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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

Chapter 4

Chemical Science and Technology Laboratory

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

PANEL MEMBERS

Lou Ann Heimbrook, Lucent Technologies, Chair

Arlene A. Garrison, University of Tennessee, Vice Chair

Thomas M. Baer, Arcturus Engineering, Inc.

Alan Campion, University of Texas at Austin

Anthony M. Dean, Exxon Research and Engineering Company

Pablo G. Debenedetti, Princeton University

Robert R. Dorsch, DuPont Life Sciences

Robert E. Ellefson, Leybold Inficon, Inc.

Daniel L. Flamm, The Microtechnology Analysis Group

Walter W. Henslee, The Dow Chemical Company

Wayne O. Johnson, Rohm and Haas Company Research Laboratory

Roy S. Lyon, National Food Processors Association

James D. Olson, Union Carbide Corporation

James W. Serum, Hewlett-Packard Company

Jay M. Short, Diversa, Inc.

Christine S. Sloane, GM Research and Development Center

Anne L. Testoni, Consultant, Hudson, Mass.

Submitted for the panel by its Chair, Lou Ann Heimbrook, and its Vice Chair, Arlene A. Garrison, this assessment of the fiscal year 1999 activities of the Chemical Science and Technologies Laboratory is based on site visits by individual panel members, a formal meeting of the panel on March 2–3, 1999, in Gaithersburg, Md., and documents provided by the laboratory.1,2

1  

U.S. Department of Commerce, Technology Administration, National Institute of Standards and Technology, Chemical Sciences and Technology Laboratory Annual Report 1998, National institute of Standards and Technology, Gaithersburg, Md., 1999.

2  

U.S. Department of Commerce, Technology Administration, National Institute of Standards and Technology, Chemical Science and Technology Laboratory Technical Activities 1998, NISTIR 6273, National Institute of Standards and Technology, Gaithersburg, Md., 1999.

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

LABORATORY-LEVEL REVIEW

Laboratory Mission

According to laboratory documentation, the mission of the Chemical Science and Technology Laboratory (CSTL) is to provide the chemical measurement infrastructure to enhance U.S. industry's productivity and competitiveness; assure equity in trade; and improve public health, safety, and environmental quality.

This mission statement fully reflects the mission of NIST to promote economic growth by working with industry to develop and apply technology. The goals and objectives of the laboratory mission are consistent with establishing the CSTL as the nation's leader in chemical and physical measurements in chemistry, chemical engineering, and biotechnology.

The CSTL has defined and documented criteria for assessing current and future programs that emphasize the relevance of each program to the stated mission. The strategic planning occurring in the laboratory provides highly effective management of numerous technical programs. The strategic plans include detailed goals and objectives that assure the availability of needed measurement capabilities for U.S. industry, accelerate technological innovations critical to future economic growth, and maximize the synergies between the expertise available within the CSTL and within other laboratories at NIST.

The results from this laboratory, as documented in the divisional reports, show that program evolution and redirection are occurring based on input from external sources, workshops for needs assessment, and a recognition that U.S. industry's technical requirements in standards and measurements are dynamic. The laboratory reallocates resources across CSTL via a variety of mechanisms, including changes in programs supported by outside agencies and turnover in the short-term grants from the NIST Director's Competence Program. The primary mechanism for change within the laboratory is an annual evaluation of all projects against a series of six program assessment criteria: industrial need, match to mission, assessment of how critical the CSTL role is for the success of the work, nature and size of impact relative to investment, timeliness and quality of output, and the opportunity afforded by recent scientific advances to foster mission objectives. The panel observed that these project selection criteria and the importance of maintaining mission relevance are clearly communicated to staff throughout CSTL and that the process is well defined and documented. Although the panel did not review the selection process in more than summary detail, the program portfolio produced by this selection process continues to be reviewed by CSTL and the panel not only to ensure consistency with mission but also to ensure that input from government agencies, international and national standards activities, industry, and the scientific community is appropriately utilized. CSTL is a leader within NIST in the formalization of program continuation and selection criteria, and although its process is only one possible approach to project selection, it is now being looked at as a best practice approach for other NIST laboratories to review. The panel is appreciative of the laboratory's efforts and looks forward to continuous improvement in this process as CSTL refines the tools used for project selection and their application.

The CSTL staff makes every effort to ensure that all available industrial roadmaps are incorporated into their scientific endeavors when appropriate. In addition, NIST staff are highly involved in the development of technology roadmaps for several different industries. For example, the laboratory staff have been leaders in the Vision 2020 program, which is putting

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

together a roadmap for the U.S. chemical industry modeled after the Semiconductor Industry Association (SIA) National Technology Roadmap for Semiconductors (NTRS).

International intercomparability is a key issue for CSTL's main customers, industries such as aerospace, semiconductors, biotechnology, chemical processing, health, and energy. The global nature of these industries, which rely on CSTL Standard Reference Materials (SRMs), calibrations, and other services, requires that CSTL's work be at the best-in-class level to ensure U.S. companies' competitiveness and trade equity. In 1998, the laboratory held a number of workshops to benchmark CSTL capabilities in key areas that have a direct impact on U.S. competitiveness and trade. Discussions of the results are provided in the divisional assessments.

