability to respond to customer needs on an emergency basis in its response to the fall 2001 terrorist attacks. The DNA Technologies Group has developed new techniques

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

to permit identification of persons from highly degraded DNA and is assisting agencies that are using these methods to help identify victims of the World Trade Center attacks.

The Biotechnology Division is by nature cross-disciplinary and has strong international connections. The two Competence awards to the division promote cross-division and cross-laboratory collaborations and communications. The interaction with CARB also promotes an externally oriented perspective. The Protein Data Bank is an international effort. The division is a coleader of the Consultative Committee for the Amount of Substance Biometrology Working Group. This activity involves about 30 countries. Division scientists played an important role in the recommendations of the International Union for Pure and Applied Chemistry (IUPAC) for differential scanning calorimetry measurements. Division staff members played leadership roles in the Second International Conference on Oxidative Stress and Aging, sponsored by the Oxidative Stress and Aging Association.

The division makes substantial use of the Web to disseminate information. It maintains four major databases: the Protein Data Bank (a research collaboratory for structural bioinformatics), the Biological Macromolecule Crystallization Database (SRD 21), the Short Tandem Repeat DNA Database, and the Thermodynamics of Enzyme-Catalyzed Reactions Database (SRD 74). These databases are important resources for scientists worldwide. Some units (e.g., the Bioprocess Engineering Group) have made significant improvements to their Web sites in the past year.

The panel notes that the research in the division aligns well with three strategic focus areas identified in the NIST strategic planning process: health care, nanotechnology, and knowledge management. The central focus of the division is closely related to health care. The SM3 program has necessitated the division’s development of expertise in nanotechnology. The division’s bioinformatics programs are an important example of knowledge management.

The panel reviewed the division’s responsiveness to prior reports. The primary challenge to the division’s ability to maintain relevance and responsiveness to customers is that of maintaining and developing critical mass in emerging areas. This challenge requires the division to reassess research priorities constantly and to encourage staff development in new areas. The panel has seen clear evidence of strategic planning and of reprogramming, particularly in genomics and proteomics, nanotechnology, and tissue engineering. The panel also expressed concern last year about maintaining the proper balance between STRS monies and funding from other sources. While some increase is seen in the use of other funding, particularly with the DNA Technologies Group, the panel believes other groups could benefit from a higher proportion of outside funding. It is difficult to change this balance rapidly.

The DNA Technologies Group has maintained high external visibility and programmatic relevance, as evidenced by the high level of external funding it has received to support its programs. Such funding has positive aspects, since it requires the group to maintain a high degree of customer responsiveness. The group is well positioned to respond to customer needs in genomics and proteomics. However, given the general manpower and resource constraints that it is facing and its deep commitment to several key external programs, the group may be spreading itself too thin and may not be able to mount the kind of program needed in proteomics. The leadership of the group and the division must carefully assess priorities and resource distribution to assure that key programs are adequately supported. The group should also develop a plan that prioritizes proteomics efforts consistent with ongoing commitments and the current expertise base.

The Bioprocess Engineering Group has made significant contributions in each of its eight areas but is spread too thin for a group of 12. The panel recommends its reducing the number of project areas and aligning better with the NIST Strategic Focus Areas of health care, nanotechnology, and knowledge management. One promising area that would draw on the group’s strengths is the characterization of

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

complex, heterogeneous proteins such as the glycosylated protein drugs being developed by the pharmaceutical industry. Currently, the Bioprocess Engineering Group does not rely on outside funding for any projects. Increasing the amount of outside funding to around 20 percent could allow the division to increase the number of researchers on each project and would demonstrate external buy-in to projects. The group’s biotech grain testing and quantitative PCR reference materials projects are areas of growing importance in the food and agriculture industries; such testing and standards are important for regulatory compliance, human health and safety, global trade, and identity preservation of crops. This effort is highly responsive to NIST customer needs and has resulted in CRADAs with seed companies. The number of people working on this project in the Bioprocess Engineering Group has doubled, from one to two, since last year, but is still understaffed relative to its full potential. The Bioprocessing Engineering Group should continue to strengthen its interactions with the DNA Technologies Group to further leverage its efforts.

The Bioprocess Engineering Group continues to deliver high-quality thermodynamics data, as evidenced by the recent publication of thermodynamic quantities for the ionization reactions of biological buffers. The group has also released thermodynamics software. However, the software requires Mathematica, a program that is widely available in academia and in engineering groups in industry but not commonly used by biologists. For the use of its biothermodynamics data, the group should consider developing software that is built on more commonly used software such as Excel or that can be used directly via the Internet.

The relationship to CARB is a critical issue for the Structural Biology Group. The University of Maryland began the CARB collaboration more than 10 years ago. In the panel’s judgment, the NIST and university cultures have been integrated successfully. The current group of NIST investigators at CARB has straddled both cultures effectively. Young NIST investigators are competitive with the best young academic faculty nationwide. However, with regard to manpower and resources, the NIST component of CARB appears to be at a crossroads. NIST manpower levels at CARB are at or near their lowest point, and the division is clearly concerned about NIST’s commitment to rebuilding its presence at CARB in light of flat budgets and decreasing permanent positions. This situation is exacerbated by the fact that another expansion of CARB has been planned, and it is not clear to the Structural Biology Group if NIST will commit the kind of resources needed to maintain a robust presence relative to its UMD peers. CARB has been an important and successful collaboration for NIST, but a clear strategic vision needs to be articulated for the NIST role in the future of this institution. The ongoing search for a new CARB Director also contributes to staff anxieties over the future.

Despite these uncertainties, the Structural Biology Group is expanding its interactions with industry in the vibrant biotechnology sector found in the Washington, D.C., area. A new CRADA with MedImmune was established to undertake a thermodynamic characterization of monoclonal IgM using calorimetric methods. Another new CRADA with Genetics Institute, Inc. explores biophysical and crystallographic attributes of thioredoxin fusion peptides and proteins.

The Bioinformatics Group faces several challenges in maintaining program relevance and effectiveness. The PDB project, an important and high-impact resource for the molecular biology community, will be challenged to keep up with the large number of new protein structures that will be generated by large-scale proteomics projects. The BISR project has the worthy goal of creating a database of commercial and noncommercial bioinformatics software. The panel suggests that one way to strengthen and grow this effort is to convince the key bioinformatics journals to require that software mentioned in publications be archived in such a database. As part of the HIVDB project, the Bioinformatics Group is developing tools for structural-based queries for drug interactions. The panel was impressed with the initial progress of this effort and recommends that feedback from industrial medicinal chemists be

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

incorporated into the query tools. The panel also recommends that the drug interaction database be extended beyond proteases to other proteins such as protein kinases. Overall, this group is responsive to a wide range of users and has a strong customer-service orientation.

The Biomolecular Materials Group is very forward looking, and its targeted technologies are just emerging in the industrial sector; the two recently funded NIST Competence programs mentioned above confirm the potential relevance of its efforts. Because of the emerging nature of the technology it is working on, this group has fewer obvious links to industrial firms. However, its projects have explicit relevance to tissue engineering firms and to regulatory agencies such as the Food and Drug Administration (FDA). The SM3 project is addressing issues that will be needed in biomicroelectromechanical systems (bioMEMs) projects. Efforts to validate new methods for characterizing nanopores with “molecular rulers” and for DNA sequencing are also important. The research on high-density biological arrays has clear relevance to high-throughput proteomics and to biohazards detection, both of which are critical research areas that would benefit greatly from improved detection techniques. The relevance of this group’s work to supporting critical emerging technologies is high. However, the panel would like a better understanding of how the group will actively link its contributions to customers.

Division Resources

Funding sources for the Biotechnology Division are shown in Table 4.2. As of January 2002, staffing for the division included 37 full-time permanent positions, of which 32 were for technical professionals. There were also 24 nonpermanent or supplemental personnel, such as postdoctoral research associates and temporary or part-time workers.

The availability of adequate human resources remains the critical resource issue for the division. Funding and personnel numbers estimated for 2002 are up by about 8.5 percent compared with those for

TABLE 4.2 Sources of Funding for the Biotechnology Division (in millions of dollars), FY 1999 to FY 2002

Source of Funding

Fiscal Year 1999 (actual)

Fiscal Year 2000 (actual)

Fiscal Year 2001 (actual)

Fiscal Year 2002 (estimated)

NIST-STRS, excluding Competence

6.5

6.5

6.6

6.9

Competence

0.8

0.8

0.4

1.0

ATP

1.7

1.9

1.3

0.7

Measurement Services (SRM production)

0.1

0.0

0.3

0.2

OA/NFG/CRADA

1.7

2.2

1.9

2.8

Other Reimbursable

0.1

0.3

0.2

0.2

Total

10.9

11.6

10.7

11.8

Full-time permanent staff (total)a

37

35

32

37

NOTE: Sources of funding are as described in the note accompanying Table 4.1.

aThe number of full-time permanent staff is as of January of that fiscal year.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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2001. The panel is pleased to note this slight growth. The rapidly changing nature of research opportunities in biotechnology will always challenge the division to assemble the critical mass of human resources needed to attack these emerging opportunities. As a whole, the division has managed its resources well. However, expertise in plants, animal cell culture, and tissue engineering is rather minimal for supporting the aspirations of the division and the needs of its customers. The panel appreciates the difficulty of expanding core personnel in the current fiscal environment, but human resources are the primary limitation for the division (also, see the discussion on manpower levels at CARB in the preceding subsection, “Program Relevance and Effectiveness”).

The division lost two staff members in bioinformatics in the past year. NIST can expect significant competition for personnel in bioinformatics. Many organizations in the Washington, D.C., area can pay people with these skills much more than government agencies can. The growth of the local biotech industry and the expansion of the Howard Hughes Medical Foundation will mean a highly competitive local job market in biotechnology. As the economy recovers, this competition will only intensify.

The challenge of employing human resources optimally is affected not just by the supply of funds but also by the type of fiscal support currently available in the laboratory. The internal STRS funds do not currently cover the salaries of all of the division staff, which has led to a significant dependence on support from other agencies. Different programs within the Biotechnology Division appear to have different attitudes toward the use of noncore funding and its application to staffing. In some programs, staff aggressively pursue OA funding in order to hire new personnel and expand into new areas. In others, permanent positions are not created unless they can be supported by NIST core money. The former approach embraces risk and increases the potential impact of a group’s work, while the latter allows program managers to be assured that mission-critical activities are sustained and NIST’s customer base will be served. The panel recognizes that both approaches have value, but suggests that modest dependence on external funds be encouraged.

The panel also noted a need for increased computer support and additional disk storage space for the Bioinformatics Group.

Process Measurements Division

Technical Merit

The Process Measurements Division’s mission is to pursue basic research efforts in measurement science; enhance the state of the art in measurement standards and services; provide recommended measurement techniques; standardize recommended practices in sensing technology, instrumentation, and mathematical models required for analysis, control, and optimization of industrial processes; and provide a central, national source for calibration of measurement equipment. The Process Measurements Division has six groups: Fluid Flow, Fluid Science, Process Sensing, Thermometry, Pressure and Vacuum, and Thermal and Reactive Processes.

A core responsibility of the Process Measurements Division is the improvement and dissemination of national measurement standards for temperature, fluid flow, air speed, pressure and vacuum, humidity, liquid density, and volumetric measurements. The division also interacts with its counterparts in other countries and represents the United States at international measurement science conferences. The division’s research currently supports 6 of the 12 major CSTL programs with a broad range of research in new and traditional fields, development of world-class measurement methods, standards, calibration services, and measurement of important physical properties for industry. The division’s efforts are divided among the development of calibrations and reference materials, the development of new mea-

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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surement methods, and database activity. The division staff balances its activities in order to perform its dual roles of addressing the calibration and reference material needs of customers and advancing the state of the art in measurement science in the fields applicable to the division’s mission.

