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Chemical Science and Technology Laboratory

INTRODUCTION

The Chemical Science and Technology Laboratory (CSTL) is the U.S. reference laboratory for chemical measurements. It is entrusted with developing, maintaining, advancing, and enabling the chemical measurement system for the nation, thereby enhancing U.S. industry’s productivity and competitiveness, assuring equity in trade, and improving public health, safety, and environmental quality.

The laboratory staff is organized in five divisions, as shown in Appendix A:

  • Biotechnology Division (BD),

  • Process Measurements Division (PMD),

  • Surface and Microanalysis Science Division (SMSD),

  • Physical and Chemical Properties Division (PCPD), and

  • Analytical Chemistry Division (ACD).

Appendix A also presents the staffing trends for the laboratory (see Figure A.3).

MAJOR OBSERVATIONS

The CSTL is engaged in a large number of chemical science and chemical technology research and metrology activities that are closely interrelated, highly effective, and clearly focused on the metrology needs of the nation. The Board reviewed a large fraction of the work under way in the laboratory and commends the technical staff and management for achieving an extremely high level of consistent quality, effectiveness, and productivity across such a broad range of activities. The CSTL remains vibrant and essential to NIST’s mission.

This section highlights a number of activities that are exemplary in nature and also identifies several opportunities for improvement. Programs and projects reviewed by the Board during the past 2 years but



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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 3 Chemical Science and Technology Laboratory INTRODUCTION The Chemical Science and Technology Laboratory (CSTL) is the U.S. reference laboratory for chemical measurements. It is entrusted with developing, maintaining, advancing, and enabling the chemical measurement system for the nation, thereby enhancing U.S. industry’s productivity and competitiveness, assuring equity in trade, and improving public health, safety, and environmental quality. The laboratory staff is organized in five divisions, as shown in Appendix A: Biotechnology Division (BD), Process Measurements Division (PMD), Surface and Microanalysis Science Division (SMSD), Physical and Chemical Properties Division (PCPD), and Analytical Chemistry Division (ACD). Appendix A also presents the staffing trends for the laboratory (see Figure A.3). MAJOR OBSERVATIONS The CSTL is engaged in a large number of chemical science and chemical technology research and metrology activities that are closely interrelated, highly effective, and clearly focused on the metrology needs of the nation. The Board reviewed a large fraction of the work under way in the laboratory and commends the technical staff and management for achieving an extremely high level of consistent quality, effectiveness, and productivity across such a broad range of activities. The CSTL remains vibrant and essential to NIST’s mission. This section highlights a number of activities that are exemplary in nature and also identifies several opportunities for improvement. Programs and projects reviewed by the Board during the past 2 years but