Technical Merit and Appropriateness of Work

The Chemical Science and Technology Laboratory provides leading-edge information to both expanding and more mature industries through work in five divisions: Biotechnology, Process Measurements, Surface and Microanalysis Science, Physical and Chemical Properties, and Analytical Chemistry. The breadth of scientific research and expertise in these divisions reflects the industries served by CSTL, including semiconductor, aerospace, biotechnology, chemical processing, health, and energy. Programs range from work on improving surface- and depth-profiling techniques used to characterize both biological and semiconductor materials, to work in analytical chemistry that increased the focus on international comparability and SRM work, to the excellent large biomolecule structure and sequence database activities. To serve such a broad customer base in an efficient and timely manner, CSTL divisions collaborate with each other and with other laboratories in NIST. The panel found that the technical work continued to provide the highest quality of chemical measurement capabilities and state-of-the-art basic and applied research in a broad range of technical areas.

The laboratory balances development of the essential measurement standards and technologies for current and future technical needs of CSTL customers. The CSTL accounts for 90 percent of the databases provided by NIST's Standard Reference Data Program and by secondary distributors. The NIST Chemistry WebBook, which provides free Internet access to chemical reference data, was enlarged and improved by CSTL this year. This database serves as a resource for kinetics data for 5,000 to 10,000 users per week, 40 to 50 percent of whom are repeat users. The mass spectral library and chemical kinetics databases were also updated and released this year. In 1998, CSTL held workshops to benchmark SI base units of temperature and amount of substance (mole). Future workshops will focus on SI-derived units, including pressure, humidity, flow rate, and others. These workshops showed that many CSTL programs are best-in-class or state-of-the-art when benchmarked against other national measurement laboratories. These results agree with studies conducted in 1997, which demonstrated that CSTL covered a broader metrology scope than any other single institution in Japan, Germany, or Brazil.

The technical merit and management of the programs in CSTL are excellent. The work and staff have been recognized internally, with Department of Commerce Silver and Bronze medal awards, and externally, with various university, scientific, and engineering society awards for excellence. The divisional reports document the technical quality of many of the CSTL staff and the merit of the programs, many of which are recognized throughout the world for their advancement of science and their impact on current and emerging industries.

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
Impact of Programs

The CSTL continued to deliver results to a wide scientific customer base in industry, government, and academia by all conventional means of dissemination. In fiscal year 1998, the laboratory staff published 340 articles in scientific journals (accounting for 17 percent of the NIST total publication effort), and CSTL staff held 63 editorships and 180 committee memberships in standards organizations and helped organize numerous conferences and workshops. CSTL had 10 patents licensed, accounting for 21 percent of the NIST total in fiscal year 1998, and has 29 patents currently active, 6 submitted, 1 awarded, and 19 pending. The laboratory has 21 Cooperative Research and Development Agreements (CRADAs) with industry, accounting for 15 percent of the NIST total. CSTL efforts resulted in the sale of over 24,000 SRMs and over 4,400 Standard Reference Databases (SRDs), which accounted for 66 percent and 90 percent of the NIST total, respectively. Laboratory staff conducted 642 calibrations.

There are numerous examples in the divisional reports of fundamental research that has a long-term impact on industry, often by augmenting research on specific technical needs for current and long-term measurement capabilities. This past year the effort of the laboratory to continue critical programs for industry and to plan for future initiatives has been highly effective. The data clearly reflect that there continues to be an ever-increasing demand for the services provided to industry by the laboratory.

CSTL conducted several economic impact studies in fiscal year 1998, which demonstrate well the effectiveness of the work of the laboratory on the economic growth of U.S. industry. For example, an independent economic assessment of the alternative refrigerants program based on a conservative analysis of direct benefits to manufacturers of refrigerants and refrigeration equipment yielded a cost/benefit ratio of 3.9 and an internal rate of return of at least 433 percent. Economic impact studies currently under way in the laboratory include evaluations of the CSTL work on the SRMs for cholesterol measurements, DNA profiling, and sulfur in fossil fuel.

The laboratory has also improved its dissemination of technical information. CSTL continues to increase utilization of the Internet to disseminate information, as highlighted by the Chemistry WebBook. The quality, format, and organization of the Web pages for CSTL vary from division to division, sometimes from project to project. The panel believes that ways to standardize the sites and increase the ease of use should be explored at the laboratory level.

The panel was pleased to see an updated release of the kinetic database and increased distribution of the NIST/Environmental Protection Agency (EPA)/National Institutes of Health (NIH) Mass Spectral Library. The impact of the dissemination of this scientific information will be felt across multiple scientific fields. The databases are enabling technologies for scientific analysis of materials and compounds requiring spectroscopic evaluation. The NIST Traceable Reference Materials (NTRM) Program is an excellent example of the ongoing effort of the CSTL to provide traceable resources to a broad spectrum of industries without placing an undue burden on laboratory staff. Further observations about the NTRM Program are provided in the section on the Analytical Chemistry Division.