The panel is impressed by the concentration of measurement knowledge and expertise in this division and by the quality of its work. The technical merit of its work remains high. The panel noted major progress in the development of new cutting-edge measurement technologies and improvements in measurement and calibration uncertainties in flow, pressure, temperature, and humidity. Ongoing efforts in the development of new sensors, measurement methods, and process models show good progress. Some highlights of the division’s work in the past year are presented below.

The division has improved flow measurements in the 1 to 1,600 L/min range with a newly completed, automated pressure-volume-temperature flow accumulator. This improvement reduces the uncertainty of flow calibration results by a factor of 4 relative to the old mercury-sealed calibrator pistons and the still-older bell-prover method, which the division has now phased out. The division’s leadership in the area of flow measurement is evidenced by its staff members chairing the BIPM/CIPM (Bureau Internationale des Poids et Mésures/Comité International des Poids et Mésures) Working Group for Fluid Flow and the Sistema Interamericano Metrología (SIM) Metrology Working Group for Fluid Flow.

In FY 2001, the division participated in four Consultative Committee for Mass and Related Quantities (CCM) Key Comparisons (KCs) and piloted three of them, two to completion of Draft B reports. These two completed comparisons were notable for being the first successful international comparisons in this pressure range (which was due to the division’s innovative transfer standard design) and for being the only CCM pressure comparisons to be completed on time. The division is developing a pressure standard based on the dielectric constant of helium to provide an alternative to the conventional dead-weight methods for intercomparison standards. The division has come to within a factor of 10 of the accepted pressure-sensing uncertainty standard. Before this new standard is available, NIST may need to replace aging piston gauges for the old standard in order to maintain competence for industrial calibrations. In another effort related to pressure gauges, division scientists developed a portable transfer standard using a vibratory/resonant MEMS sensor that achieved impressive performance in terms of sensitivity and stability, as demonstrated with data taken in a NIST-directed international comparison of pressure gauges.

The division has been the pilot lab for the CIPM Key Comparison 3 (K3) covering temperatures from 84 K to 933 K (−189 °C to 660 °C). As the pilot lab, the division has authored a comprehensive report on K3, which was approved by the Consultative Committee on Temperature (CCT) in 2001. This is a major accomplishment in improving the ITS-90 standard in this temperature range and helps establish the equivalence of the measurements performed by various national measurement institutes (NMIs), a resource that is important to industry in international trade. The 8th International Decadal Conference, Temperature: Its Measurement and Control in Science and Industry, is being organized under CSTL’s leadership.

The division completed constant-volume gas thermometry measurements up to 700 °C, demonstrating that the NIST spherical acoustical resonator produces the most accurate thermodynamic gas temperature measurements as a realization of the ITS-90 temperature scale. Work is in progress to improve the accuracy at higher temperatures by comparing acoustic and microwave resonances. The Competence project on Johnson Noise Thermometry, a further effort to develop new, practical temperature standards, has progressed beyond experimental design to the first prototype stage.

The division has collaborated with an ultradry gas manufacturer to demonstrate excellent agreement between atmospheric pressure ionization mass spectrometry and the division’s cavity ring-down

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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spectrometer (CRDS), measuring less than 10 ppb water vapor as produced by the division’s Low Dew Point generator. A commercial version of CRDS for water vapor measurement at low parts-per-billion levels, a metric required by U.S. industry, is being evaluated by the group in collaboration with the manufacturer.

The division is also developing Evanescent Wave Cavity Ring-down Spectrometry as a diagnostic technique for remote sensing of chemicals. Tests with a broad-spectral-range light source have allowed measurement of water and trichloroethylene. The importance of this technology is indicated by the division’s collaborations in this area with industry, national laboratories, and academia.

A new NIST Competence project on molecular electronics focuses on developing metrology to measure electrical properties of newly conceived molecular circuitry and appropriately aims at establishing metrologies for this new area of study. Another NIST competence project is dedicated to the rapidly expanding field of microfluidics needed in “lab-on-a-chip” applications and is presently measuring flow profiles before addressing sensing approaches. This resonates with the trend of chem-bio, biomedical, and analytical chemistry technologies. The division should lend its standard-setting and fundamental measurement science abilities to this rapidly growing field.

The division has developed three tools pertinent to plasma etch monitoring: radio frequency (RF) waveform analysis; planar, laser-induced fluorescence (PLIF); and neutral mass spectrometry. Analysis of RF as an indicator of plasma state has matured to a level at which the panel encourages testing on plasma etch tools used in semiconductor manufacturing. The division has demonstrated expertise in PLIF, which can provide a spatial map of both ground-state CF and CF2 radicals in a plasma. The division should maintain plasma measurements of the neutral species, using mass spectrometry as a complementary measurement tool for plasma processes.

The division has achieved a detection level in the <1 ppm range using chemical microsensors utilizing MEMs microhotplate technology. This is sufficient sensitivity for detecting many chemical agents without preconcentration, as sought by the Defense Threat Reduction Agency. The division has successfully leveraged its microhotplate as a tool to explore catalytic, doped-metal-oxide, matrix, and thermal cycling approaches to trace gas detection. It has also established strong ties with customers, as evidenced by OA contracts and CRADAs. The panel cannot assess whether the metal-oxide/catalytic hotplate sensor is going to be sensitive and stable enough for the detection of all chemical agents but is impressed by the initiative taken in the division to work on this topic. To make gas sensors viable, the panel believes that a demonstration of stability and sensitivity should be early goals of the effort.

Program Relevance and Effectiveness

The panel is especially pleased with the effort made this year by the Thermal and Reactive Processes Group to contact semiconductor and tool manufacturers to identify metal and dielectric deposition process areas in need of modeling research. Contacts with semiconductor manufacturers identified atomic-layer deposition, plasma-enhanced chemical vapor deposition (CVD), and thermal CVD modeling and measurements for advanced integrated circuit (IC) interconnects as areas in which the division has expertise and equipment to address fundamental issues. The result of this outreach is a redirection of research within this group to metal-organic thermal CVD. Research will investigate the mechanism involved in CVD of metallic thin films. The panel looks forward to further feedback from industry participants on the progress of this work.

The division is continuing its dialog with manufacturers of semiconductor gas mass flow controllers. These companies use the thermophysical property data on reactive process gases to enable more accurate flow-rate calibration. As new data are obtained on these reactive gases, the preliminary results

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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are posted on the Web with conservative uncertainties until final values are published. This makes rare data immediately available to the user community.

Making at least some of the division’s databases freely available on the Internet boosts NIST’s image in and appreciation from the technical community. It could also spur innovation and trade. The panel recommends continuing this effort. The panel commends the CSTL for providing unfettered access to the gas and liquid property data needed by the semiconductor industry. These databases might be usefully extended to include fluid property data needs for other sectors. Such a proactive approach will add to NIST’s relevance to industry and further its contact and connections with U.S. industry. The panel also commends the division for maintaining a Web page with division results and accomplishments.

The division provides primary calibration of gauges and sensors used for temperature, humidity, pressure, and flow measurements over a wide range of operating parameters. The principal customers of this service are secondary calibration laboratories and industrial users who want fast, low-cost calibrations. The appropriate focus for the division’s calibrations remains high accuracy, including in many cases information feedback on the design or condition of the gauge. The panel encourages continued efforts to automate these primary calibration services and consideration of the viability of lower-cost calibrations, where practical, to help free staff time for the evaluation and analysis rather than using it for data taking.

The division’s work in the measurement of the basic thermophysical properties of gases generates and updates fundamental properties, such as speed of sound, heat capacity, density (equation of state), and viscosity, for a variety of gases needed by the semiconductor industry. Such data enable the prediction of calibration factors for mass flow controllers and for improvement of modeling used for CVD. These data fill an important need in the semiconductor and high-technology industries. Physical properties of hazardous gases heretofore unavailable, with uncertainty ranges of 0.01 to 0.5 percent, are being systematically measured, and preliminary data are being made freely available on the Internet and eventually included in NIST’s physical property data publication series.

The panel encourages the division to benchmark activities as a way to measure performance and progress in pertinent areas. The panel would like to see indicators such as numbers of journal publications, citations of previous work, patents, CRADAs, Web site hits, and other measures of information creation, use, and transfer. Numbers do not tell the whole story of the effectiveness of NIST research, but comparisons of trends over the years can reveal migration of modes of information transfer and can aid researchers and management in evaluating their effectiveness.

Division Resources

Funding sources for the Process Measurements Division are shown in Table 4.3. As of January 2002, staffing for the division included 59 full-time permanent positions, of which 54 were for technical professionals. There were also 15 nonpermanent or supplemental personnel, such as postdoctoral research associates and temporary or part-time workers.

The panel commends the division for its retention rate for postdoctoral researchers over the past 5 years. Retention of postdoctoral fellows provides one good source of qualified researchers to fill permanent CSTL staff positions. The panel would like to encourage the division to perform more benchmarking of its personnel efforts—for example, examining turnover at CSTL compared with that at other government laboratories.

The current economic downturn might provide a special opportunity for NIST to develop further industrial connections. Because many companies that normally operate within the field of use targeted by NIST have surplus employees and yet may not want to lose those well-trained employees perma-

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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TABLE 4.3 Sources of Funding for the Process Measurements Division (in millions of dollars), FY 1999 to FY 2002

Source of Funding

Fiscal Year 1999 (actual)

Fiscal Year 2000 (actual)

Fiscal Year 2001 (actual)

Fiscal Year 2002 (estimated)

NIST-STRS, excluding Competence

7.9

8.7

8.7

8.6

Competence

0.8

0.9

1.0

1.1

ATP

0.4

0.5

0.7

0.3

OA/NFG/CRADA

0.8

1.0

1.6

2.7

Other Reimbursable

1.2

1.1

1.1

0.8

Total

11.1

12.3

13.1

13.5

Full-time permanent staff (total)a

59

57

58

59

NOTE: Sources of funding are as described in the note accompanying Table 4.1.

aThe number of full-time permanent staff is as of January of that fiscal year.

nently, the division might utilize an industrial sabbatical program, following the example of its present academic sabbatical program. In such a program, companies might detail employees to NIST while paying a portion of their salary. NIST would pay the balance of the salary and would gain by the insight and viewpoint provided by these industrial partners and through use of their expertise for NIST projects.

Surface and Microanalysis Science Division

Technical Merit

According to division documentation, the mission of the Surface and Microanalysis Science Division is to serve as the nation’s reference laboratory for chemical metrology research, standards, and data to characterize the spatial and temporal distribution of chemical species and to improve the accuracy, precision, sensitivity, selectivity, and applicability of surface, microanalysis, and advanced isotope measurement techniques. The current mission statement does clearly and concisely define the division’s current role and responsibilities within the CSTL and NIST.

The Surface and Microanalysis Science Division is organized in four technical groups: Atmospheric Chemistry, Microanalysis Research, Surface and Interface Research, and Analytical Microscopy. In addition to the personnel in these groups, the division staff includes two active and one emeritus NIST fellows. The fellows pursue very active research programs and provide mentoring and technical guidance to younger staff across division organizational boundaries. The division is fortunate to have its programs supported by these fellows, productive scientists who are internationally recognized as leaders in their fields.

Several changes were made to division organization in 2001. First, leadership of the Analytical Microscopy Group changed; the former group leader returned to work as a researcher, and another staff member assumed the leadership role. The panel compliments the division on enabling both individuals to fulfill career aspirations and allowing a smooth transfer of responsibility. Second, the Surface and

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

Interface Research Group, previously called the Surface Dynamical Processes Group, underwent a name change in order to reflect more accurately its current and planned activities.

The organization of the Surface and Microanalysis Science Division has generally enabled the division to respond effectively to the need for programmatic evolution while maintaining logical groupings of expertise by analytical method or class. Technical activities are organized at the CSTL and NIST program level, allowing many opportunities for collaboration across CSTL and NIST. Currently, division projects are aligned in support of CSTL’s 12 programs and play a central role in four: Semiconductor Metrology, Nanotechnology, Chemical Characterization of Materials, and Environmental Measurements. In 2002, the division will be deeply involved in CSTL’s newly defined programs in Biomaterials, Environmental Technology and Systems, Industrial and Analytical Instruments and Services, Microelectronics, and Emerging Technologies.