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 not explicitly discussed in this chapter have been deemed by the Board to be “on track”; they are fulfilling their missions, are achieving their objectives, and are generally considered to be excellent. The CSTL is truly a national resource, conducting outstanding research to support the continued development of a wide range of measurement capabilities, providing critical and reliable chemical and physical properties data and essential reference standards. Its work spans the entire scientific spectrum, from fundamental physics through chemistry and into biology, and supports an astonishingly diverse group of industries. The quality of the scientific staff is superb, and the laboratory has undergone a rather dramatic transformation over the past decade or so to become entrepreneurial and customer-focused while being mindful to maintain and advance its core competencies. Evidence of its high technical quality, relevance, and effectiveness, some of which is presented in this report, is abundant. CSTL’s work has been increasingly organized along programmatic lines in order to encourage and require collaboration and cooperation among divisions and between laboratories. These strategic directions include nanometrology, biometrology, properties information infrastructure, process metrology, and chemical metrology, which are all well aligned with NIST’s Strategic Focus Areas. Adopting this matrix management approach has enabled the laboratory to tackle important problems that are inherently interdisciplinary by assembling teams with the appropriate backgrounds and expertise. A few outstanding examples of both intra- and interlaboratory collaborations include the following: the Tissue Engineering Competence Program, a collaboration between the Biotechnology Division of CSTL and the Polymers Division of the Materials Science and Engineering Laboratory (MSEL); extensive collaborations between the Physical and Chemical Properties Division and the Analytical Chemistry Division on new biological (including weapons) and health-related applications of mass spectrometry in support of missions of the National Institutes of Health (NIH) and Department of Homeland Security (DHS); and Johnson Noise Thermometry, a collaboration between the Process Measurements Division and the Electronics and Electrical Engineering Laboratory. Significant accomplishments include the following: Moving several divisions to the Advanced Measurement Laboratory (AML) has ensured that CSTL will maintain its extremely high technical quality in many areas, allowed it to close the gap in other areas, greatly enhanced its capabilities, and allowed it to move in new directions, thus enhancing its position and value to the nation. Instrumentation that barely met specifications in their old locations (despite years of tuning) immediately exceeded expectations owing to the superior environmental control in the AML. The addition of the next-generation analytical electron microscope, with sub-Å spatial resolution, in early 2006 to the existing suite of analytical instrumentation already installed will make the AML a leading facility in the world for nanometrology. CSTL’s expanded efforts at the Hollings Marine Laboratory (HML) in South Carolina are outstanding. The existing and proposed new projects are truly synergistic, applying CSTL’s expertise to areas of interest to the other HML partners and thus leveraging the investments of all parties. The excitement and enthusiasm of the HML staff are palpable. The interactions at the HML represent an exemplary model of scientific collaboration among a number of federal and state agencies. The CSTL has appropriately adopted the International Organization for Standardization/International Electrotechnical Commission (ISO/IEC) Standard 17025, General Requirements for the Competence of Testing and Calibration Laboratories. This new quality program has been adopted by all measurement service groups, which has resulted in an increased emphasis on documentation and formal validation before new or improved measurement services are offered. ThermoML is a powerful new approach, developed by the Thermodynamics Research Center (TRC), for the acquisition, evaluation, storage, and dissemination of thermophysical and thermochemi-