Two CSTL projects exemplify the laboratory's impact on U.S. industry. DNA measurements and standards have had a major impact on the forensic use of DNA technology. The FBI and other crime laboratories requested a suitable SRM in 1988, and the first DNA-profiling SRM was released in 1992. SRM 2390 received an R|andsymbol|D 100 Award and was a major factor in the establishment of the DNA Advisory Board through the 1994 Crime Bill. Accuracy

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

of human identification through DNA analysis was enhanced in 1995 by the release of an updated reference material, SRM 2391. Additional support is provided with a Short Tandem Repeat DNA Internet database. Forensic identification and medical detection were enhanced by the production of SRM 2392, the first mitochondrial DNA standard. Anecdotal support, as well as strong sales of the SRM, continue to provide evidence of the value of this activity to society, both in the conviction and exoneration of individuals accused of crimes. An authoritative economic impact evaluation of the DNA SRMs is under way.

Alternative refrigerants came to the attention of the public and scientific community with the Montreal Protocol in 1987. Industry needed property data and design tools to identify the most likely replacement working fluids to replace chlorofluorocarbon and hydrochlorofluorocarbon refrigerants. CSTL has had 40 years of experience in fluid properties and possesses the capabilities to make experimental measurements over a broad range of temperature and pressure. In addition to providing data and models, the laboratory staff created a database of refrigerant properties (REFPROP), which provides easy access to property data on numerous pure fluids and a range of mixtures for engineers and researchers. The information has been adopted as an industry standard and is distributed through a number of professional and technical organizations, including the Air-Conditioning and Refrigeration Institute, the American Society of Heating, Refrigerating and Air-conditioning Engineers, and several companies.

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
Laboratory Resources

Funding sources3 for the Chemical Science and Technology Laboratory (in millions of dollars) are as follows:

 

Fiscal Year 1998

Fiscal Year 1999 (estimated)

NIST-STRS, excluding Competence

37.8

39.0

Competence

2.0

2.4

ATP

3.0

2.8

Measurement Services (SRM Production)

2.3

2.1

OA/NFG/CRADA

9.6

12.6

Other Reimbursable

3.0

2.8

Total

57.7

61.7

As of January 1999, staffing for the Chemical Science and Technology Laboratory included 276 full-time permanent positions, of which 240 were for technical professionals. There were also 127 nonpermanent and supplemental personnel, such as postdoctoral research associates and part-time workers, in addition to 229 guest researchers.

Positions opened by previous retirements led to significant hires in 1998 in CSTL management and technical positions. Excellent candidates were identified through aggressive advertising, and key hires were made in a timely fashion. CSTL researchers are involved in several interlaboratory projects. The panel was pleased to note that the appropriate division and laboratory resources were allocated to these projects and that additional incentives were not necessary to encourage such activities.

The majority of the laboratory funding is from internal NIST sources, though other agency funding was received from the Air Force, Navy, Army, National Aeronautics and Space Administration (NASA), Health and Human Services, EPA, Department of Energy, Department of Commerce, Defense Nuclear Agency, and others. The diversity of OA funding shows the broad scope of work undertaken by the laboratory and reduces the dependence on outside funding from any one agency.

The ability to do world-class measurements attests to the caliber of the facilities, equipment, and human resources allocated to the CSTL projects. Building I-B at the Center for Advanced Research in Biotechnology (CARB) was finished in 1998, adding 28,000 square feet

3  

The NIST Measurement and Standards Laboratories funding 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 it is allotted 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 governmental (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.

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

for biotechnology research to the original CARB facility. Construction was completed on the Advanced Chemical Sciences Laboratory (ACSL), which will provide 82,000 square feet of state-of-the-art laboratory and office space. Relocation of the Analytical Chemistry Division and the Biotechnology Division is occurring throughout 1999.

Facilities improvement continues to be a major issue for the three remaining divisions: Process Measurements, Surface and Microanalysis Science, and Physical and Chemical Properties. Relocation of selected groups from these divisions to the Advanced Measurement Laboratory (AML) is essential. Although it is anticipated that NIST's fiscal year 2000 congressional appropriations will allow construction of the AML to begin, the anticipated completion date is at least 5 years away. Refurbishment of the existing buildings must begin as soon as possible, and CSTL must develop a facility plan to address the period prior to completion of the AML.

Concerns regarding capital equipment funding for specific programs appear in the divisional reports. In general, though, the operational lifetime of scientific hardware is highly limited, and funding must be carefully monitored to assure that needed funds are being appropriated to the key areas to maximize the impact to U.S. industry.

DIVISIONAL REVIEWS

Biotechnology Division
Division Mission

According to division documentation, the mission of the Biotechnology Division is to provide measurement infrastructure necessary to advance the commercialization of biotechnology by developing the scientific/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.