The technical programs in the Surface and Microanalysis Science Division are of very high quality. Staff continue to receive recognition for their work within NIST and from the larger scientific community and are much sought after as speakers at major international technical symposia, conferences, and workshops. The following section of the report discusses program highlights and issues relating to the projects under way in each of the division’s four groups.

The Surface and Interface Research Group, formerly the Surface Dynamical Processes Group, conducts theoretical and experimental research into chemical processes at surfaces and interfaces. As with its name, the focus of this group has and will continue to evolve and change. In the past, the group focused almost exclusively on the development and application of molecular spectroscopy to surface reactions; now it is beginning to broaden its work to include the development and use of other surface-sensitive and high-spatial-resolution probes such as near-field scanning optical microscopy (NSOM), atomic force microscopy (AFM) of soft surfaces, and conductance-based scanned probes. The evolving emphasis in this group on the development of novel tools is especially commendable. The group maintains its position as an international leader in sum frequency generation optical spectroscopy (SFG-OS) of surfaces and buried interfaces. The leader of the SFG-OS project received the Department of Commerce Bronze Medal in 2002 in recognition of his seminal efforts in this area.

In FY 2001, the group ended research into reactions of radicals at surfaces. The group performed fundamental measurements of the interactions of ground-state (3P) and electronically excited (1D) oxygen radicals with fused silica. This is a system of strong interest to the semiconductor and biomaterials industries, as oxygen radicals are the key reactive species in oxygen plasma reactors used for resist ashing and surface cleaning in semiconductors processing, and in polymer surface modification for biocompatibility in biomaterials. Fused silica is used for plasma containment, and it is important that the reaction models be known in order to help plasma scientists predict species lifetime and reactivity. It is unfortunate that this important research has been discontinued. The panel suggests that the division establish contact with plasma reactor companies to determine whether the research can be continued with outside resources.

The Surface and Interface Research Group is participating in two new CSTL FY 2001 competence programs: (1) Molecular Electronics and (2) Polymeric Thin Films: A Test Bed for Combinatorial Methods. A primary component of the Molecular Electronics program focuses on new, two-photon and conductance-based scanned probes. The secondary component focuses on ultrafast SFG-OS and theoretical studies of electron dynamics. In the Polymeric Thin Films program, the group will contribute to the development of novel instrumentation for hyperspectral imaging and rapid sample analysis, including nanoscale optical probes for analysis at various wavelengths (ultraviolet [UV], infrared [IR], and microwave). The group has assembled and tested a scanning confocal microscope. The application of these tools to polymeric films, and particularly to rapid sample screening, is noteworthy.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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The Surface and Interface Research Group continues its development of nonlinear optical probes and their application to surfaces and buried interfaces, which is of note because these techniques can serve as in situ probes capable of real-time monitoring of processes at the molecular scale. Two National Research Council postdoctoral fellows have worked to take vibrationally resonant SFG-OS past proof-of-principle and into important practical application by studying the formation kinetics of self-assembled monolayers. This method is being applied to study the chemistry of copper electrodeposition in situ.

Members of the Surface and Interface Research Group were recognized by the 2001 CSTL Technical Achievement Award for their paper describing an exciting advancement in ultrahigh-resolution analysis of materials.3 It is applicable to many industrial-relevant systems, including polymer film and semiconductor surfaces.

The Microanalysis Research Group performs research at and beyond the state of the art in techniques for electron and x-ray beam microanalysis applied to understanding the chemical, morphological, and crystallographic properties of materials. The group’s goal is to improve the analytical resolution, sensitivity, accuracy, and precision of measurements made with scanning electron microscopy, electron microprobe analysis, analytical electron microscopy, scanning Auger electron spectroscopy, x-ray fluorescence, and x-ray photoelectron spectroscopy. Members of this group are some of the most influential scientists in their fields; their work is of outstanding quality.

The Microanalysis Research Group continues to pioneer new spectrometers for x-ray microanalysis. Researchers are using x-ray microcalorimeter detectors developed by EEEL in Boulder, Colorado, to study the fundamentals of low-energy x-ray line generation (e.g., L, M, and N lines of medium to high atomic number materials). Data on the absolute energy position and relative line intensities are scarce but are essential to accurate qualitative and quantitative microanalysis. This group’s researchers are uniquely and appropriately situated to advance this work. It will have impact on every industrial and academic group that uses energy dispersive and wavelength dispersive x-ray spectrometry—which takes in nearly every high-tech industry and university in the United States. Many workers in the semiconductor industry are anxiously awaiting commercialization of these microcalorimeter detectors and will shortly thereafter be seeking accurate low-energy x-ray line information. The Microanalysis Research Group is also furthering the commercialization of a new, high-throughput x-ray detector, the low-energy silicon drift detector. The panel believes that this work epitomizes what NIST should be doing—both developing new instruments to enhance metrology and performing measurements for standards.

Researchers in the Microanalysis Research Group are exploring the use of fractal analysis of particle shapes for automatic classification. The work in this area is highly interesting and important to many industries (for example, automotive and semiconductor) and to government agencies (such as the Environmental Protection Agency [EPA] and DOD) that must characterize or identify particles and their sources. The group is approaching this research with sound fundamental principles. The panel recommends that the activity be focused to address first an understanding of the critical parameters of more standard particles, such as those available commercially or through NIST. Ultimately, the goal should be to provide a software tool kit for individuals to use in particle identification. The panel recommends discussions with industry researchers responsible for generating particle-classification algorithms; this will help the group avoid repeating industry’s efforts. The panel encourages the division to continue the

3  

Michaels et al., “Scanning Near-field Infrared Microscopy and Spectroscopy with a Broadband Laser Source,” J. Appl. Physics 88(8):4832-4839, 2000.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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development of such software tools on PC-compatible platforms for easy dissemination to potential customers.

The panel recognizes the quality and relevance of the work that this group is performing in understanding the fundamental science behind measurements of films using cross-sectional transmission electron microscopy (TEM). High-resolution TEM is often used to measure gate dielectric thickness during process development in the semiconductor industry. As films approach monolayers of thickness, accurate understanding of measurement errors and proper measurement methods are essential. This group’s careful research has resulted in new models for building virtual gate dielectric stacks that can then be compared with experimental data for error analysis. The panel encourages the continuation and completion of this work, as it will help scientists at industrial laboratories provide more accurate measurements to semiconductor process development engineers, resulting in higher device yields and performance.

The panel encourages the Microanalysis Research Group to accelerate its focus on measurements of the surface and bulk of silicon-germanium (SiGe) films and substrates, especially with high spatial resolution. The panel recognizes the expertise that this group has in TEM, x-ray spectroscopy, and grazing incidence x-ray photoemission spectroscopy (GIXPS) that is being explored for application to this material system. High-performance microprocessor manufacturers such as Intel, IBM, and Advanced Micro Devices (AMD) are increasingly adopting SiGe substrates and films. Lack of adequate measurement methods is preventing wider adoption of these materials; wider adoption by domestic semiconductor manufacturers would give them a competitive edge in this important market. The panel also encourages the division to continue to expand efforts in high lateral resolution chemical and elemental mapping and characterization of surfaces and interfaces, including the development of new instrumentation and analytical methods. The panel encourages collaboration with other divisions outside of CSTL on these efforts.

The Atmospheric Chemistry Group continues to focus on carbon isotope metrology and on elemental/organic splits in the carbon content of airborne particulate samples. The most confounding aspect of air quality associated with particulate matter continues to be discrimination of the myriad of emission sources responsible for airborne particulate carbonaceous material. The Atmospheric Chemistry Group has appropriately identified two key needs that clearly fall within the NIST mission: SRMs of quantified particulate mixtures from known emission sources, and chemical methods (both physical measurements and data analysis) to profile and distinguish different types of emission sources from atmospheric samples. During the past year, the group has focused on three categories of activity consistent with the high-relevance elements identified in its mission:

  1. Providing reference materials to enhance the accuracy and precision of chemical measurements used for compliance with asbestos and air quality regulations. The group’s careful, systematic, and arduous asbestos research is an example of valuable and unique national service consistent with the core NIST mission. The panel recognizes the high quality of expertise applied to produce SRMs for critical certifications of asbestos measurements. In addition, the group released one new standard reference material—SRM 2784, Urban Dust—and four reference materials. However, in the broader mission beyond asbestos measurements, personnel limits prevent the group from moving to research with higher payoffs to address the critical need for reference materials representing mixtures of known and quantified particulate emission sources.

  2. Providing an analysis of the sensitivity of artifacts in the thermal-optical measurement of elemental/organic carbon ratios to chemical speciation and physical properties of an airborne sample

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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and to temperature-ramp protocols used in the measurement process. This information could provide insights to highlight significant reliability concerns with this commonly used technique. It also might raise awareness of the consequent large uncertainties in emission-source apportionments that are based on its use. The rate of progress on this effort is compromised, however, by personnel limitations.

  1. Applying analytical methods to assist specific clients where reliable and conveniently available technical competence is required. Examples include developing a reference protocol to measure gas mask leakage, and application of radiochemical measurements to carbon-date particulate samples from the EPA air quality field studies. These client-oriented projects are executed with competence.

The panel notes that the Atmospheric Chemistry Group has not aggressively pursued novel techniques for isotopic profiling of emission sources, a goal highlighted last year, because of personnel limitations.

The Analytical Microscopy Group conducts research on the chemical and structural properties of matter using ion- and photon-based microscopies. This includes understanding fundamental aspects of the excitation process, quantitation methods, standards development, and commercial instrumentation improvements. This group continues to be a premier source of research and applications for methods such as secondary ion mass spectrometry, laser Raman microprobe, and Fourier transform infrared microprobe. The group’s work on the development of new SRMs for dopant profiling is essential for the semiconductor industry, and NIST researchers are viewed as the international leaders in this field. The panel encourages this work and looks forward to the release next year of the SRM 2133, phosphorus implant in silicon. The panel repeats its suggestion to develop other dopant profile standards of value to industry, such as boron, arsenic, and phosphorus in common metal silicides. The panel was impressed by the SIMS instrumentation that is undergoing installation in this group’s laboratories and looks forward to seeing results from these instruments in next year’s review. In other work, the group is taking a leading role in the investigations of how to perform very shallow depth profiling using time-of-flight SIMS and is developing cluster-ion SIMS techniques that will allow the composition of “soft” surfaces such as biomaterials and polymers to be characterized. The panel looks forward to seeing this work extended to practical materials in the future.

Homeland security has long been a focus of the research of the Analytical Microscopy Group. In past reviews, the panel has commended the high-quality work that this group has done in developing methods for analyzing particles in support of international nuclear safeguarding. The panel recognizes this year’s work to apply autoradiography in order to increase and improve uranium particle sampling throughput by pre-selection. More recent work on developing methods for calibrating gas masks has been performed in collaboration with researchers in the Analytical Chemistry Division and in the Fire Research Division of the Building and Fire Research Laboratory. This interesting activity will continue in FY 2002 and should result in new methods for testing the efficacy of gas masks in the field using particle aerosols. Finally, the division has been assisting in the development of trace explosives detection portals (TDEP) as a method of screening airline passengers for explosives and drugs. The group’s unique knowledge of high-accuracy and high-throughput methods for analyzing particle composition makes it appropriately positioned to drive new methods and standards for accurate screening for security threats. The group’s work on the application of cluster-ion SIMS to studying known explosives will provide TDEP manufacturers with new ways of distinguishing harmful materials from the large background of benign organics.

In collaboration with the Process Measurements and Analytical Chemistry Divisions, the Analytical Microscopy Group released a new series of standards for Raman spectroscopy. This technique, widely

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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used for the characterization of materials, has lacked a comprehensive set of standards. This work by NIST will enable researchers and instrument manufacturers to have more accurate quantitative information for compositional analysis.

