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Chemical Science and Technology Laboratory



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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 4 Chemical Science and Technology Laboratory

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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-

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 2002 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.

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