A challenge to the division is the rapid growth of biotechnology, where entirely new approaches can be invented, commercialized, and become obsolete in fewer than 5 years. In light of this situation, the division does an excellent job of meeting its mission. The panel suggests that the division may wish to consider adding the words “create” and “use” to “provide” at the beginning of the mission statement. This modification reflects the breadth of effort in the division, where the work ranges from fundamental research to the development of important standards materials and methods.

The division has established a variety of long-range research programs to maintain critical expertise needed for the development of advanced measurement methods, SRMs, and databases for use by industry and other research enterprises. These activities foster collaboration among NIST scientists conducting biotechnology research and raise the quality and visibility of the NIST biotechnology program, which leads to enhanced collaborations with industry, universities, and other government agencies.

The dynamic nature of the biotechnology-related industries requires an evolving Biotechnology Division that strengthens selected existing programs while developing new technical expertise in emerging areas. The division participates in the annual laboratory-wide reprogramming activity in which current and proposed projects are quantitatively ranked

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

according to specified criteria, such as industrial requirements and match to mission, in order to allow CSTL programs to evolve in response to changing measurements and standards needs and to take advantage of new technologies. This process has successfully allowed the Biotechnology Division to build an appropriate portfolio of activities; however, the panel believes that the division could more fully exploit available opportunities by:

  • Expanding the DNA technologies effort to match the commercial demand;

  • Emphasizing specific biomolecular surfaces and model systems useful to U.S. industries, e.g., sensors, diagnostics, and pharmaceutical research;

  • Building expertise in bioprocessing and focusing on developing measurement techniques and reference data for the bioprocessing industry; and

  • Emphasizing the expansion in bioinformatics related to the Protein DataBank.

Technical Merit and Appropriateness of Work

The Biotechnology Division comprises four groups: DNA Technologies, Bioprocess Engineering, Biomolecular Materials, and Structural Biology. The following section discusses some of the key programs and issues ongoing in these areas.

The DNA Technologies Group engages in DNA and molecular biology research to enhance measurement technologies in mutation detection and genetic toxicology and to provide SRMs relating to the detection and characterization of DNA. The work conducted in DNA technologies in general, and bioinformatics especially, seems very compelling based on the global utility of these technologies.

Use of short tandem repeats (STRs) by crime laboratories throughout the world is rapidly becoming the standard method of human identification. Continued collaboration between the division and the forensic testing community led to development of a NIST Web site providing information on STRs, including a database of all currently used genetic testing systems. SRMs developed and supplied by the group continue to be a critical component of this methodology. Completion of interlaboratory testing occurred in 1997 for the new SRM 2392 for human mitochondrial DNA, and in fiscal year 1998, validation and sequencing studies were completed. Production of SRM 2392 is scheduled for 1999.

The DNA Technologies Group has developed molecular-scale methods to characterize DNA damage at levels approaching one base pair per million. The group has used these methods to study the kinetics and specificity of DNA repair by newly discovered enzymes. It also uses this technique to quantify cell death and DNA damage resulting from administration of individual and combined drugs for human immunodeficiency virus treatments.

The Bioprocess Engineering Group focuses on the development of measurement methods, databases, and generic technologies related to the use of biomaterials in manufacturing. Protein biospectroscopy measurement methods and data have been developed that will lead to improved understanding of intra- and interprotein electron transfer processes. A new initiative to develop fluorescence intensity standards has also been launched this year in response to industry and government needs. This program is consistent with the mission of developing improved standards and supports the general trend in biotechnology and medical diagnostics to provide quantitative measurements.

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

Chromatography and microcalorimetry measurements have been combined with chemical equilibrium analysis to study the biothermodynamics of enzyme-catalyzed reactions in industrially important biotransformations, such as the metabolic pathway to chorismate (converting glucose to aromatic amino acids). Such analyses supply a critical source of data to process engineering for the chemical, agricultural, and pharmaceutical industries not accessible from industrial or academic sources. For this program to meet the long-term needs of companies in these areas, it will be important to continue to emphasize industrial needs, which can best be understood through close industrial relationships and collaborations, analysis of Web site hits, attendance at workshops, and meetings to provide an ongoing assessment of the NIST program. The panel encourages further collaboration with molecular groups within NIST and CARB to assist in both defining needs for targeting future efforts and refining communication on the value of this type of data to the target industrial audience of bioprocess engineering.

Research projects in biocatalytic systems focus on enzyme characterization by site-directed mutagenesis, 15N nuclear magnetic resonance (NMR) spectroscopy, x-ray diffraction of protein crystals, and computational chemistry. These techniques are being used to address focused, industrially important biotransformation problems such as hydroxylation and aromatic amino acid metabolic pathways.

The Biomolecular Materials Group examines control over biological molecules at interfaces. Chemically controlled surfaces engineered for specific biomolecular interactions are essential components of biosensors, bioelectronics, biocatalytic systems, and many diagnostic devices. The group has made progress in this research by fabricating a rugged artificial membrane system, composed of both artificial and natural lipid components, which mimics cell membranes. This unique membrane matrix is important both as a research tool and potentially as a commercial development. The group has progressed in research on the chemistries needed to attach the lipids to a surface.