Finally, the panel would like to recognize the extraordinarily high technical quality of the work of the division’s two active NIST fellows. One is the internationally recognized expert in the generation and emission of electrons from solid surfaces under x-ray and electron-beam irradiation. This was tangibly recognized by the outside scientific community in FY 2001 with the American Vacuum Society’s Albert Nerken Award. This fellow’s work is essential to the accurate interpretation and quantitation of x-ray photoelectron and Auger electron spectroscopies (XPS and AES, respectively). Research projects under his direction in FY 2001 have produced key databases or updates: SRD 20 on X-Ray Photoelectron Spectroscopy released version 3.1 in April 2001, and SRD 82 on Electron Effective Attenuation Lengths released version 1.0 in September 2001. He is also active in encouraging young researchers inside and outside of NIST to continue and expand the work in this field. The second fellow is one of the leading researchers in electron microprobe analysis, pioneering the application of new x-ray detector technology on traditional platforms such as high-vacuum, high accelerating voltage SEMs as well as new instrumentation such as variable pressure and low accelerating voltage systems. He has been the driving force behind the implementation of microcalorimeter x-ray detectors on SEMs for small particle analysis; this work is helping to meet an essential need of the semiconductor and other industries dependent upon understanding the composition of extremely small features.

Program Relevance and Effectiveness

The Surface and Microanalysis Science Division uses a variety of methods to ensure the relevance and effectiveness of its programs. It is mapping key activities to the NIST Strategic Focus Areas. For example, nanotechnology is supported by the division’s project on cluster-ion SIMS for high-resolution depth profiling, the Competence program on molecular electronics, and overall general chemical imaging. Support of homeland defense has been an integral part of the division for many years, with projects in forensic particle analysis, quality assurance and control methods for the U.S. Atomic Energy Detection System (USAEDS), gas mask standards, and analysis of explosives particles. The division has new activities in support of health care, including monitoring boron neutron capture chemotherapy using SIMS analysis of tissue samples, drug delivery using nonlinear optical spectroscopy, and nanoscale analysis of compounds of pharmaceutical interest using near-field scanning optical microscopy. The panel recommends that the division perform periodic, perhaps annual, formal comparison of its activities with those occurring in other CSTL divisions, other NIST laboratories, and appropriate domestic universities to ensure that the work is complementary, not overlapping.

Researchers visited or met with many different corporations in FY 2001 to consult on measurement methods, discuss potential collaborations, and gain insight into new work areas. Division researchers interacted with various industries, including the following: chemical (Dow, DuPont, Visteon, PPG); consumer products (Proctor & Gamble); aerospace (General Electric); semiconductor (AMD, Agere, Cirent, KLA-Tencor, SEMATECH); and analytical instrumentation (Noran, Gatan, Photon Imaging, X-ray Optical Systems). CRADAs and consortia are currently in place on combinatorial methods and polymer characterization.

In order for the division to further enhance the effectiveness and relevance of its work, the panel repeats its recommendation that a sincere effort be undertaken to encourage staff members to utilize the NIST Industry Fellows Program. This division plays an important role in providing standard methods and materials to U.S. industry, but most NIST researchers do not have a personal understanding of the

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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challenges faced by their customers. While interactions in professional societies and conferences and visits by industrial customers provide a limited perspective, nothing can replace having NIST researchers spend even short periods of time at a customer site. The panel recognizes that utilizing the Industry Fellows Program is not always easy, but by being flexible in assignment duration, rewarding researchers for their participation, and setting specific division and CSTL goals for success, the program can be used more successfully. Industry utilizes such programs; CSTL can do so as well.

The division is very visible both nationally and internationally. The professional staff publishes its work extensively in prestigious scientific journals (80 publications in FY 2001); organizes and sponsors conferences and workshops (7 in FY 2001); and presents at major conferences, often as invited speakers (94 presentations in FY 2001). Staff members produce and maintain Web-distributed databases that are widely used by a variety of technical communities. SRD 20 (X-Ray Photoelectron Spectroscopy Database) alone produces more than 30,000 hits per month! The panel commends the division for greatly improving the accessibility and appearance of its Web site.

The ongoing division programs are also clearly focused on the needs of NIST’s customers in other government agencies. Staff meet regularly with their colleagues in organizations such as EPA, DOD, and the U.S. Department of the Treasury to ensure that the division has the input it needs to fulfill the part of its mission directed toward supporting national security and the environment. Specifics of program relevance and the mechanisms that the division uses to stay aware of customer needs are discussed below.

The panel is pleased to see that the division staff have thought about how to meet customer needs for well-characterized materials that can substitute for completely characterized SRMs during the long (3 to 7 year) SRM development period. The new intercomparison materials (IM) project will allow the division and CSTL to respond more quickly to customer needs. Examples of IMs that might have strong impact include additional implant materials (boron, arsenic, and phosphorous in SiGe or silicides), particles, thin films (dielectrics on silicon), and real dust samples.

The division has shown the ability to stop work when a project fulfills the requirements of its customers or lacks further driving force. Examples of the former are the work on electron microprobe homogeneity standards and the generation of index of refraction standards; examples of the latter are synchrotron-based measurements of nitrided gate dielectrics. And the division can change the direction of a project when required to do so by its customers: future software development for image processing using lispix (a public domain image analysis program) and the desktop spectrum analyzer are being converted from Macintosh to PC platforms. More information and data are being distributed in electronic format using Web sites instead of being sent as individual copies. This maximizes the impact and effectiveness of dissemination of the division’s research results. The panel recommends that the division continue to evaluate the full scope of its program in order to stay focused on highest-priority work.

The activities of the Atmospheric Chemistry Group have provided information that is clearly relevant to regulators seeking to formulate air quality strategies and to establish compliance with air quality and emissions standards. Because its expertise is complementary to the broad spectrum of atmospheric aerosol measurements, it is critically important that a group focused exclusively on atmospheric chemistry collaborate within the community of atmospheric scientists to have significant impact. The Atmospheric Chemistry Group continues to make progress in this regard through collaboration with EPA on the development and application of measurement techniques and calibrations.

The panel recognizes the Atmospheric Chemistry Group’s effort over the past year to identify an environmentally relevant research agenda within its reach and to build to critical mass. In September 2001, the Workshop on Atmospheric Measures and Standards: Improving the Scientific Base for Informed Decisions on Atmospheric Issues was organized and hosted by the division. Attendees were

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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TABLE 4.4 Sources of Funding for the Surface and Microanalysis Science Division (in millions of dollars), FY 1999 to FY 2002

Source of Funding

Fiscal Year 1999 (actual)

Fiscal Year 2000 (actual)

Fiscal Year 2001 (actual)

Fiscal Year 2002 (estimated)

NIST-STRS, excluding Competence

4.6

4.7

5.3

5.3

Competence

0.4

0.4

0.2

0.2

ATP

0.4

0.3

0.3

0.2

Measurement Services (SRM production)

0.1

0.1

0.0

0.1

OA/NFG/CRADA

2.9

5.7

5.1

3.7

Other Reimbursable

0.3

0.3

0.2

0.1

Total

8.7

11.5

11.1

9.6

Full-time permanent staff (total)a

36

36

36

38

NOTE: Sources of funding are as described in the note accompanying Table 4.1.

aThe number of full-time permanent staff is as of January of that fiscal year.

solicited from key government agencies (National Oceanic and Atmospheric Administration [NOAA], EPA, Tennessee Valley Authority), industry (Ford Motor Company, ExxonMobil, Northrop Grumman Corporation), universities, and other interested organizations. Key gaps in measurement technology and standards were identified, but no action plan has yet been developed.

Division Resources

Funding sources for the Surface and Microanalysis Science Division are shown in Table 4.4. As of January 2002, staffing for the division included 38 full-time permanent positions, of which 35 were for technical professionals. There were also 8 nonpermanent or supplemental personnel, such as postdoctoral research associates and temporary or part-time workers.

The division’s operational budget has remained essentially flat over this time period. The increase observed in FY 2000 and FY 2001 was due to one-time grants for major equipment from the division’s other agency (OA) funding sources.

The quality of the personnel in the Surface and Microanalysis Science Division continues to be outstanding. In general, the staff think that the work they do is important and interesting and that it contributes to fulfilling the NIST mission; the morale is high throughout most of the division. In particular, the younger members of the staff believe that they are an important part of NIST. They appreciate the active mentoring they receive from more-senior division scientists.

Although the quality of people is extremely high, there do not appear to be enough technical staff members to fully exploit the capabilities of their equipment and the needs of the division’s customers. For example, it appears that the work on radical reactions with surfaces did not end from a lack of customer need but because of the disappearance of key research personnel. The relatively flat budgets experienced by the division, and by NIST as a whole, over the past several years have made it difficult to bring in new staff. However, it is young scientists, hired now, who are needed to lay the foundation

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

that will enable the division to continue to turn out high-quality technical results with an impact on industry and the U.S. public. While the panel is particularly impressed by the enthusiasm and qualifications of the younger people currently on staff, the division must continually freshen its mix of personnel. Turnover is very low, mainly occurring because of retirements, but limited resources make it a challenge for division management to bring in necessary new hires. Only one new technical professional was hired in the division this year, and the division will probably lose two promising postdoctoral researchers at the end of their terms in FY 2002 because appropriate openings on staff are not available. The division, CSTL, and NIST run the risk of losing fresh ideas and future technical leaders if they cannot find a method to continually update the staff.

In addition to not being able to retain new, young staff members, the division has not hired any new support staff in the past several years. There are no dedicated Web programmers, electronics specialists, machinists, or equipment maintenance specialists. In such a situation, there are two possible consequences: (1) important tasks will not be completed, or (2) the professional staff will be forced to take time away from their primary project-oriented duties to carry out key support tasks. Web programming falls into the first category; the panel commends the division for significantly improving its Web site during the past year but knows that this was done by existing technical professionals at the expense of their regular research work. Caring for laboratory instruments falls into the second category; routine equipment maintenance is being done by technical professionals who should be focused on new ways to use the equipment instead of on how to keep the equipment going. The panel once again encourages division and laboratory management to consider acquiring dedicated support staff for the purpose of ensuring that key tasks get done and that technical staff can operate with maximum productivity.

The morale of the Atmospheric Chemistry Group is suffering under the uncertainty of its future technical direction. The panel is very concerned that the staffing resources of this group are not sufficient to effectively execute an environmentally significant research agenda, despite an effort over the past year to identify a research agenda within the group’s reach. This is not a new concern; it has been raised in the last two reviews. In light of the complementary analytical strength of the other groups within the Surface and Microanalysis Science Division, the panel sees an opportunity for the division to achieve its environmental objectives by blending the people and key research objectives of the Atmospheric Chemistry Group into the other three groups within the division. For example, within the framework of CSTL’s focus on environmental issues (FY 2001: Environmental Measurements; FY 2002: Environmental Technologies), group members might enhance research directed at the chemical speciation of single particles within samples having high particle-numbers and also enhance research on the complementary algorithms for data analysis. The development of those techniques to resolve individual particle information in airborne samples could provide critical new information to resolve emission sources of airborne particulate samples. With the opportunity to leverage expertise and resources in the complementary groups within the Surface and Microanalysis Science Division, critical mass for sustained progress might be attained. Other corrective action plans undoubtedly merit consideration as well, but the panel is confident in its conclusion that laboratory and division management must address the issues of the size and focus of this group, either by giving it the resources and direction to succeed, or by reorganizing the critical activities into other CSTL groups.