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 cal reference data. It is currently being balloted by the International Union for Pure and Applied Chemistry for acceptance as an international standard and is now being used voluntarily by five scientific thermodynamics journals, leading simulation software companies, and data repositories around the world as the accepted format for the exchange of these data. This product is a fine example of CSTL’s forward-looking approach to research and development (R&D) that results in a resource of great value. Opportunities for improvement include the following: Unless increased, the budget is likely to affect the laboratory’s ability to maintain the knowledge base and expertise of its highly experienced staff, its ability to attract new staff in order to replace losses in existing areas, and its ability to initiate new activities that are needed to support the nation’s measurement and metrology needs of the future. The fact that NIST is no longer part of the consortium that manages the Protein Data Bank is cause for concern. While there is some merit to the argument that competitive renewal proposals might result in enhanced performance, NIST should continue to be a partner in this enterprise for two reasons. First, the collection and dissemination of the physical and chemical properties of molecules (in this case biomolecules) is clearly a central part of NIST’s mission; second, this collection of data is so critically important to the nation that it should reside permanently in a federal laboratory. Despite repeated recommendations and encouragement from the Board over a number of years, little progress has been made in defining goals for the Biotechnology Division and in implementing strategies to achieve those goals. The Board has consistently agreed that this is a vital area to which CSTL can and should make significant contributions, that CSTL cannot possibly contribute to all fields of this exploding area of science and technology, and that CSTL should select a few areas that are consistent with its mission and focus on those areas where its efforts will make a difference. The new CSTL Director has been developing a new strategy for dealing with the biological sciences within the laboratory that may include reorganizing the Biotechnology Division along disciplinary lines (like the other four CSTL divisions) and looking at biosciences more broadly as an activity that spans all of the divisions of the laboratory. The Board endorses this approach. The CSTL/Center for Advanced Research in Biotechnology (CARB) interaction has not been particularly effective; the laboratory should vigorously pursue new ways to increase collaboration and cooperation with this potentially valuable asset. Efforts should be focused on the development of areas in which NIST’s expertise can contribute to problems of interest to CARB scientists, resulting in synergistic interactions. The Hollings Marine Laboratory is an outstanding example of this kind of collaboration, and CSTL should consider using it as a model for the development of stronger ties to CARB. TECHNICAL QUALITY AND MERIT Overall, the quality of the technical work done in the Biotechnology Division is very high and in most cases outstanding. The work reviewed is highly effective and relevant, driven by a clear strategy, with stakeholders identified and often participating in the application of the technology or measurement techniques as soon as they are developed. However, the breadth of the technology and the rate of change in the biosciences area are clearly challenging the division to maintain its position in the life sciences and associated biotechnology. Unless additional resources are made available, the division will not be able to meet the rapidly growing and changing needs of the nation in this area for research, standards, and metrology.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 The Biotechnology Division has played and should continue to play a pivotal role in NIST’s effort to address critical measurement and data needs for the rapidly developing biotechnology industry. The division remains a vital resource to NIST and to CSTL, serving as a key link to the biotechnology industry, and it is critical to NIST’s global presence in the rapidly evolving biotechnology field and to strengthening the position of the United States in the global economy. The Biotechnology Division manifests the NIST part of the joint institute with the University of Maryland Biotechnology Institute’s Center for Advanced Research in Biotechnology. The division’s involvement with CARB has been important to the quality and relevance of the division’s research programs; strengthening its ties with CARB and CARBII is deemed critical to CSTL’s continuing development of the highest-quality metrology-based research and standards activities. The Structural Biology Group’s programs (most in collaboration with CARB) are judged to be outstanding. Anticipated areas of expansion include Good Manufacturing Practices bioprocessing, plant and insect transformations, high- and medium-resolution structural biology, microarray/gene expression, and protein production/characterization. The Board regrets NIST’s elimination from the consortium that manages the Protein Data Bank (PDB), which is the single worldwide repository for the acquisition, evaluation, and dissemination of three-dimensional protein and nucleic acid structural data. The Biotechnology Division of CSTL played a significant role in developing the current PDB, and the Board encourages CSTL (and NIST) to find a way to reengage in this effort. The Process Measurements Division has undergone a significant restructuring and project/mission refocusing, with a number of activities relocating to the new, state-of-the-art AML. All of this has been beneficial to the group, which is newly energized and well focused on clearly defined objectives. The division’s strategy of continuous improvement of its capabilities by continuing research on traditional measurement parameters provides the basis for it to maintain preeminence among National Metrology Institutes (NMIs) in most parameters for which it provides measurement services. As one of many specific examples, the division’s Thermometry Group is the world leader in this key measurement parameter, as judged by range, uncertainty, and participation in international technical activities. This integration of research and standards maintenance is a model that should be considered for application to other standards activities across NIST. PMD’s humidity generation and measurement capability appears well on the way to matching or exceeding other NMI capabilities over all ranges and to providing calibration to customers with faster, more automated services. Its trace humidity measurements are already unsurpassed worldwide and show promise for additional improvement in both range and uncertainty. The division does not have high-flow-rate natural gas measurement capabilities that are equivalent to the best NMIs in the world; this deficiency is potentially detrimental to the nation’s commercial competitiveness in this area by not having NIST-traceable metering standards. The division is addressing this issue, however, by developing relationships with two companies that do have outstanding high-flow-rate test and calibration stands. This collaboration should allow the division to improve capabilities and to reduce uncertainties and thus to match or exceed those of the best European NMIs quickly and at reduced cost. Improvements in flow, temperature, pressure, and other basic measurement parameters have obvious and direct impact in commerce and industry. As the division’s research projects enable more measurement standards to be based on “intrinsic” principles rather than on physical artifacts, significant improvements in performance and accuracy can be expected to spread steadily throughout the U.S. measurement system. Examples of current projects to develop standards of this type include Johnson Noise Thermometry, Gas Concentration Standards Based on Cavity Ring-Down Spectroscopy, and the Atomic Standard of Pressure.