The group has also developed infrared (IR) ellipsometry and neutron reflectivity techniques to explore structural characteristics of biological molecules such as cell membrane receptors, optically active proteins, and redox enzymes and the relationship between structure and functional activity. Molecular structure information is also provided by IR and surface plasmon resonance-enhanced Raman spectroscopies and by nonlinear optical spectroscopies. Genetically engineered proteins are used in systematic studies of how structural changes in membrane proteins lead to functional changes. An important challenge for the group is to focus on developing new standards and measures of membrane systems for the pharmaceutical, medical diagnostic, and biotechnology industries.

The division's Structural Biology Group, housed at CARB, focuses on four key areas of industrial biotechnology: macromolecular structure determination by x-ray crystallography; molecular structure and dynamics elucidation by high-field NMR spectroscopy; physical, molecular, and cellular biochemistry; and computational biochemistry and modeling. CARB established close links in fiscal year 1998 with several local industrial organizations, such as the Institute for Genomic Research (the world leader in genomic sequencing) and Life Technologies, Inc.

A new area of focus for the x-ray crystallography and modeling groups has been the enzymes involved in the chorismate pathway. This effort is part of a division-wide activity aimed at the vitally important industrial area of metabolic engineering.

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

The group has begun a new enterprise to construct a comprehensive database for molecular recognition. An initial area of focus, recommended at two workshops by academic, government, and industrial scientists, is on calorimetry data as applied to host-guest interactions.

Impact of Programs

It is clear to the panel that this division will have a significant impact on the biotechnology industry. For example, the Bioinformatics Group has the potential to generate significant economic impact through sequence, functional, and structural data analysis. The level and size of the industrial need in this area is so great that it will be essential for the division to maintain its focus on areas of greatest impact.

The panel is impressed by the effectiveness of the division's dissemination of scientific accomplishments. It published 96 manuscripts in 1998, ranging from protein structure determination to methods for p53 mutation analysis. The group has been active at numerous professional conferences and sponsored workshops, including the Workshop on Calorimetry. The group organized a well-attended workshop, “Standards for Nucleic Acid Diagnostic Applications,” to determine appropriate standards for nucleic acid diagnostics needed by the emerging molecular diagnostics community. Presentations at this meeting covered specific standardization needs common to molecular diagnostic instrumentation, as well as methods to assist this community in measurement techniques and critical quality assurance procedures. NIST staff have also established and maintained a number of Internet databases such as the STR DNA Database and the Biological Macromolecule Crystallization Database (BMCD), and they have cross-referenced the BMCD with the Nucleic Acid Database at Rutgers University. The efforts in this area are outstanding, and the panel encourages NIST to continue this work at the current level.

The panel believes that the Biomolecular Materials and Bioprocess Engineering Groups need to strengthen external discussions to generate a more broadly informed view of industrial needs. They will need to form partnerships or consortia with leaders in these fields to have the greatest impact on U.S. commerce.

The new, state-of-the-art laboratories in CARB I-B were completed, equipped, and occupied in fiscal year 1998. Over 200 scientists from academic, government, and industrial laboratories attended an unveiling symposium, which focused on important issues in structural biotechnology. Additionally, the space will house temporarily the new Protein Data Bank, which has been awarded to the Research Collaboratory for Structural Bioinformatics (RCSB), a collaboration initiated by the division in fiscal year 1998. This year's efforts have focused on interactions with scientists from Rutgers University, the University of California San Diego Supercomputer Center, and the NIST SRD Program. This organization provides a unique framework for the development of Web-based resources of general interest to the academic, private, and industrial research communities. The RCSB will assume the responsibilities of managing and distributing the Protein Data Bank during fiscal year 1999.

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
Division Resources

Funding sources for the Biotechnology Division (in millions of dollars) are as follows:

 

Fiscal Year 1998

Fiscal Year 1999 (estimated)

NIST-STRS, excluding Competence

6.6

7.1

Competence

0.9

0.8

ATP

1.9

1.8

Measurement Services (SRM Production)

0.0

0.1

OA/NFG/CRADA

0.9

1.8

Total

10.3

11.6

As of January 1999, staffing for the Biotechnology Division included 37 full-time permanent positions, of which 34 were for technical professionals. There were also 42 nonpermanent and supplemental personnel, such as postdoctoral research associates and part-time workers.

To have any measurable impact, the panel believes that significant growth in the staff in the area of bioinformatics is necessary. The DNA Technologies Group will need significant capital equipment resources to develop standards useful for the latest generation of sequencing and synthesizing instrumentation if it is to continue to be effective.