In general, the division’s instrumentation resources adequately support the technical programs. Capital equipment needs are carefully analyzed, and instruments are acquired in a systematic and timely fashion. OA funding is used to acquire major pieces of equipment such as the new, dynamic SIMS instrument and the x-ray photoelectron and Auger electron spectrometer; these tools are then leveraged across many research efforts. As a result, the division has a unique collection of state-of-the-art instrumentation, especially in electron microscopy, secondary ion mass spectrometry, near-field probes, and laser/surface probes.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

The lack of a state-of-the-art focused ion beam (FIB) sample preparation system remains a noticeable gap in the division’s resources. As discussed in last year’s report, FIB technology remains an essential technique for cross-section and thin-section preparation of samples to be used in scanning electron and transmission electron microscopy. It is increasingly used in manufacturing processes for thin-film heads on disk drives and in MEMS structures. Unfortunately, little is known about the mechanisms involved in the high-energy (>30 keV) ion sputtering used in FIB, and the potentially negative impact of these mechanisms on sample composition and structure is not known. NIST is ideally situated to pioneer this research, and the panel again encourages the division to quickly build a coalition to acquire a commercial FIB system and, just as importantly, the required human resources to perform research in FIB sample preparation methods and materials modification applications. If action is not taken in the next fiscal year, NIST runs the risk of missing the opportunity of meeting an important need of U.S. industry. The panel suggests that alternative methods of funding—including collaborations with ion beam research groups outside of NIST but in the local area (for example, at UMD)—be explored to bring in equipment and people in a timely manner.

Physical and Chemical Properties Division

Technical Merit

According to division documentation, the mission of the Physical and Chemical Properties Division is to serve as the nation’s reference laboratory for measurements, standards, data, and models in the areas of thermophysics, thermochemistry, and chemical kinetics. The division consists of six groups— three at Gaithersburg (Computational Chemistry, Experimental Kinetics and Thermodynamics, and Chemical Reference Data and Modeling) and three at Boulder (Experimental Properties of Fluids, Theory and Modeling of Fluids, and Cryogenic Technologies). Additionally, three independent projects are located at Boulder—the Thermodynamics Research Center, Membrane Science and Technology, and Properties for Process Separations.

The programs of this division comply with the primary NIST mission to promote U.S. economic growth by working with industry to develop and apply technology, measurements, and standards. Each group in the division has ties to appropriate industries, and the division as a whole maintains a desirable balance between the programs that support shorter-term industrial needs and the research that will allow NIST to fulfill longer-term national science and technology requirements. Excellent balance also exists between experimental and theoretical expertise in the research programs. The division conducts work of unsurpassed quality in fundamental measurements of thermophysical and thermochemical properties. A key factor contributing to the value of the division’s work is its outstanding researchers. Selected highlights of these programs are presented below.

The panel commends the Physical and Chemical Properties Division for its excellent balance between experimental and theoretical expertise in all areas of its research program. The panel notes particularly the continued emphasis on maintaining the unique experimental capabilities of the division. This is important, as experimental work continues to be deemphasized throughout the thermodynamics community, as reported in NIST Special Publication 975.4

4  

U.S. Department of Commerce, Technology Administration, National Institute of Standards and Technology, Report on Forum 2000: Fluid Properties for New Technologies—Connecting Virtual Design with Physical Reality, NIST Special Publication 975, National Institute of Standards and Technology, Gaithersburg, Md., 2002.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

The Computational Chemistry Group has made excellent progress since it was founded in 1997. The group aims to provide computational chemistry-related data, benchmarks, and validation of methods to U.S. industry and academic researchers. A Virtual Measurement System is being explored for chemical kinetics that will allow accurate prediction of rate constants, including estimates of uncertainties, using theoretical methods. The results of these calculations are compared with experimental data provided by the Experimental Kinetics and Thermodynamics Group. The panel commends the syner-gism between these groups. Significant progress has been made in the past year in improving the understanding of proton tunneling. Research into isopotential searching to predict paths of unknown reactions has progressed to alpha testing in industry and academia. This technique has identified a potential new path for the decomposition of the explosive RDX, which suggests new strategies for detecting concealed quantities of this compound (a homeland security initiative). An excellent example of the pivotal role that the Computational Chemistry Group can play is the Fluid Properties Simulation Challenge that the group has helped organize over the past year. Participants from industrial and academic research laboratories studying molecular modeling and simulation exchanged ideas in a June 2001 NIST workshop on how to create a set of problems related to fluid properties in order to stimulate research on validating predictive molecular simulations. The contest to solve these problems is currently under way and will conclude in the fall of 2002.

The Experimental Kinetics and Thermodynamics Group provides reliable kinetic and thermodynamic data pertaining to industrial processes, environmental chemistry, energy efficiency, and fire suppression. Studies of the physical properties of ionic liquids and measurement of rate constants of fundamental chemical reactions in these liquids are under way. Ionic liquids are nonvolatile, nonflam-mable, recyclable solvents for polar and nonpolar compounds. They have been proposed as “green” solvents.) The division’s research will provide essential data required to develop industrial processes exploiting the unique properties of ionic liquids. The division has initiated an examination of the chemical kinetics and mechanisms of combustion of real fuel mixtures instead of simple, one-compo-nent surrogates. This will provide information critical to an understanding of the generation of toxic pollutants and particulates in practical fuel mixtures. Rate constants for the reaction of OH with halogenated organics of atmospheric importance have been measured with unprecedented accuracy, providing new insights into reaction mechanisms, rigorous tests of kinetics theory, and tests of ab initio calculations by the Computational Chemistry Group. The division’s Web-based Chemical Kinetics Database (http://kinetics.nist.gov) continues in beta testing. Targeted evaluations of selected rate constants for chlorination chemistry and data related to small hydrocarbon radical chemistry have been added to the database this year. The panel applauds the division’s efforts on this database, which is critical to the more efficient design of industrial chemical processes. However, the kinetic rate constants in the database have not been updated since mid-2000 because of the lack of funds. This database should be a high priority for the division, and it is important to fund the work necessary to complete the full public release and to maintain an up-to-date database.

The Chemical Reference Data and Modeling Group, which compiles, evaluates, correlates, and disseminates Standard Reference Data, has had another productive year. It released the seventh edition of the NIST Chemistry WebBook (http://webbook.nist.gov). In FY 2001, the number of chemicals included in the WebBook increased by 11 percent to more than 40,000, and a subset of the Thermodynamics Research Center (TRC) data was added. The WebBook is accessed by 10,000 to 20,000 users per week, of whom 50 percent are return users, demonstrating the value of this tool. The division has begun work with academic and industrial partners to provide direct machine access to WebBook data using computer programs that reside on a user’s machine.

The division has completed evaluation of 57,000 mass spectra received since the last release (1998)

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

of the NIST Mass Spectral Database for gas chromatography (GC)/mass spectrometry (MS) analyses, and a new release is planned for 2002. This analysis tool has enormous practical application in industry. The NIST Automated Mass Spectral Deconvolution and Identification Software (AMDIS) is also of great value in general analytical chemistry, particularly in the detection of chemical weapons. This makes implementation of the international Chemical Weapons Treaty easier and more effective technically. The panel also applauds the initiation of cross-divisional efforts with the Analytical Chemistry Division to devise mass spectral methods for the detection of biological weapons, providing support for the NIST homeland security strategic focus area.

The Properties for Process Separations project provides critically evaluated data and models for industrially important processes including distillation, adsorption, and supercritical fluid extraction. Gas chromatographic techniques developed in this project were recently applied to the study of natural gas odorant adsorption on surrogate soil surfaces. These data show that sulfide odorants are more likely to be adsorbed (fade) than are mercaptan odorants. This finding has significant implications for pipeline leaks below ground level. The kinetics of the hydrolysis of carbonyl sulfide to hydrogen sulfide have been measured in a multiyear study. A key finding is that the reaction rate to H2S is very slow at typical temperatures, and thus hydrolysis of carbonyl sulfide is an unlikely route to fugitive H2S in liquid petroleum gas. This project has led to the development of a new patented apparatus. The project’s new initiative to use in situ Fourier-transform infrared (FTIR) spectroscopy to collect vapor-liquid equilibria data, particularly on mixtures that are reactive, corrosive, or toxic, is in the laboratory testing phase. Data on this class of difficult mixtures will be measured at temperatures to 450 K and pressures to 20 MPa.

The Theory and Modeling of Fluids Group provides model-based correlations and predictions, evaluated standard reference data, data on water and aqueous systems, and computer simulation of solid-fluid equilibrium. The group made significant progress in ab initio quantum mechanical routes to technologically important properties of gas-water mixtures. These data are needed for many applications, such as the engineering design of combustion turbines. Work on water-argon systems and systems of the other noble gases is complete. The project’s focus will now shift to water-nitrogen and water-hydrogen. The group completed an important study on aircraft fuel tank safety. The study produced detailed liquid-vapor phase equilibria on Jet-A fuel through the use of a Peng-Robinson equation-of-state in an extended corresponding state method. This work is part of a collaboration with the Building and Fire Research Laboratory that aims to recommend improved regulations for the inerting of fuel tank vapor spaces, venting requirements, and jet fuel formulations.

The Membrane Science and Technology project provides significant resources for industries that seek more efficient chemical and pharmaceutical separations and waste-reduction processes through membrane technologies. This year, a researcher developed a new apparatus to continue the study of high-throughput membrane transport, funded through the NIST Advanced Technology Program. This enhanced apparatus uses sensitive in-line fluorescence detectors and a fiber-optic multiplexer to provide in situ analysis of eight samples simultaneously. The high-throughput work is relevant for efforts to measure fundamental diffusion and solubility data and to elucidate transport mechanisms. Further work has also been done on data measurement systems for pressure-driven membrane separations. The panel is concerned, however, that the division is unable to maintain a critical mass of staff for the project.

The Experimental Properties of Fluids Group measures high-accuracy, comprehensive thermophysical and transport property data on pure fluids and mixtures using state-of-the-art, and often unique, laboratory apparatus. This group collaborates particularly closely with the Theory and Modeling of Fluids Group on projects related to alternative refrigerants and natural gas technology. A significant example of this collaboration is the completion and imminent release of the refrigerant properties database, REFPROP7 (http://www.nist.gov/srd/nist23.htm). This database update incorporates new

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

measured data and an enhanced user interface with higher-speed calculations. The group continues work on enhancing its measurement capabilities by completing the installation of a double-sinker densimeter to measure liquids and dense gases, particularly replacement refrigerants. This unique apparatus will provide primary standard density data by reference to a silicon standard. During the past year, the group completed measurements on the heat capacity of refrigerant R125 near the liquid-vapor critical point, and pressure-density-temperature data for R410A refrigerant blend. These data will facilitate the development of new refrigerant systems that can be used under extreme conditions without major losses in capacity and efficiency.

Significant and rapid progress in restoring full and improved operations in the Thermodynamics Research Center was made during the past year after its transfer to NIST Boulder in mid-2000. A major new initiative was completed with the establishment of the TRC Data Entry Facility. This facility, which uses new, interactive Guided Data-Entry software, ensures that all relevant experimental data are captured and added to the TRC SOURCE data file. In addition, a new Data Quality Program has been designed to control source data quality at all stages of data entry, evaluation, and database management. More than 850,000 numerical values on 16,400 chemical substances, 9,000 mixtures, and 3,800 reaction systems are available in the TRC SOURCE database. These data will be used to support relevant NIST and CSTL missions. The panel is impressed with this rapid and efficient transition and now looks forward to efforts to integrate the TRC’s staff and projects with the other data collection and evaluation activities of the division.

The Cryogenic Technologies Group conducts research to help commercial firms and government agencies develop and improve technologies for the $10 billion cryogenic process and product industry. Databases, laboratory measurements, cryogenic process models, and technology transfer are the key elements of this program. A significant recent advance is the use of photo-etching to create the flow channels in a miniaturized parallel plate heat exchanger. This will facilitate fundamental studies in cryogenic heat transfer.

Program Relevance and Effectiveness

The panel is pleased by the Physical and Chemical Properties Division’s efforts to ensure that its programs are relevant to the needs of its customers. The division employs a variety of mechanisms to gather input on current and planned divisional activities, particularly encouraging suggestions and requests from external organizations. Division personnel interact with people from other institutions at standards committee meetings, technical conferences, road-mapping activities, professional society and committee meetings, and trade organization events. Staff take lead roles in organizing many of these gatherings and often hold them at NIST. For example, in FY 2001, the division organized the 5th International Conference on Chemical Kinetics, the International Association for the Properties of Water and Steam Annual Meeting, and a Workshop on Predicting the Thermophysical Properties of Fluids by Molecular Simulation. Division personnel have informative relationships with guest researchers and collaborators from industry and universities.

