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4 Chemical Science and Technology Laboratory 35

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36 AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003 PANEL MEMBERS James W. Serum, SciTek Ventures, Chair Alan Campion, University of Texas, Austin, Vice Chair John Ball, U.S. Army Primary Standards Laboratory Jeffrey B. Bindell, University of Central Florida Ulrich Bonne, Honeywell Laboratories Douglas C. Cameron, Cargill, Inc. John W. Kozarich, ActivX Biosciences, Inc. Max G. Lagally, University of Wisconsin at Madison R. Kenneth Marcus, Clemson University Mack McFarland, Dupont Fluoroproducts James D. Olson, The Dow Chemical Company Athanassios Z. Panagiotopoulos, Princeton University Gary S. Selwyn, Los Alamos National Laboratory Michael L. Shuler, Cornell University Christine S. Sloane, General Motors Corporation Peter Wilding, University of Pennsylvania Medical Center Jerome J. Workman, Jr., Argose Inc. Submitted for the panel by its Chair, James W. Serum, and its Vice Chair, Alan Campion, this assessment of the fiscal year 2003 activities of the Chemical Science and Technology Laboratory is based on site visits by individual panel members, a formal meeting of the panel on February 25-26, 2003, in Gaithersburg, Maryland, and documents provided by the laboratory. 1U.S. Department of Commerce, Technology Administration, National Institute of Standards and Technology, Chemical Science and Technology Laboratory: Annual Report FY2002, NISTIR 6954, National Institute of Standards and Technology, Gaithersburg, Md., February 2003.

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CHEMICAL SCIENCE AND TECHNOLOGY LABORATORY LABORATORY-LEVEL REVIEW 37 The Chemical Science and Technology Laboratory (CSTL) is the nation's reference laboratory for chemical measurements. Its mission is to provide a chemical measurement infrastructure to support and enhance U.S. industry's productivity and competitiveness; assure equity in trade; and improve public health, safety, and environmental quality. The laboratory is organized in five divisions: Biotechnology, Process Measurements, Surface and Microanalysis Science, Physical and Chemical Properties, and Analytical Chemistry (see Figure 4.1~. Following the panel's major observations from this year's review, this chapter presents an overall assessment of the laboratory. Chapter 11 provides division-level assessments, with detailed discussions of some of the more noteworthy projects. Major Observations The panel presents the following major observations from its assessment of the Chemical Science and Technology Laboratory: CSTL's research and standards programs are technically excellent overall, with many considered to be world-class by the scientific and technical community in general and by international standards Chemical Science and Technology Laboratory 1 1 1 Biotechnology Division DNA Technologies Bioprocess Engineering Biomolecular Materials Structural Biology Process Measurements Division Fluid Flow Fluid Science Process Sensing Thermometry Pressure and Vacuum Thermal and Reactive Processes Surface and Microanalysis Science Division Microanaly- sis Research Surface and Interface Research Analytical Microscopy Physical and Chemical Properties Division Computational Chemistry Experimental Kinetics and Thermo- dynamics Chemical Reference Data and Modeling Experimental Properties of Fluids (Boulder) Theory and Modeling of Fluids (Boulder) Cryogenic Technologies (Boulder) . Analytical Chemistry Division Spectro- chemical Methods Organic Analytical Methods Gas Metrology and Classical Methods Molecular Spectrometry and Microfluidic Methods Nuclear Methods FIGURE 4.1 Organizational structures of the Chemical Science and Technology Laboratory. Listed under each division are its division's groups.

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38 AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003 organizations in particular. The laboratory's outstanding performance in the Key Comparisons of Na- tional Metrology Institutes (NMIs) conducted under the auspices of the CIPM (Comite International des Poids et Mesures) is a particularly fine example of CSTL's capabilities. CSTL has clearly demonstrated both the relevance and effectiveness of its programs to its cus- tomers, primarily U.S. industry, government, and academia, but also to international science, technol- ogy, and commerce. Evidence of the impact of its work includes customer feedback from symposia and workshops, formal economic impact studies, and documented leadership in the international standards community. Even during an extended period of flat budgets, the laboratory's innovative practices and suc- cessful partnering have sustained exceptional productivity and the continuation of its high visibility, recognition, and world leadership in the development of measurement standards. In particular, the panel cites significant advances in the clinical in vitro diagnostics (IVD) and NIST-Traceable Reference Materials (NTRM) programs. Having commercial facilities produce NIST-traceable gas standards is an excellent example of creative leveraging of CSTL's efforts. CSTL has implemented an excellent strategic planning process that is closely aligned with the goals and objectives of the overall NIST strategic plan (the NIST 2010 plan) and that has enabled it to effectively anticipate future customer needs. Linking the annual operating plan tightly and transparently to the strategic plan has been an excellent management decision that allows the laboratory to effectively plan its ongoing programs while responding to unanticipated needs and opportunities. The panel encourages the development of a coherent plan for responding to the explosive growth of onnortunities for the Biotechnolo~v Division. In particular. it is not clear that there currently exists ~ ~ ~7, ~ , , 1 1 ,. ,1 1 1 1 , 1 1 , ,1 1 1 , r enough In-house expertise In the biological sciences to guide and support the development ot programs in this field. Standard Reference Material (SRM) productivity could be enhanced by building stronger in- house collaborations. The Analytical Chemistry Division continues to be central to the laboratory's standards develop- ment. The panel is concerned, however, that declining support for personnel and equipment will ulti- mately erode both quality and productivity and encourages the laboratory to develop a plan to ensure the successful continuation of the important work conducted by this group. CSTL has made great progress in Web site design and information dissemination; as indicated in last year' s report, however, there remain lapses in data updates that detract from the utility and value of these sites. Also, the panel recommends that over the course of the next year the laboratory develop common entry points for all of the chemical information available on its site, perhaps using a search engine format similar to that of the Chemical Abstract Services Syfinder. While the panel is encouraged with the small increase in laboratory funding over the past year, it is concerned that proposed federal reductions in Advanced Technology Program funding will require nontrivial repositioning of the laboratory programs. CSTL should address this issue explicitly in its strategic and operational planning processes. Technical Merit The technical merit and quality of CSTL's work continue to be excellent, in many cases world-class. Its performance in the CIPM Key Comparisons is probably the finest single example of its stature in the national measurements community. The panel also wishes to draw attention to several other examples that illustrate the outstanding, ongoing quality and technical merit of CSTL projects, including these:

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CHEMICAL SCIENCE AND TECHNOLOGY LABORATORY IVD; 39 Significant advances in clinical markers technologies and the completion of several SRMs for Significant advances in the rigorous validation of biomarkers for health diagnostics; Significant advances in the research on properties and equation-of-state of fluid mixtures near the critical point, and the release of an updated version of the NIST database REFPROP (alternative refrigerants); Development of the extensible markup language (XML) data format for spectroscopic hyperdata. This general data format enables very impressive methods for spectral data storage and analysis and is destined to become a nationally accepted standard format; Demonstration of a 10,000-fold improvement in the sensitivity of microfluidic sensors; A major update of the NIST Mass Spectral Database, which is among NIST's most widely disseminated Standard Reference Databases (SRDs); and Successful completion of a Johnson Noise Thermometer prototype and documentation of a noise- to-power accuracy ratio of better than 0.1 percent over the range considered. The panel views the ability to recalibrate these sensors remotely for example, for space station applications as very significant. Program Relevance and Effectiveness CSTL continues excellent practices to ensure that its technical programs are relevant to the needs of its customers. Various mechanisms are used to gather outside input on current or planned activities; these include participation in standards committee meetings, technical conferences, benchmarking and roadmapping activities, professional society meetings and committees, and trade organization events. Staff members take lead roles in organizing these gatherings and often hold them at NIST. Researchers maintain informative relationships with a large number and wide variety of guest researchers and collaborators in industry and at universities to support and leverage their work. Overall, the programs of CSTL have a strong impact on a wide array of industries and research communities. CSTL' s contributions often provide critical bridges between research directed toward the short-range goals of industry and the long-range, open-ended inquiries pursued in universities. Particu- larly noteworthy for their relevance and effectiveness are the laboratory's efforts in SRMs, SRDs, and international standards activities. These services and activities rarely garner headlines, but they under- pin many critical measurements in the chemical, pharmaceutical, medical, and other industries and are therefore very highly leveraged investments. Finally, CSTL responded quickly and decisively to recent national crises and is actively assessing its current capabilities and planning for possible future contribu- tions to the national homeland security effort. The panel wishes to highlight the following programs for their significant impact: Widely recognized leadership in the development of clinical standards and diagnostic devices, ensuring continued U.S. dominance in an area fostering more affordable health care at home and abroad. New methods developed by CSTL for the amplification and automated detection of DNA fragments served a critical need in the identification of victims of the World Trade Center disaster. This technology could be the basis of a multitude of applications existing in the military and supporting homeland security requirements. The frequency of visits to the NIST Chemistry WebBook site (an increase of 43 percent in 2002) and the inclusion of databases in commercial instrument packages. Roughly one-half of all gas chroma- tography/mass spectrometry instruments sold worldwide include the CSTL Mass Spectral Database,