Process Measurements Division
Division Mission

According to division documentation, the mission of the Process Measurements Division is to develop and provide measurement standards and services, measurement techniques, recommended practices, sensing devices, instrumentation, and mathematical models required for analysis, control, and optimization of industrial processes. Research is directed to uncover fundamental knowledge related to chemical process technology and to generate essential data in this field. Efforts include the development and validation of predictive computational tools and correlations, computer simulations of processing operations, and requisite chemical, physical, and engineering data.

The panel believes the division's goals and projects are generally consistent with this mission statement. Moreover, the division effectively conforms to the NIST mission by meeting the needs of U.S. industry and the public. This division makes a significant contribution to the promotion of U.S. economic growth through partnership with industry by sustaining an impressive array of international benchmarking and cooperative programs and by holding timely workshops in important contemporary technical areas.

A variety of short- and long-term review processes continue throughout the year and scrutinize each project. The cycle includes outside assessments, staff proposal reviews, preliminary assessment of new proposals, reprogramming, and identification of areas to

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

emphasize and deemphasize. The laboratory appears committed to making this an annual process, and the panel applauds this effort. Longer-term strategic planning is undertaken at all levels of management, from group leader to laboratory director. This range of input is a key part of a generally commendable planning process. The panel encourages the division to gather input from companies as well as the open literature when assessing its project evaluation tools. The current selection matrix may not provide an ideal or realistic process for evaluation. The panel encourages the use of “sanity checks” in the use of any tool for project prioritization but believes that the exercise of assigning numerical scores does promote useful discussion among researchers and managers.

Technical Merit and Appropriateness of Work

Widespread demand for the division's calibration services in pressure, humidity, vacuum, temperature, and flow is a positive index of the quality of its work. The panel was most impressed by the forward-looking work in the areas of microhotplate sensors, biosensors, and self-assembling monolayers (SAMs); the implementation of the International Temperature Scale of 1990 (ITS-90) thermometry scale; and the programs directed toward humidity standards, verification, and measurement. Below, the panel discusses other highlights of the division's programs and also comments on the general activities of each of the Process Measurements Division's five groups: Fluid Flow, Thermal and Reactive Processes, Process Sensing, Thermometry, and Pressure and Vacuum.

The Fluid Flow Group makes effective use of computational fluid dynamics (CFD) to analyze various flow problems, such as irregularities in flow through realistic fluid delivery systems. The calibration and testing facilities have been upgraded as part of a multiyear effort to improve accuracy and automation of primary gas flow standards. A new design for flow testing in the 1 to 100 liters per minute flow range was built in 1998 and is in validation testing. Improved test precision and reliability have been demonstrated for the high-flow-volume system. The new computer-controlled design for intermediate flows should increase calibration throughput using automated testing runs. Additionally, the group has taken advantage of NIST telepresence calibrations to carry out controlled calibrations at remote sites.

The High Temperature Processes and Reacting Flows Groups were consolidated into the new Thermal and Reactive Processes Group during fiscal year 1999. The panel views this as an artful reprogramming driven by the loss of staff and evolving program priorities. A number of existing projects continue this year, including the development of Raman spectral standards, for which three glass matrices were selected as candidate Raman intensity calibration standards. The Rotating Disk Chemical Vapor Deposition Reactor project studying particle growth, nucleation, and transport has continued to examine particle and chemical kinetics in a simplified flow system. The panel notes that preparation of test apparatus has continued for 2 years along with theoretical work on modeling of transport and particles for this reactor; experimental data and comparisons with the existing data and theory should be forthcoming within the next year. In other work under way, initial measurements of the heat transfer properties of supercritical carbon dioxide were made over a wide range of operating conditions on a counterflow heat exchanger constructed specifically for NIST work on supercritical fluid processes.

The group's instrumented spray combustion test apparatus is a unique facility, but there are not enough scientists assigned to this apparatus to safely and adequately conduct the tests. A possible solution would be for the division to bring in industrial partners to help operate the

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

facility. Allowing companies to simulate proprietary burner designs and conduct tests using realistic feedstocks rather than model fuels such as methanol might induce industrial participation. Such collaborations would require the laboratory to modify the experimental guidelines and objectives of the NIST work. For example, attempts to develop detailed characterizations to correspond to CFD modeling and kinetic computations would have to be replaced with a more engineering-driven approach using dimensional analysis and statistical correlation to produce more immediate operating guidelines, which would be valuable to industrial partners in the near term. The Process Sensing Group has developed arrays of chemical sensors, based on microhotplate technology, to measure characteristic changes in conductivity driven by adsorbed gas species. These arrays, which will ordinarily have built-in redundancy in the form of spare elements that can be activated as necessary, offer the promise of detecting specific gases with a small, inexpensive sensor. This technology has vast potential: small, rugged sensors that measure composition of matter for a few hundred to a few thousand dollars could revolutionize process control technology in the petrochemical, food-processing, semiconductor, pharmaceutical, pulp and paper, and agricultural chemical industries. Proof of principle has already been demonstrated. Further development of the sensor, development of satisfactory reliability metrics, and technology transfer to an industrial partner are the next necessary steps for creation of a viable product.