The division’s programs have an impact on a wide array of industries and research communities. Programs often bridge the gap between the short-range research goals of industry and the long-range, open-ended inquiries commonly pursued in universities. Staff awards demonstrate the value placed on the division’s work. In FY 2001, a staff member received two NASA Group Achievement Awards for the development of the Earth Science Research Strategy and for contributions to the 1999/2001 Stratospheric Aerosol and Gas Experiment III Ozone Loss and Validation Experiment. Another staff member received the Robert Vance Award from the Cryogenic Society of America for advancements in

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

the field of cryogenics. The division’s products include databases that scientists use to develop computational models and analytical techniques for industrial, environmental, and fundamental chemistry applications. The panel commends the division not only for gathering, evaluating, and maintaining the information necessary to produce these databases, but also for performing critical experiments and computations in areas such as gas- and liquid-phase kinetics, thermodynamics, mass spectrometry, and fluid properties in order to produce data and the underlying understanding that allow the division to make high-quality information readily available to technical communities.

The division’s work also has significant impact in international standards activities. Division staff are active in a number of organizations working on alternative refrigerant standards, including the International Energy Agency, the International Union of Pure and Applied Chemistry, and the International Organization for Standardization. In addition to data-based products and committee activities, the division provides unique standards and services regarding fluid flow under cryogenic conditions.

The Physical and Chemical Properties Division makes strong and well-directed efforts to convey its research results to the relevant scientific and engineering communities. It effectively utilizes basic tools such as publications and presentations. In FY 2001, division staff published 158 papers, primarily in peer-reviewed journals; made 135 presentations (22 invited) at scientific meetings; and served on 67 national and international scientific committees. The extent of the division’s reach into relevant communities can be seen in several other statistics. The Chemistry WebBook was visited from more than 350,000 unique Internet addresses last year (an increase of 40 percent). Roughly one-half of all GC/MS instruments sold worldwide include the Mass Spectral Database; 2,500 copies of this database are sold annually. The 5th International Conference on Chemical Kinetics organized and hosted by the division attracted 150 participants from 13 countries spanning the globe. The division’s unique Workshop on Predicting the Thermophysical Properties of Fluids by Molecular Simulation—goals of the workshop were to identify prediction needs that could be satisfied by molecular simulation and to drive research to ensure that simulation will be a relevant tool in the long term—was attended by 42 persons from industry and academic institutions. The impact of division research is felt in a variety of ways by different research disciplines, but overall, NIST plays a major role in the cross-fertilization of many fields and in integrating the results for the benefit of industrial users throughout the world.

Because of their high reliability, the advanced pulse tube refrigerators developed in the Cryogenic Technologies Group are used across a wide spectrum of applications, from radio astronomy to superconducting electronics and superconducting motors. This reliability results from the complete absence of moving parts such as pumps and compressors. The interest in this technology is evidenced by the large number of awards, invited or plenary lectures, and short courses given by the group’s staff. More than 29 cryogenic companies have been customers of the group through consultations and CRADAs.

The panel looks for continued improvement in Web access to the products produced by the Physical and Chemical Properties Division. Coordinated access to the data in the Chemistry WebBook and the TRC database should be a goal, as acknowledged by the division. The panel recommends investigating ways to significantly expand the type of data available through the Chemistry WebBook (e.g., to include mixture data) using TRC resources. In addition, the panel strongly recommends that the division addresses the issue of cost recovery for databases in general, possibly through a subscription mode for full access to the data via the Web.

Division Resources

Funding sources for the Physical and Chemical Properties Division are shown in Table 4.5. As of January 2002, staffing for the division included 55 full-time permanent positions, of which 46 were for

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

TABLE 4.5 Sources of Funding for the Physical and Chemical Properties Division (in millions of dollars), FY 1999 to FY 2002

Source of Funding

Fiscal Year 1999 (actual)

Fiscal Year 2000 (actual)

Fiscal Year 2001 (actual)

Fiscal Year 2002 (estimated)

NIST-STRS, excluding Competence

9.1

8.7

6.9

7.0

Competence

0.1

0.0

0.0

0.0

ATP

0.4

0.4

0.6

0.7

OA/NFG/CRADA

3.5

2.9

2.8

3.2

Other Reimbursable

0.3

0.3

2.6

2.4

Total

13.4

12.3

12.9

13.3

Full-time permanent staff (total)a

65

64

56

55

NOTE: Sources of funding are as described in the note accompanying Table 4.1.

aThe number of full-time permanent staff is as of January of that fiscal year. The drop in staff between FY 2000 and FY 2001 resulted from the move of the Fluid Science Group to the Process Measurements Division.

technical professionals. There were also 19 nonpermanent or supplemental personnel, such as postdoctoral research associates and temporary or part-time workers.

The division’s STRS resources are basically flat, which requires division management to obtain additional resources from other sources or to terminate projects and reallocate existing resources to ensure the impact of remaining programs. Either approach has the potential to affect the quality of the division’s work negatively. The percentage of the division’s funding received from other government agencies was 22 percent in FY 2001, essentially unchanged from FY 2000. The current level is high enough to demonstrate that the division’s work is relevant to external parties. A significant fraction (15 percent) of the current funding arises from sales of the Mass Spectral Database. About 90 percent of the revenue from these sales is returned to the division to maintain this important database. Other divisional products are provided to customers free of charge over the Web, including the Chemistry WebBook and the Chemical Kinetics Database. The panel notes that the information in these databases is critical to many scientists, and NIST might consider imposing a user fee for access, especially since the resources to support the project are limited. In particular, funds for support of the Chemical Kinetics Database are so tight that the database cannot be kept current, as discussed earlier. Users might welcome paying a fee in order to guarantee that the databases are current and provide increasingly useful features.

The staff in Gaithersburg and Boulder are a key asset of the Physical and Chemical Properties Division. Many examples of significant individual accomplishments by staff attest to the high quality of the team. One staff member was elected a fellow of the American Physical Society for outstanding contributions toward improved understanding of structural and dynamic properties of simple and complex liquids. Two others received the 2001 Russell B. Scott Award for the best paper presented at the Cryogenic Engineering/International Cryogenic Materials Conference. NIST-wide awards (the Jacob Rabinow Applied Research Award and the Judson French Award) and a Department of Commerce Bronze Medal were also conferred on division members. Division personnel are lead editors of two major journals (International Journal of Chemical Kinetics and International Journal of Thermophysics),

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
×

and associate editors of 14 other publications. These awards and positions of responsibility demonstrate the regard in which division staff are held by their peers in the scientific and industrial communities.

Despite major improvements, serious issues remain within the Boulder facilities. Building 24 lacks an elevator to provide access to the second floor where most of the division space is located. The only access other than by the stairway is via a forklift. The division states that an elevator is “on the site master plan but is at least a year or two away.” The panel believes that the installation of elevators must be moved to the highest priority in order to meet current access standards in both Building 24 and Building 2. The heating, ventilation, and air-conditioning system in Building 24 is not adequate for laboratory ventilation or temperature control, and no plans are in place for improvement. A plan should be developed immediately to ensure the interim safety of workers in the chemical laboratories and to bring the laboratories up to currently accepted standards.

Staff in Gaithersburg appear satisfied with their physical facilities, although the panel continues to have concerns as noted in the FY 2001 report. As acknowledged by the division, in some laboratories air cleanliness, dust control, and air filtration are still insufficient; the quality, capacity, and reliability of the power supply are still problematic; and the exhaust and ventilation systems are still inadequate. While the current quality of the Gaithersburg facilities is generally comparable with that at research universities, these deficiencies will eventually interfere with the division’s ability to perform the type of high-precision experiments that are needed to supply industrial and academic researchers with the accurate, high-quality data that are the division’s hallmark. The panel urges that a detailed plan be developed for improvement of division facilities.

No capital equipment funding issues appear to be limiting the initiatives undertaken by division scientists in Gaithersburg or Boulder. In fact, some of the apparatus in the division are not even available in industrial laboratories.

The division’s research is split equally between the Boulder and Gaithersburg sites. The panel is particularly pleased with the concerted effort made during the past year to familiarize personnel at each site with the research carried out at the other. This has involved regular intradivision seminars held by teleconference and visits between sites. Close coordination is required to maximize research effectiveness within the division, and the panel commends this effort. With the retirement of the current division chief, CSTL management should consider the structure of the division and the effect of the geographical split on the coordination and efficacy of division research programs.

Analytical Chemistry Division

Technical Merit

The Analytical Chemistry Division states its mission as serving the nation’s premier reference laboratory for chemical measurements and standards to enhance U.S. industry’s productivity and competitiveness, assure equity in trade, and provide quality assurance for chemical measurements used for assessing and improving public health, safety, and the environment. The division maintains world-class core competencies in analytical mass spectrometry, analytical separation science, atomic and molecular spectroscopy, chemical sensing technology, classical and electroanalytical methods, gas metrology, nuclear analytical methods, and microanalytical technologies. These core competencies reside in five groups: Spectrochemical Methods, Organic Analytical Methods, Gas Metrology and Classical Methods, Molecular Spectrometry and Microfluidic Methods, and Nuclear Methods.

During FY 2001, division staff members won several awards, most notably, two LabAutomation

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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Conference Poster Awards, an IR-100 Award, and an award for Distinguished Service in the Advancement of Analytical Chemistry by the American Chemical Society.

The Molecular Spectrometry and Microfluidic Methods Group demonstrates a high degree of technical expertise applied to a wide range of meaningful programs relevant to molecular spectroscopy and technology associated with microfluidic devices. In all of the programs, there appears to be a concerted effort to employ cutting-edge technology, but at the same time, there is a notable willingness to look outside NIST for collaboration and support when it is necessary. The quality of the technical effort is validated by the high level of acceptance of the products and the publication and dissemination of information in leading peer-reviewed journals. In FY 2001, the group filed five new patent applications. In addition, during the year, two new patents were issued to the group.

The Molecular Spectroscopy and Microfluidic Methods Group has demonstrated its productivity and innovation with its work on design and applications of plastic microfluidics systems. The decision to concentrate effort on polymer-based substrates is laudable, and the progress made in characterizing fluid flow and temperature measurement in the microstructures is most impressive. This area alone resulted in eight peer-reviewed papers in FY 2001. An important element of this group’s success has been its willingness and ability to interact with other groups within CSTL and NIST.

The Spectrochemical Methods Group conducts research involving the development, critical evaluation, and application of methods for the identification and measurement of inorganic chemical species using optical, mass, and x-ray spectrometries. The instrumentation capabilities of this group include inductively coupled plasma (ICP) and thermal ionization mass spectrometers, wavelength and energy dispersive x-ray spectrometers, ICP optical emission spectrometers, and a glow discharge optical emission spectrometer.

The most significant development from the Spectrochemical Methods Group in FY 2001 was a comprehensive method for the accurate determination of mercury in a wide variety of materials. The new, cold vapor isotope dilution inductively coupled plasma mass spectrometry (CV-ID-ICP-MS) methodology is a relatively straightforward, but highly versatile, approach for elemental mercury determinations. The technique is built on the combination of this group’s expertise in ID-MS as a benchmark method, ICP-MS detection power, and well-known cold vapor generation methods. This very important development was acknowledged by Research and Development magazine’s 2001 R&D 100 award. Seven NIST SRMs for coal have been certified for their mercury content by this method. This methodology has also been incorporated at the NIST Hollings Marine Laboratory in Charleston, South Carolina, where it will be an important tool in the archiving of marine specimens.