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 The division has achieved significant reductions in measurement uncertainty for flow-measurement projects of water, atmospheric gases, and hydrocarbons. NIST gas-flow-rate uncertainty was reduced by an order of magnitude in the 0.1 to 2000 standard liters per minute (slm) range and is now the best in the world. Hydrocarbon-flow-rate uncertainty in the range of interest to the Department of Defense (DOD) has also been reduced by an order of magnitude, and for higher-rate gas flows (to 78,000 slm), the uncertainty has been cut in half. In response to a constant push for improved flow-rate measurements from the DOD, these projects bring the U.S. capability in these ranges in line with those of the best NMIs. The Surface and Microanalysis Science Division is responsible for the characterization of the spatial and temporal distribution of chemical species, with a particular focus on microanalysis, surfaces and interface analysis, and advanced isotope measurement techniques. The overall quality of the personnel in this organization is very impressive. Two NIST fellows, in particular, are both luminaries in the areas of X-ray microanalysis and Auger and X-ray photoelectron spectroscopies, and the Board hopes that plans are in place to continue their essential work in the event of possible upcoming retirements. Recent work on developing the silicon drift detector approach is remarkable; it will take the technique to the point where it will assuredly achieve great industrial importance. Multidimensional (hypercube) data storage using a newly developed extensible markup language (XML) format has been further developed and is being adopted in many other areas of the laboratory. High-level international adoption of this approach is likely to result in an increased richness and depth of analysis of complex analytical systems. The division followed the Board’s recommendation in the previous report: the characterization of SiGe films has been completed, and resources have been moved on to other activities. The nascent effort in super-resolution spectroscopy (a new NIST competence project) is extremely promising. It will provide an entirely new way to characterize materials on the sub-100 nm length scale, a challenge of immense current interest, importance, and relevance to a number of areas of science and technology. The Physical and Chemical Properties Division is responsible for providing measurements, standards, data, and models for the following: the thermochemical, thermophysical, and interfacial properties of gases, liquids, and solids, both as pure materials and as mixtures; the rates and mechanisms of chemical reactions in the gas and liquid phases and at surfaces; and fluid-based physical processes and systems, including separations and low-temperature refrigeration, heat transfer, and flow. Many capabilities of the PCPD are unique when compared with the state of the art in physical and chemical properties science. A few examples are summarized below: Unique fluid properties experimental apparatus. Several capabilities in the Experimental Properties of Fluids Group, including heat-capacity, isochoric PVT (pressure, volume, temperature), viscosity, and automated thermal conductivity apparatus, have become the only working examples in the world. Maintaining these capabilities is important because experimental work continues to be deemphasized throughout the thermodynamics community elsewhere. Mass spectral database. This database is supplied under license from NIST on over half of the world’s commercial mass spectrometers. NIST is responsible for gathering, authenticating, updating, and archiving the data. A new release is planned for 2005 in which 20,000 new compounds, spectra for more than 2,000 compounds, and, for the first time, gas chromatography retention index data for 19,000 compounds will be added. State-of-the-art Helmholtz energy reference equation of state (EOS). A recently developed “short-form” version of the reference fluid EOS can be used to describe all of the thermodynamic properties for fluids with limited data sets but with higher accuracies (typically 0.1 to 0.5 percent in density, 1 to 3 percent in liquid heat capacities and sound speeds) than previously attained for these fluids.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 ThermoML. Developed over several years by the Thermodynamics Research Center, this XML-based approach for the storage and exchange of thermophysical and thermochemical property data has been accepted by the International Union for Pure and Applied Chemistry and is now being voluntarily used by five scientific thermodynamics journals. The TRC also provides a unique database of critically evaluated experimental data. Primary standard dual sinker densimeter. This apparatus is used to provide data for accurate equations of state (most recently for propane) and density standards over a wide range of temperatures and pressures for NIST reference materials (e.g., work on toluene is in progress). An exploratory project to investigate the feasibility of the densimeter for use as a primary temperature standard showed that a similar apparatus with larger sinker volumes would be required. Computational Chemistry Comparison and Benchmark Database (CCCBDB). This database, developed by the Computational Chemistry Group, provides benchmark data for evaluating theoretical methods and for assigning uncertainties to quantum chemical computations, particularly thermochemistry. The Web site, which contains tutorials and graphical user interfaces, receives an average of 25,000 visits per month. Microfluidic critical point apparatus. This new apparatus consists of a high-performance liquid chromatograph capillary (300 µm diameter, 20 mm long) that can be rapidly heated to produce critical opalescence, which yields measurement of the critical temperature and pressure as well as information on heat flow in near-critical fluids. This is a project in the division’s ongoing initiative on small-sample, high-throughput thermophysical properties measurements. Cryogenic flow calibration apparatus. This facility, unique in the United States, has been used to calibrate liquid nitrogen flowmeters for more than 40 years. NIST provides a vital service with this facility. However, since the flowmeter companies use the NIST-calibrated meters as reference standards to calibrate the meters that they sell, the demand is relatively small (15 to 20 meters calibrated annually). Increased staffing in Computational Chemistry Group. The division has increased its investment in the Computational Chemistry Group (partially through personnel realignments), resulting in an increase in staffing from four staff members 7 years ago to nine staff members currently and almost an equal number of full-time, postdoctoral guest researchers. This investment has produced a lively and dynamic group whose work is synergistic with that of the experimentalists in the division, greatly adding value to their outputs. The Computational Chemistry Group is also aggressively developing new methodologies in quantum chemistry and molecular modeling to support NIST-wide efforts to understand complex systems. The group has demonstrated sophistication as well as the wisdom it has shown in selecting problems for their distinctiveness and relevance. The Analytical Chemistry Division maintains outstanding metrology based on core competencies in the following: 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 generally cover all those of importance in the analytical sciences. In 2005 the Organic Analytical Methods Group (OAMG) placed an emphasis on dietary supplement Standard Reference Materials (SRMs) (through the National Institutes of Health [NIH]), marine health and bioscience applications (through the Hollings Marine Laboratory), forensic and homeland security measurements and standards, clinical standards, and protein quantification. These are among the more important analytical applications facing society today. OAMG’s work represents superior productivity while maintaining high quality, providing advanced metrology work in its key activity areas. An important methods development project was the determination of brominated flame retardants in the environ-