The Process Sensing Group is also attempting to use SAM as a building block for biosensors. The group has made significant progress in preparing samples and in understanding and probing the structure and chemistry of SAM surfaces. This work has led to excellent collaborations with key researchers and major commercial developers of biosensors. Resources for continued development of these sensors should be a priority for an area that offers another exciting opportunity for CSTL.

The group has conducted an extensive research effort in using radio-frequency (RF) measurements and laser-induced fluorescence to determine plasma uniformity and ion flux characteristics in semiconductor etching applications. Modeling of plasma ion dynamics and details of chemical kinetics are needed to understand fine-line, as well as “lower-tech, ” plasma etching and cleaning techniques for process chambers. This effort has provided some provocative insight and an important interface with other research and development groups. The panel believes that this is an important competency area and should be continued at its present level.

Cavity ring-down spectrometry (CRDS) for water vapor and other trace gas analysis progressed to the point where commercialization could be evaluated. The humidity generation and measurement group currently is building a second CRDS system to validate water vapor measurement capability. The NIST researchers intend to assist with commercialization. The panel believes it may now be time for a thorough assessment of this project, involving CSTL personnel, potential outside users of the technology, and instrument manufacturers.

The Thermometry Group continued its commendable efforts toward realization of the ITS-90 temperature scale over a broad range of temperatures using standard platinum (Pt) resistance thermometers and new rhodium/Pt and Pt/palladium (Pd) alloy thermocouples (wires and thin films). A clever extension of NIST-developed thin film Pt/Pd thermocouple technology has been to deposit a temperature measurement grid on the back side of semiconductor wafers, enabling a direct comparison between radiometric and thermometric temperature measurements for rapid thermal processing (RTP). The instrumented test wafer becomes a practical tool for in situ calibration of optical pyrometers used for mass production RTP. This calibration is essential

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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to assure reproducibility and is vitally important for transferring a process developed on one RTP tool to another. Semiconductor equipment manufacturers have already shown an active interest in this development.

Two coupled thrusts in the Thermometry Group are to measure humidity using various gravimetric and instrumental techniques along with a strong program to develop methods for generating known humidity levels. Particularly noteworthy is the use of the low frost point generator to test the newly developed cavity ringdown method and comparisons between these measurements and commercial frequency-modulated IR absorption instruments. These techniques are capable of generating and quantifying the parts per billion (nanomole/mole) humidity levels that are becoming vital to the semiconductor industry (as documented in the SIA Roadmap). The researchers are working with instrument companies and gas vendors to develop commercial implementation of this leading-edge technology. This is a continuing and meritorious project.

The Pressure and Vacuum Group supports calibration of low pressures important for vacuum and low-flow-rate measurements. Research on partial pressure measurement is an appropriate and important continuing focus, designed to assist the semiconductor and other industries. World-class pressure gauge calibration covering 10-8 Pa 106 Pa is carried out using diverse pressure-generating and measurement technology such as ultrasonic manometry and dead weight testers. A new low-flow-rate automated calibration apparatus is near completion. Cross-calibrations of flow devices across overlapping ranges were done successfully this year between the Pressure and Vacuum Group and the Fluid Flow Group. Qualification of flow element structures as a field calibration flow element was also demonstrated in fiscal year 1998, making NIST-traceable flow calibration available in the field.

The panel believes that the group should establish a presence in mass flow controller (MFC) calibration and response specification metrology for the semiconductor industry. MFCs are an important component in virtually all semiconductor manufacturing equipment, and this metrology is not done well elsewhere. Although Semiconductor Equipment and Materials International, an industry association, has published some specifications in this area, they are often written by industry “volunteers” rather than high-level metrology scientists. This is a natural project for the division and could have high impact and visibility.

Evaluation of residual gas analyzers for partial pressure measurement is a continuing research activity in the group. The research was extended this year to closed ion source (CIS) mass spectrometers. An important target for CIS use is sampling semiconductor processes. Field evaluation of CIS analyzers on a WF6/H2 tungsten deposition machine at the University of Maryland is appropriate, and relevant research should be continued.

Impact of Programs

The panel was pleased to see profuse dissemination of results and databases on the Internet. However, this effort is likely to consume significant technical manpower, especially as each group appears to independently develop and maintain its own Web page. The Process Measurement Division, as well as CSTL and NIST in general, would benefit from uniform standards and reusable software for this purpose. In addition, attention to human interface standards and increasing user-friendliness would make information more accessible and stimulate widespread deployment throughout the industrial and scientific community.

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

The panel found many indications of the positive impact divisional programs have on industry. Examples such as publications, work with consortia, industrial visits, hits on the division's Web sites, and extensive use of calibration services are all evidence that this division reaches out to industry and that companies are aware of and use NIST products. However, data on such activities do not quantitatively measure the value of divisional projects to industry. An evaluation system should include diverse input and support.