The group has extended the ID-ICP-MS method to determinations of iodine. Iodine deficiency has been noted as a major problem by the World Health Organization. Unfortunately, few reference materials exist for iodide content in body fluids. The use of ID-ICP-MS has allowed the certification of iodide content in SRM 2670a Toxic Elements in Freeze-Dried Urine. Future work will implement the same procedure for determinations in blood serum. A number of otherwise-difficult determinations were performed employing high-resolution (HR) ICP-MS and ICP-MS operating under so-called cold plasma conditions. In collaboration with the Organic Analytical Methods Group, HR-ICP-MS was employed as an element-specific detector for iron speciation studies in body fluids. Because 56Fe is the most abundant isotope of iron, the presence of isobaric interferences is problematic for sensitive detection. In the case of ICP-MS, the large abundance of ArO+ at 56 daltons is a perennial problem. The resolving power of the Finnigan Element HR-ICP-MS allows these determinations to be made without the presence of the ArO+ background. Cold plasma conditions are a useful means of drastically reducing the contributions of Ar-related ions to ICP-MS spectra. Specifically, cold plasma operation

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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allows sensitive determinations of Ca and K, which are usually not accessible at all due to the suite of Ar isotopes in the same mass region. Measurements of Ca and K have been performed on reference materials in support of the National Reference System for the Clinical Laboratory Program.

The Spectrochemical Methods Group is working to certify a new, silica-on-filter reference material. Crystalline silica inhalation is a major health risk in the mining and construction industries worldwide, but the lack of reference materials is a major hindrance to implementation of more stringent standards and their enforcement. The group is working with the Occupational Safety and Health Administration, the National Institute for Occupational Safety and Health, and the Mine Safety and Health Administration to develop an SRM that is appropriate for instrumentation calibration. Sample preparation methods have been evaluated for both ICP optical emission spectroscopy and ICP-MS. The production and certification of the SRM is scheduled for FY 2002.

Research activities in the Nuclear Methods Group are focused on the science supporting the identification and quantification of chemical species by nuclear analytical techniques. Current research activities involve the full suite of nuclear analytical techniques, including instrumental and radiochemical neutron activation analysis (INAA and RNAA), prompt gamma-ray activation analysis (PGAA), and neutron depth profiling (NDP). In addition, the group is developing analytical applications of neutron-focusing technology. The measurement capabilities that reside within this group provide an excellent complement to those in the Spectrochemical Methods Group in that they depend on characteristics of the nucleus of the element rather than on the electron shells probed in spectrochemical techniques, and therefore are insensitive to the chemical state. Nuclear analytical methods are also nondestructive and do not require sample dissolution. The Nuclear Methods Group may be underutilized relative to its capabilities to provide an independent assay for work throughout the division.

INAA and RNAA are powerful reference techniques that have been used at NIST for many years. The instrumentation and methodologies have continued to evolve, providing increased sensitivity, specificity, precision, and accuracy. To that end, the Nuclear Methods Group has characterized the sources of error and imprecision to a very high degree of certainty. The group is putting particular effort into establishing the position of nuclear methods as primary methods of measurement. This requires a complete uncertainty statement written in terms of SI units, meaning that each step in the sample handling and each component of the measurement system must be characterized. In principle, a primary method is one in which analysis is possible without using a standard. Such methods are powerful tools in novel materials characterization and a vital component in the NIST SRM certification program.

INAA methods are now paying particular benefits in the characterization of sample homogeneity in small analytical specimens. Many analytical techniques employed for elemental analysis are based on the use of small sample quantities (i.e., 1 mg) in the solid form. These samples are then put into solution. In such situations, the degree of representation that the specimen has for the bulk of the sample comes into question. This is also true for Standard Reference Materials where elemental certification is based on the use of 100- to 500-mg quantities. To be truly valid for real-world situations, SRMs must be certified on the size scales to which they are applied. Taking advantage of the sensitivity and nondestructive nature of INAA, the use of this technique for homogeneity studies of small samples has been evaluated and implemented for the determining sampling characteristics for a number of environmental SRMs. The minimal analytical uncertainty associated with INAA allows extraction of the variability that is due to the material inhomogeneity from the observed total variability within a given set of measurements. This very important characteristic will be a valuable contribution to the certification of SRM 2783, Urban Air Particulate Matter on Filter. This particular SRM is the primary SRM for EPA’s National Air Quality Program.

The capabilities of the Nuclear Methods Group in the areas of PGAA and NDP are of particular

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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importance to U.S. industry and other government agencies. The capabilities are enabled by the NIST’s Cold Neutron National Users Facility. PGAA provides unique information for analysis of light elements, particularly hydrogen. Nondestructive, matrix-independent measurements of hydrogen in diverse materials such as Nafion (ionomer) membranes used for fuel cells and in fundamental studies of embrittlement in metals and alloys are very important applications. PGAA is also used to advantage in a wide variety of polymers and refractory materials such as zeolites, for which sample dissolution for analysis is not an option. A wide range of elements, including lanthanides, can be determined in these matrices as well. Important instrumentation improvements now permit the focusing of the cold neutron beams down to 100 µm × 100 µm spot sizes for laterally resolved measurements. Depth-resolved analyses are possible using the NDP methodology for determinations in specialty materials. For example, in collaboration with the Army Research Laboratory, the group determined the percentage of boron in tungsten alloys, and a collaboration with Advanced Micro Devices used NDP for the analysis of boron in silicon matrices. The technique has also been used to determine the long-term stability of primary boron and lithium standards.

Research in the Organic Analytical Methods Group is directed toward the development, critical evaluation, and application of methods for the identification and measurement of organic and organometallic species using mass spectrometry and analytical separation techniques. These separation techniques include gas chromatography (GC), liquid chromatography (LC), supercritical fluid chromatography (SFC) and extraction (SFE), capillary electrophoresis (CE), and capillary electrochromatography (CEC).

Acquisition of an LC/MS/MS instrument during the past year increased the Organic Analytical Methods Group’s capabilities for the determination of analytes of health, nutritional, forensic, and environmental importance, as well as for structural studies of natural products. A matrix-assisted laser desorption time-of-flight mass spectrometer (MALDI-TOF) system was obtained to characterize biomolecules. This instrument was acquired with support from the Defense Threat Reduction Agency in order to begin development of protocols for generation of mass spectra from bacteria. The combination of proteins produced by one species of bacteria differs from that of another. The MALDI-TOF system is used to generate a mass spectrum from the bacterial proteins to permit the identification of bacteria much faster than is now done by conventional approaches. This will be applicable to counterterrorism activities as well as to food safety. The MALDI-TOF system will also be used to characterize health status protein markers and proteins expressed by genetic modification of foods.

The Organic Analytical Methods Group’s research in separation science continues to focus on investigations of the physical and chemical processes that influence sample retention in LC, GC, SFC, CE, and CEC. Results from these fundamental studies are used to design stationary phases tailored to solve specific separation and analysis problems and to assist in method development and optimization. Recently, the group explored a novel approach to the synthesis of LC stationary phases based on polymer immobilization. Polyethylene acrylic acid copolymers were immobilized on silica as an alternative to conventional silane surface modification chemistry. The resulting columns were evaluated for the LC separation of carotenoid isomers, and preliminary results indicate exceptional selectivity for this class of compounds. Research in chiral separations is continuing in several areas, using LC, CE, and GC. The determination of chiral drug species in hair samples using LC may permit environmental exposure to be distinguished from illicit use. In other studies, functionalized cyclodextrins have been evaluated as chiral selectors in CE. A capillary electrophoresis method with indirect detection was used to characterize the patterns of sulfate substitution of these materials. The selectors were then investigated as chiral additives in capillary electrophoresis. These studies emphasize the importance of the use of well-characterized selectors for reproducible results in chiral CE.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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Research in organometallic speciation has continued, with improvements in the GC-atomic emission detection (AED) method for methylmercury and alkyltin species. The new approach involved derivatization and a solid phase microextraction step to concentrate the analytes prior to GC-AED analysis. This approach has been used to provide several SRMs for methylmercury in marine tissue. This same general approach has been used to measure butyltin species in several of the sediment-matrix SRMs. It should be emphasized that methods developed for heavy metal speciation are of key importance to directed work taking place in the Hollings Marine Laboratory.

Research activities within the Gas Metrology and Classical Methods Group are focused on gas metrology, classical wet chemical methods (gravimetry and titrimetry), coulometry, ion chromatography, and maintaining the theoretical infrastructure for pH and conductivity measurements.

Program Relevance and Effectiveness

The Analytical Chemistry Division provides traceability of chemical measurements used in programs of national and international importance through Standard Reference Materials, NIST-Traceable Reference Materials (NTRMs), Measurement Quality Assurance Programs in critical areas, and comparisons of NIST chemical measurement capabilities and standards with those of other national measurement institutes. The division strives to ensure that the projects undertaken are responsive to the metrology needs of its customers, which include national and international industry, basic research communities, and other government agencies. It has been actively seeking out its customers, leading other metrology agencies, and fostering international partnerships. Examples demonstrating program relevance and effectiveness follow.

Increased requirements for quality systems documentation for trade and for effective decision making regarding the health and safety of the U.S. population have increased the need for demonstrating “traceability to NIST” and establishing a more formal means for documenting measurement comparability with standards laboratories of other nations and regions. During the past year, the division quantified more than 140 SRMs to address such needs. The division contributed to certifying 686 of the 1,400 NIST SRM chemical standards, and providing from storage >16,000 of the 32,000 NIST SRM units sold in FY 2001. The NIST-Traceable Reference Materials Program addresses the need for reference materials with well-defined linkage to national standards. An NTRM is a commercially produced reference material with a well-defined traceability linkage to existing NIST standards for chemical measurements. Eleven specialty gas companies worked with NIST to certify more than 8,500 NTRM cylinders of gas mixtures that have been used to produce more than 500,000 NIST-traceable gas standards for end users with a market value of approximately $110 million. Thirty-six NTRMs were value-assigned for four specialty gas companies during FY 2001.

International agreements and decisions concerning trade and social well-being are increasingly based on mutual recognition of measurements and tests between nations. The division has taken a leadership role in the International Committee of Weights and Measures-Consultative Committee on the Quantity of Material (CCQM) and the Chemical Metrology Working Group of the Inter-American System for Metrology (SIM). The CCQM has formed seven working groups responsible for selecting and overseeing the operation of key comparisons that address chemical measurement-related issues important for international trade and for environmental, health, and safety-related decision making. The Analytical Chemistry Division is leading activities within five of the seven working groups. During FY 2001, the division participated in 25 CCQM comparison studies, serving as pilot laboratory in 13 of them. During the past year, six intercomparison exercises were developed to assess the proficiency of SIM NMI’s and their designated collaborators for addressing chemical measurement problems within

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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their regions and in the Americas. The Analytical Chemistry Division has established agreements with the Chemical Metrology Working Group leaders to allow non-CCQM member countries within SIM to participate in such studies. Division members are working within the framework of the Cooperation in International Traceability in Analytical Chemistry to establish practical, metrologically sound, vertical traceability links between the NMIs and chemical testing laboratories in various countries and regions around the world.

The division provides chemical measurement quality assurance services in support of other federal and state government agency programs. During the past year, the division conducted 25 projects with 11 federal and state government agencies. Division members had technical interactions that involve laboratory research and measurement activities with more than 20 professional organizations and societies, including the American Industry/Government Emissions Research consortium (AIGER), the American Association for Clinical Chemistry, the American Society for Testing and Materials, the Certified Reference Materials Manufacturers Association, the National Food Processors Association, the National Council on Clinical Chemistry, and the National Environmental Laboratory Accreditation Council.

The Molecular Spectrometry and Microfluidic Methods Group has several programs and projects directed at providing standards for spectroscopy. An essential program involving cooperation between the three NMIs of the North American Metrology Organization (NORAMET) (Canada, United States, and Mexico) is based on the production of holium oxide solution reference materials for wavelength calibration in molecular absorption spectrometry. Another project seeks to develop a fluorescein solution fluorescence standard for use in flow cytometers, fluorimeters, fluorescence microchip readers, and other similar instruments. A new SRM (SRM 2241) provides a relative intensity standard for Raman spectroscopy using 785-nm excitation. This SRM will provide the analytical Raman community with practical methods to standardize spectral data. Another spectroscopy standardization effort has been directed at providing ultraviolet (UV), visible (VIS), and near-infrared (NIR) wavelength standards for transmission measurements. The aim of these standards is to provide SRMs intended for verification and calibration of spectrophotometers operating in the transmission mode. The development of these new standards, especially those for fluorescence measurement, is laudable.