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 ment. The research showed that these materials, which can compete with thyroid hormones and act as endocrine-function disrupters, are ubiquitous in the environment and may have serious health ramifications if left unchecked. Another new OAMG project responded to a request by the Department of Justice (through the NIST Office of Law Enforcement Standards) regarding the standardization and uses of pepper spray canisters, for which there are no standard formulations or efficacy measurements. The project will define the pepper extract compositions of different suppliers and the propellant systems used. These are particularly fine examples not only of the technical excellence of CSTL’s work but also of its agility and responsiveness to requests from other agencies. The molecular spectroscopy work has focused on standards for fluorescence, near-infrared, Raman, and ultraviolet-visible spectroscopies. There has been a conscious effort to transfer the solid-material, optical SRM production to secondary sources of supply, following development and characterization by the CSTL staff. The Analytical Chemistry Division should develop a plan for the seamless continuation of optical SRM production; this capability is being lost within NIST, since one of the few staff members in this area retired in 2004. The optical imaging community needs optical standards for microarray and imaging methods that focus on spatial resolution, absorbance or intensity, and spectral line shape; homogeneity standards for comparison of optical images would also be of acute interest. This technical area requires renewed invigoration and expansion to meet current and projected consumer demands. The division does not currently have any specialized imaging technology expertise, whereas aspects of spatial imaging, and particularly image processing, are highly developed within other divisions of CSTL, particularly in the Surface and Microanalysis Science Division. The CSTL should encourage collaborations between these divisions to assist the Analytical Chemistry Division in developing new competencies to support the particular needs of its customers. The potential of the Nuclear Methods Group and the Gas Metrology and Classical Methods Group has been unrealized owing to operational structural issues. The Board saw little evidence of innovation or new project proposals that address emerging needs, and some group leaders were not prepared to make recommendations that would address some impending difficulties. An overall strategy for the prioritization of activities was not apparent to the Board. These two groups continue to operate using a model by which very good science is done and high-quality products are delivered, but without the crosscutting, interdisciplinary activities that have been developed in the other groups. A serious infusion of new talent is required to set new priorities and operation paradigms. As technical relevance and high commercial importance increasingly drive the work of Chemical Science and Technology Laboratory, ACD and CSTL management should consider realignment of the division’s present group structure to better reflect areas of technical synergism and customer service operations. Finally, both the Analytical Chemistry Division and the Process Measurements Division could provide great service to the pharmaceutical industry by engaging in the process analytical technology (PAT) activities now being spearheaded by the Food and Drug Administration (FDA). The need for automation in calibrating analytical instrumentation will require the development of optical and chemical standards, algorithm standard practices, and standard database models for testing algorithms and real-time calibrations. These demanding applications will require the metrology excellence of NIST to be successful in order to achieve the pharmaceutical industry’s ambitious goal of 100 percent monitoring. Several groups would welcome NIST’s involvement; these include the American Society for Testing and Materials’ International Main Committees E13 on Molecular Spectroscopy and Chromatography and E55 on PAT, the United States Pharmacopoeia, and the FDA.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 RELEVANCE AND EFFECTIVENESS The Chemical Science and Technology Laboratory provided the Board with a number of measures of output and impact that are included here. Table 3.1 summarizes some of the CSTL outputs and interactions demonstrating the high level of activity of the laboratory. In addition to documenting output, CSTL has attempted to measure impact. It has done so in part by commissioning a number of formal economic impact analyses by outside experts (e.g., RTI International) over the past 8 years. These reports are very detailed, and the methodology is thoroughly discussed. In these analyses, selected programs were evaluated both to quantify their impact and to guide CSTL’s strategic planning. They included Standards for Calcium Testing (Gallaher et al., 2004); NIST-Traceable Reference Material Gas-Mixture Standards (Gallaher et al., 2002); Cholesterol Standards (Leech and Belmont, 2000); Standards for Sulfur in Fossil Fuels (Martin et al., 2000); Alternative Refrigerants (Shedlick et al., 1998); and Thermocouple Standards (Marx et al., 1997). Benefit-to-cost ratios varied from 3:1 to more than 100:1 across these programs, with social rates of return being generally much higher. Another example of impact was provided in a letter to then-NIST Director Arden Bement, dated December 22, 2004, from Margo Oge, director of the Environmental Protection Agency’s Office of Transportation and Air Quality. She stated that “the development of [diesel fuel] SRMs directly supports the introduction of ultra-low-level diesel fuel with the implementation of the U.S. EPA 2007 highway heavy-duty and 2010 Tier 4 non-road diesel regulations. These regulations when fully implemented, will provide roughly $150 billion annually in health and welfare benefits to the American Public.” The selected examples cited above help demonstrate the economic value of CSTL to the nation. CSTL management has effectively documented these contributions and used these tools to guide its planning. The following discussion addresses selected examples of CSTL relevance and effectiveness. In the Biotechnology Division, the DNA Technologies Group continues to produce highly visible work with programmatic relevance, with many of its programs effectively reaching its customers in industry and in the scientific community. The program of advanced mass spectrometry of modified DNA bases provides a vital link between NIST and NIH and the National Institute on Aging. The work of this group for the Early Detection Research Network of the National Cancer Institute is outstanding and has been renewed. The program in human mitochondrial DNA for forensic applications and disease diagnosis which is directed at near-term needs of the nation, is also notable. The Bioprocess Measurements Group remains focused on measurements and standards that support the needs of the agricultural, biomanufacturing, and pharmaceutical industries; homeland defense; and medical technologies. Of particular relevance and promise is the group’s work to develop measurement standards and to provide data and reference materials for the detection of biothreat agents and for the safe, reliable testing of detection devices, as well as its work on remediation technologies, and in personnel training. The Biomolecular Materials Group working on cell and tissue measurements has developed well-focused projects that include the following: development of quality-assurance and quality-control evaluation of collagen reference surfaces; fluorescence measurements for characterizing cytosolic green fluorescent protein (GFP) fluorescence intensity preservation in mammalian cultured cells; evaluation of the cytotoxicity of silicon nanoparticles and fluorescent dyes for the staining of live cells; and the use of calibrated and validated indicator cells on commercially relevant surfaces. Each of these projects has key stakeholders that are well defined (for example, the pharmaceutical industry, tissue culture plasticware manufacturers, cell culture reagent manufacturers, imaging tools/analysis manufacturers, and the FDA). The group has leveraged its cell metrology expertise to develop a successful program at