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40 AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003 enabling the application of these techniques to problems that span nearly every area of science and technology. The pursuit of DNA diagnostics for the detection of human disease in the NISTINational Cancer Institute (NCI) Biomarker Validation Laboratory. This NIST component of the NCI Early Detection Research Network (EDRN) serves to refine recently discovered cancer biomarkers and to format new research tests for field trials in EDRN clinical laboratories. Significant advances are now being made in the areas of breast and prostate cancer and in the identification of clinical markers for radiation damage and processes involved in aging. The development of an XML data format for spectroscopic hyperdata in the transmission electron microscope (TEM) laboratory is extremely important work. This general data format supports very powerful methods of spectral data storage and analysis and is destined to become a nationally accepted standard format. These data are critically important in almost every area of science, technology, and manufacturing. Developments in microheater sensors have reduced detection limits to as low as 20 to 200 ppb for satin; these sensors can also detect mustard gas and GA-tabun with a response time of approximately 50 seconds. A new, monolithic preconcentrator may further increase sensitivity by an additional factor of 10. Carbon nanotubes have been grown on MEMS micro-ho/plates, enabling the evaluation of their performance as gas sensors. This project is relevant to both homeland security and Chemical Weapons Convention defense technologies. Laboratory Responsiveness CSTL provided a detailed, written, point-by-point response to the observations and recommenda- tions made in the FY 2002 assessment. The panel is, in general, quite satisfied with the laboratory's response. Many recommendations were implemented, and thoughtful replies were provided in cases in which management either could not implement a suggested change (usually for resource or NIST-wide structural reasons) or chose a different solution based on its own programmatic priorities and resources. A few examples of the kinds of laboratory responses include the following: Determined efforts to bring all calibration programs into compliance with ISO/IEC 17025 have resulted in significant progress and already rate highly in the eyes of calibration service customers. It would be especially beneficial for NIST to publish its ISO-compliant quality manual and other relevant quality documents on the Web. Commercial and government calibration and testing laboratories could use such documents for a variety of purposes, including use as guides and templates for their own documents. The panel is pleased to note that the laboratory has started to address the issue of management training for group leaders; this is an important issue, given the broad range of responsibilities now assigned to group leaders and the general lack of training in these areas in the careers of scientists and engineers. The panel was pleased to see the reorganization of the effort in atmospheric chemistry in the Surface and Microanalysis Science Division in response to repeated suggestions by the panel over several years. Some responses to the FY 2002 recommendations were not as strong as those noted above. For example, progress in providing timely Web updates and more interactive site designs continues to be slow. The dissemination of new knowledge and data generated by the laboratory is critical to its continued success and utility; now that the Web is the dominant point of contact between NIST and its

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CHEMICAL SCIENCE AND TECHNOLOGY LABORATORY 41 customers, it is imperative that the Web site be an efficient and easy-to-use interface. If resource limitations at the laboratory level are indeed the constraint to more rapid progress, the panel urges management to work collaboratively with the directors of the other laboratories and with the NIST Director's Office to address this NIST-wide issue of great importance. Laboratory Resources Funding sources for the Chemical Science and Technology Laboratory are shown in Table 4.1. In January 2003, staffing for the laboratory included 271 full-time permanent positions, of which 234 were for technical professionals. There were also 81 nonpermanent or supplemental personnel, such as postdoctoral research associates and temporary or part-time workers. Although there is a small increase in CSTL funding for FY 2003, mandatory salary increases will translate once more into an essentially flat budget. Within this environment, hard choices have had to be made, involving trade-offs between personnel and laboratory equipment. The loss of five professional staff in one division during 2002 has heightened the panel's concern over the trend in reduction of full- time-equivalent personnel. As in the previous assessment, the panel observed too many priority projects with subcritical resources devoted to them. Given that an era of flat budgets has taken hold, the panel strongly advises the laboratory to take a hard look at its priorities and examine areas in which potential TABLE 4.1 Sources of Funding for the Chemical Science and Technology Laboratory (in millions of dollars), FY 2000 to FY 2003 Fiscal Year Fiscal Year Fiscal Year Fiscal Year 2000 2001 2002 2003 Source of Funding (actual) (actual) (actual) (July 2003 estimate) NIST-STRS, excluding Competence 37.7 36.9 38.3 45.1 Competence 2.4 1.9 2.7 2.7 ATP 3.3 3.2 2.5 2.1 Measurement Services (SRM production) 2.2 1.9 2.6 2.2 OA/NFG/CRADA 14.2 14.3 12.4 10.7 Other Reimbursable 3.4 5.8 6.1 6.3 Total 63.2 64.0 64.6 69.1 Full-time permanent staff (totally 275 264 273 271 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. Compe- tence funding also comes from NIST's congressional appropriations but is allocated by the NIST director's of lice in multiyear grants for projects that advance NIST's capabilities in new and emerging areas of measurement science. Advanced Technol- ogy 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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42 AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003 in-house funding resources may exist. One area suggested is charges for database use. Such an activity would require backing from comprehensive evaluations of cost and usage issues. Another area sug- gested for examination is optimization of professional-to-support staff ratios. Also in the line of re- strained budgets, the laboratory director should exert even greater effort to keep researchers informed of pending programmatic realignments and perhaps even to invite their input as decisions are being made. This would not only serve to increase morale but would also be a resource for new ideas based on the experiences of the staff. Facilities and instrumental infrastructure in CSTL are very good overall. Updates in the elevators and exhaust hoods in some buildings have improved the working environment. The panel was pleased to hear that some funding has at last become available to begin repairs on the Boulder facility. Two important pieces of equipment, the electron microprobe and the Auger spectrometer, remain in need of attention to be brought online. It is still not clear when the CSTL equipment will be moved to AML.