The Molecular Spectrometry and Microfluidic Methods Group has provided the spectroscopy community with a new product, SpectroML, that is an extensible markup language for molecular spectroscopy data. This is a Web-based mechanism for interchanging UV and VIS spectral data generated on different spectrophotometers. The effort is well supported by industry and key professional committees.

The Molecular Spectrometry and Microfluidic Methods Group has carried out research on and developed standards supporting forensic measurements of gunshot residue. The aim of this project is to provide a gunpowder reference material for quality assurance in the detection and characterization of explosives. The project is relevant to the NIST homeland security SFA and should prove extremely valuable.

The Spectrochemical Methods Group was very active in international standards activities during the past year. The group participated in five pilot and key comparisons of the Inorganic Working Group of the CCQM. The specific projects were (1) CCQM K-13, cadmium and lead content in sediment; (2) CCQM P-12, lead in wine; (3) CCQM P-26, sulfur in fuel; (4) CCQM P-14, calcium in serum; and (5) CCQM P-29, cadmium in rice. This group has taken significant leadership positions in many other international interactions, reflecting the high esteem in which it is held by the community.

The Organic Analytical Methods Group’s research activities in organic mass spectrometry have focused on the development of techniques for characterization and quantitative determination of proteins in biological matrices. Levels of specific proteins and other biomolecules in blood are indicative

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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of certain disease; measurement of these health-status markers can permit more rapid diagnosis of disease with greater certainty than is possible by other methods. The United States spends $1.1 trillion per year on health care, approximately 15 percent of which is attributed to diagnostic measurements. Thus, the development of appropriate standards is of key consequence in economic and health-related matters. The group’s priorities for SRM and measurement method development have been established by valuable consultation with numerous professional and government agencies. The technical impact of this work has been to provide a sound basis for the standards required by the diagnostic industry. The economic impact of these standards will come from the major role they will play in assuring the quality of health care measures and providing U.S.-based companies with the capacity to meet new European Union regulations. SRMs include glucose in human serum, drugs of abuse in hair, and troponin. Twelve health-status markers have been identified as the highest priorities for immediate studies. This year’s research efforts have been directed toward the development of reference methods for troponin I (a new marker of myocardial infarction), thyroxine (a marker for thyroid function), cortisol (a marker for endocrine function), speciated iron (how iron is associated with proteins is important for elevated or low iron levels), homocysteine (a risk factor for myocardial infarction), folic acid (an essential nutrient that reduces the risks of heart disease and neural tube defects), and prostate-specific antigen (a marker for prostate cancer). To this end, an interlaboratory comparison exercise of candidate troponin I reference materials was carried out in collaboration with the Troponin Subcommittee of the American Association of Clinical Chemists. Ten troponin I materials were evaluated by 13 manufacturers of immunoassays.

The Association of Official Analytical Chemists International has developed a nine-sectored triangle in which foods are positioned on the basis of their fat, protein, and carbohydrate content. NIST has been working with other government agencies and the food industry over the past several years to provide an increased array of SRMs to cover each sector, with values assigned for proximates (procedurally defined values for fat, protein, carbohydrate, and so on), fatty acids, cholesterol, vitamins, elements of nutritional interest, and so on. Concentration values in the food-matrix SRMs are assigned on the basis of a combination of measurements from NIST and interlaboratory comparison exercises involving approximately 20 member laboratories of the National Food Processors Association’s Food Industry Analytical Chemists Subcommittee. SRMs for numerous analytes have been completed using chocolate, fish tissue, spinach, and peanut butter matrices.

The Gas Metrology and Classical Methods Group continues to be very active internationally in pH measurements. In FY 2001, it participated in a pH key comparison (CCQM-K17) and a phthalate buffer (pH 4.0) comparison and assisted the pilot laboratory of the German NMI in preparing the solutions for these comparisons. The group completed a SIM pilot study on pH (SIM QM-P4) with 16 participating laboratories in South America, Mexico, and the Caribbean. Members have continued to be active in IUPAC commission V.5, completing revisions to the pH document that will define the traceability of pH to the Bates-Guggenheim convention, thus ensuring continued traceability of pH to sound thermodynamic principles.

In collaboration with EPA and the remote-sensing community, the Gas Metrology and Classical Methods Group developed a quantitative database of infrared spectra. This database is required for establishing remote IR-based technology as a reliable tool for real-time monitoring of airborne chemical contaminants along plant boundaries and within plant facilities. Because the spectra are being prepared using NIST primary gas standards, well-defined traceability to NIST can be established for any subsequent field measurements. These spectra will be specified for use by industry in the new update of EPA method TO-16. At the present time, the group has released data for 40 compounds. The group is active in international ozone measurement activity, and it completed the upgrade of the EPA Standard Refer-

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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ence Photometer (SRP) network with new electronics. Many countries have expressed interest in receiving an SRP to provide traceability in ozone measurements, and Portugal, Spain, BIPM, and Brazil have ordered SRPs. Because of the strain this program places on resources, the division has agreed to transfer of the responsibility for world traceability for ozone to the BIPM in Paris, France.

The Analytical Chemistry Division promotes U.S. industry through the development of high-priority standards and through standards organizations such as ASTM. Over the past 2 years, the division developed the capability to produce low-concentration nitric oxide gas standards. These standards are required by the automotive industry in new-car development and for meeting new regulations in California, and they are needed by industry to meet new regulations covering stack gas emissions. This research has resulted in two new, nitric oxide gas SRMs, one at 0.5 ppm (SRM 2737) and one at 1.0 ppm (SRM 2738).

In July 2001, a meeting was held at NIST with representatives from AIGER to discuss research and standards needs to support emissions testing for the next generation of automobiles. AIGER is composed of the California Air Resources Board, the EPA, and automobile industry representatives (DaimlerChrysler, Ford, General Motors).

Division management recognizes the changing demand for new SRMs and the need for advanced technologies to support the growing materials, biotechnology, and semiconductor industries as the U.S. and global economy improves. These complex commercial reference standards require an increase in effort from the Analytical Chemistry Division that can come about only by forming partnerships, as the Gas Metrology and Classical Methods Group has done with the NTRMs, or by selective postdoctoral hiring, or encouraging long-term guest researchers (from other agencies or from industry) and aggressively seeking increased external funding. In today’s highly commercial environment, technical success must be tied to and directly quantified in terms of 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 an impact argument needs to be developed by the researcher and to be widely publicized to best gain recognition from funding sources.

The panel finds that the division has not adequately addressed its Web site and overall Internet presence to the level needed for the appropriate global impact of its results on information exchange. The division indicated that, owing to lack of manpower and common software tools, and its perception of the value-added aspect of this task at this time, little to no added effort was put forth in FY 2001. The panel restates its recommendation that the division consider how best to apply current Web capabilities, until such time as a common software/Web protocol can be provided, to meet the needs of global technology and information transfer.

The programs within the Analytical Chemistry Division are critical to quantifying the value of international commerce via the SRM and NTRM standards. This laboratory is a national asset in terms of both the technical capability that it applies within the United States and internationally and its substantial impact on U.S. commerce. On the basis of this review, the panel sees the division as being highly effective in the means it uses to conduct and communicate its results to customers on a global basis, although tangible acknowledgment of the NIST impact by U.S. industry is disproportionally low.

Resources

Funding sources for the Analytical Chemistry Division are shown in Table 4.6. As of January 2002, staffing for the division included 67 full-time permanent positions, of which 61 were for technical

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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TABLE 4.6 Sources of Funding for the Analytical Chemistry Division (in millions of dollars), FY 1999 to FY 2002

Source of Funding

Fiscal Year 1999 (actual)

Fiscal Year 2000 (actual)

Fiscal Year 2001 (actual)

Fiscal Year 2002 (estimated)

NIST-STRS, excluding Competence

8.5

8.4

8.6

9.0

Competence

0.3

0.3

0.3

0.4

ATP

0.1

0.1

0.3

0.5

Measurement Services (SRM production)

2.2

2.2

1.6

1.6

OA/NFG/CRADA

2.0

2.4

2.9

3.0

Other Reimbursable

1.5

1.5

1.7

1.6

Total

14.6

14.9

15.4

16.1

Full-time permanent staff (total)a

66

68

69

67

NOTE: Sources of funding are as described in the note accompanying Table 4.1.

aThe number of full-time permanent staff is as of January of that fiscal year.

professionals. There were also 25 nonpermanent or supplemental personnel, such as postdoctoral research associates and temporary or part-time workers.

The current division technical staff is a responsive group of interactive teams 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. As previously noted, recognition of staff scientists by peers outside NIST is high, as evidenced by awards to division members.

To utilize its limited resources better and to enhance staff satisfaction, the panel recommends that the division establish and encourage technical training and cross-training on its many analytical systems. This goal might be accomplished through a mentoring program or by self-help programs that are rewarded with added levels of responsibility. The division should foster and proactively manage interactions between the varied disciplines within NIST to form new dynamic work teams. Different technologists can see a problem from completely different angles, resulting in the use of alternative techniques that may produce cheaper, faster, or better results.

The division should also use recognition and rewards to openly acknowledge technical and administrative contributions to the organization at all levels. Such recognition would enhance the perception that management cares about how things are done, not just about what is done.

Division leadership should seek new ways to communicate to all staff, including that of involving all of the team as part of the project planning process. Gaining all of the staff’s input and acceptance of program objectives, budget limitations, and milestones is the motivation. This can result in higher staff morale. The technical staff voiced concern that a disconnect exists between the information that management thinks it is sharing and the information that the technical staff receives and acts upon. Communication both up and down the ladder when budget reduction, performance enhancement, and direction are being questioned may help bring teams together for a win-win outcome.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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Given the resource restraints under which the division has had to operate for the past few years, the staff and management have made great sacrifices to balance competing needs for operations, infrastructure improvements, and metrology development activities. Nearly every scientist is involved in SRM development and certification. The challenge for leadership is how to find the funds to grow or maintain essential technologies for the development of new SRMs, the division’s key product. The impact of reduced resources (people, equipment, and funds) is taking a toll on the staff and on their ability to respond to a broader range of commercial SRM needs. The division should more often critically assess the opportunities to delete programs and SRMs so that greater emphasis can be placed on priority projects.

To continue to provide the state-of-the-art SRMs and metrology techniques required by U.S. industry, division staff must have access to modern analytical instrumentation comparable to that used by the laboratories of their industrial contemporaries. A more aggressive procurement plan for analytical instrumentation should be developed and implemented. Key to this plan would be a time line and a listing of alternative sources (e.g., customer cost-share) of funding for the purchase of instrumentation. The panel noted shortcomings in novel instrumentation developments or the use of the most modern commercially available instrumentation in many groups. The lack of collision-cell ICP-MS instrumentation and updated gas chromatographs are examples. The panel suggests that the division leadership act upon next-generation instrumentation needs for metrology research. Novel instrumentation beyond what is commercially available is needed for leading-edge problem solving in metrology.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 2002. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002. Washington, DC: The National Academies Press. doi: 10.17226/10510.
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This assessment of the technical quality and relevance of the programs of the Measurement and Standards Laboratories of the National Institute of Standards and Technology is the work of the 165 members of the National Research Council's (NRC's) Board on Assessment of NIST Programs and its panels. These individuals were chosen by the NRC for their technical expertise, their practical experience in running research programs, and their knowledge of industry's needs in basic measurements and standards.

This assessment addresses the following:

  • The technical merit of the laboratory programs relative to the state of the art worldwide;
  • The effectiveness with which the laboratory programs are carried out and the results disseminated to their customers;
  • The relevance of the laboratory programs to the needs of their customers; and
  • The ability of the laboratories' facilities, equipment, and human resources to enable the laboratories to fulfill their mission and meet their customers' needs.
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