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 TABLE 3.1 Summary of Selected Outputs and Interactions of the Chemical Science and Technology Laboratory in FY 2004 Divisiona Publicationsb Talks Committeesc Seminars Conferences CRADAsd Patents Issuede SRMs/RMsf SRDs Calibrationsg 830 1 20 12 8 1 0 0 0 0 0 831 120 152 39 3 22 3 1 8 2 0 836 65 45 76 13 5 1 0 1 0 682 837 38 90 80 10 4 4 1 3 5 0 838 86 114 83 21 5 6 0 2 16 0 839 71 159 135 36 6 3 0 135 0 323 Total 381 580 425 91 43 17 2 149 23 1,005 a830, Laboratory Office; 831, Biotechnology Division; 836, Process Measurements Division; 837, Surface and Microanalysis Science Division; 838, Physical and Chemical Properties Division; 839, Analytical Chemistry Division. bPublications appearing in print in FY 2004. Another 165 manuscripts have been submitted for publication. cCommittee totals include 61 editorships and the Thermodynamics Research Center. dCRADAs signed in FY 2004. eThere are a total of 44 active patents. fSRMs/RMs (certificates issued). gCalibrations were performed for more than 306 customers. NOTE: CRADA, cooperative research and development agreement; SRM, Standard Reference Material; RM, Reference Material; SRD, Standard Reference Data.

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 the Hollings Marine Laboratory; the objective of this program is to determine optimal assays for monitoring cell state pre- and post-cryopreservation. In quantitative cell biology, the group met every milestone of the Tissue Engineering Competency Program (joint with the Polymers Division of the Materials Science and Engineering Laboratory) earlier than scheduled. The Process Measurements Division’s trace humidity work is particularly important to the U.S. semiconductor industry. The division has performed commendable work in chemical sensing using its “Micro-Hot Plate” to support the DHS. It should continue to build on the momentum and success it has achieved in collaboration with other government and industrial research and development (R&D) organizations to provide the fundamental scientific understanding, property data, and measurement standards for such promising microelectromechanical systems technology. This division’s high-quality research and standards programs are clearly focused on meeting the needs of U.S. industry and government. In the area of calibration, the Surface and Microanalysis Science Division has developed some highly accurate standards for testing explosive detectors, but they appear to have short lifetimes. Microencapsulation technology (which the Board suggested as a possible cure) was already under consideration. Related division work for the DHS that is focused on developing calibration standards for testing “drug-sniffing” instruments could be very significant. However, the division should ensure that the work it undertakes in responding to other agencies will indeed fulfill a real need; it should not hesitate to decline a request if its scientific and technical evaluation suggests that the work is likely to be irrelevant, even if successful. The Analytical Chemistry Division develops strategic priorities in large part guided by feedback from major customer visits. Its other agencies (OA) funding and collaborative research activities are impressive. OA dollars have increased 23 percent, from $3.5 million in FY 2004 to $4.3 million in FY 2005 (projected)—a concrete demonstration of the relevance and technical quality of the division’s research and services. The Organic Analytical Methods Group has responded effectively to requests from other agencies and has anticipated future needs. Excellent examples of relevance and effectiveness include the group’s work on dietary supplement SRMs (for the NIH Office of Dietary Supplements), marine health and bioscience applications (with the Hollings Marine Laboratory), forensic and homeland security measurements and standards, clinical standards (in support of the need of U.S. industry to meet directives of the European Union for in vitro devices), protein quantification (of general interest), brominated fire retardants in the environment, and the standardization of pepper spray canisters (at the request of the Department of Justice). The Organic Analytical Methods Group is extremely efficient and productive. The group’s clients include the National Oceanic and Atmospheric Administration; the Environmental Protection Agency (which increased funding significantly); the NIH Office of Dietary Supplement for Botanical Dietary Supplements; the National Institute of Justice (NIJ); the Office of Law Enforcement Standards—a NIST liaison group with the NIJ; the Defense Threat Reduction Agency; and recent NMIs with International Comparison Analyses. This group effectively disseminates its results and establishes priorities. An infusion of new scientific talent over the past few years has improved the group’s visibility through publications and conference presentations. The laboratory will have a long-term impact on analytical methods and the well-being of marine animals by developing new methods to support environmental science. RESOURCES In general, the facilities and equipment of the Chemical Science and Technology Laboratory are excellent and provide CSTL staff the physical resources they need for their work. The Advanced

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An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Years 2004 – 2005 Measurement Laboratory (AML) has provided CSTL with much-needed, state-of-the-art space. CSTL staff expressed some concern about the quality of the space allocated to those divisions on the Gaithersburg campus that were not relocated to the AML. It appeared to the Board either that there was no plan for the renovation of existing space or relocation of these divisions to new space, or that any such plan had not been discussed in detail with the staff involved. CSTL management should work closely with the staff to develop plans for space and to keep them informed as these plans develop. NIST has responded to concerns expressed in previous assessment reports of the Board about the quality of the Boulder facilities. They have been renovated and are now deemed acceptable by the Board members who visited the site during this assessment period. Equipment there is generally state of the art and meets the needs of CSTL researchers. The Analytical Chemistry Division, however, finds it difficult to acquire the equipment necessary for it to remain at the cutting edge of its field. In CSTL in general, it appears to be relatively easier to procure large, expensive analytical equipment (e.g., electron microscopes, surface analysis equipment) than it has been to keep essential, though less-expensive (about $50,000) pieces of equipment (spectrometers, chromatographs and so on) at state of the art. In the area of human resources, CSTL is now at the point where attrition, due to retirements and the combination of flat budgets and maintaining competitive salaries, leaves it at risk of losing essential core competencies and unable to grow to meet metrology needs in rapidly expanding fields, such as the biosciences. The laboratory has lost 22 technical staff (nearly 10 percent) between 1999 and 2004 (see Figure A.3 in Appendix A), and a number of retirements are expected in the coming years. The CSTL has done an outstanding job of managing these losses, but it will be unable to fulfill its mission without an adequate increase in its budget to replace staff with essential skills and to hire new staff to develop those new programs that are essential in order to support emerging areas of science and technology. Salary increases are required to recruit and retain staff in all divisions, but this issue is especially acute in the biosciences, where competition for the best talent is severe. The following areas are essential to maintain and are in danger of disappearing: heat capacity, thermal conductivity, phase equilibria measurements, optical reference standards, optical imaging spectroscopy, primary pH measurements, and high-precision gas standards production. The Analytical Chemistry Division has increased the relative number of postdoctoral fellows in an attempt to partially compensate for this loss of staff; however, this strategy is unhealthy for the long term. The Biotechnology Division continues to operate using a model in which individual principal investigators conduct their research independently, with very little staff support. This model is in stark contrast to that employed by nearly all other laboratories that conduct research in biology-related areas. The CSTL should consider increasing the ratios of technical support staff to Ph.D. investigators in order to improve efficiency. The Analytical Chemistry Division has successfully mitigated budget cuts by a careful analysis and restructuring of its cost recovery system; the other divisions should also critically evaluate cost recovery, where allowable, as a mechanism for increasing revenues to sustain existing efforts and to support new work.

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