Division Resources

Funding sources for the Process Measurements Division (in millions of dollars) are as follows:

 

Fiscal Year 1998

Fiscal Year 1999 (estimated)

NIST-STRS, excluding Competence

8.1

8.6

Competence

0.6

0.8

ATP

0.3

0.2

Measurement Services (SRM Production)

0.1

0.0

OA/NFG/CRADA

0.4

0.9

Other Reimbursable

1.2

1.1

Total

10.7

11.6

As of January 1999, staffing for the Process Measurements Division included 59 full-time permanent positions, of which 53 were for technical professionals. There were also 12 nonpermanent and supplemental personnel, such as postdoctoral research associates and part-time workers.

Flat budgets coupled with increased costs have made staffing levels an issue in the Process Measurements Division; the allotted manpower for some projects is below the level necessary to sustain quality work. Though the division is making excellent use of temporary staff such as postdoctoral research associates and guest researchers, projects often suffer when such temporary help leaves. The panel applauds management's strategy to terminate weaker programs rather than making across-the-board budget cuts.

The general-purpose laboratory equipment available to Process Measurement Division researchers is comparable with that in industrial laboratories, but the specialized equipment is significantly better. The array of tools is adequate for current programmatic needs. In at least two groups, automated calibration apparatuses are being built to improve precision and be less manpower-intensive, which should improve productivity.

As discussed elsewhere in this chapter, the current physical plant remains an impediment to calibration and research efforts. Problems with the physical facilities include limited availability of space, inadequate climate control, and copious airborne particulates. Electrical power outages, in particular, are having a serious effect. The multidegree temperature fluctuations in the Pressure and Vacuum Group laboratories interfere with the ability to conduct research and have often aborted calibrations in progress. The problems are critical and occur too

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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frequently. Although this group will be moved into a temperature-controlled facility in the new Advanced Measurement Laboratory (AML) in several years, the problem is very serious and demands near-term solution.

Surface and Microanalysis Science Division
Division Mission

According to division documentation, the mission of the Surface and Microanalysis Science Division is to serve as the nation's reference laboratory for chemical metrology research, standards, and data to characterize the spatial and temporal distribution of chemical species and to improve the accuracy, precision, sensitivity, and applicability of surface, microanalysis, and advanced isotope measurement techniques.

The mission statement of the Surface and Microanalysis Science Division is appropriate and is consistent with the CSTL and NIST missions. The panel notes that the division would benefit from specific, measurable goals or a roadmap of technical development. Such goals and roadmaps would allow the division to determine whether it is fulfilling its mission. The panel believes that the importance of the support that the division provides to national security could be mentioned in either the mission or vision statements.

The Surface and Microanalysis Science Division effectively uses externally developed roadmaps such as the SIA Roadmap, the Chemical Industry Technology Vision 2020, and the OIDA Roadmap to understand and respond to future industry needs. Given the lack of a roadmap for atmospheric chemistry metrology, it would be appropriate for the division's Atmospheric Chemistry Group to coordinate requirements for material standards and compliance measurements with the U.S. EPA.

The division plans its activities each year using the standard criteria of the CSTL, covering industry needs, degree of impact, and new scientific opportunities. CSTL guidelines for reprogramming provide opportunities for the introduction of new projects and encourage the termination of completed or less successful work. This process for project selection ensures that new projects respond to the changing needs of the division 's customers. It is not clear, however, how ongoing projects are evaluated for progress—in particular, for how well they are meeting explicit and quantitatively defined customer requirements. The panel therefore recommends that the division develop and evaluate annual project metrics and milestones.

Technical Merit and Appropriateness of Work

The Surface and Microanalysis Science Division continues to perform extremely high-level and high-quality research on the spatial and temporal distribution of chemical species in heterogeneous systems. It is the foremost national laboratory of its kind in the world. Several projects and staff were given significant awards: the CSTL Technical Achievement Award for SRM 2806 - Medium Test Dust in Hydraulic Fluid, the Department of Commerce Bronze Medal, and a Maryland Distinguished Young Scientist Award. The entire division earned the National Defense Meritorious Unit Citation “in recognition of . . . exemplary contributions as a member of the Air Force Technical Applications Center Materials Product Team throughout the past five

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

years.” The following section of the report discusses highlights and issues relating to specific programs under way in the division's four groups: Microanalysis Research, Analytical Microscopy, Atmospheric Chemistry, and Surface Dynamical Processes.

The Microanalysis Research Group performs leading-edge work in electron and x-ray beam microanalysis. To respond to the greatest industry need, the group focuses on the most popular instrumental methods. For example, existing reference materials and calibration techniques for Auger electron spectroscopy (AES) and x-ray photoelectron spectroscopy (XPS) are inadequate for modern standards of precision and accuracy. Group researchers are performing critical theoretical and experimental investigations on the inelastic mean free path of electrons in solids to improve quantitative analyses. This work has been heavily cited worldwide in surface analysis journals. The high-resolution AES instrument that is currently being acquired will also allow state-of-the-art analyses for industry, government, and academic collaborators and will provide high-quality data for the Process Measurement Division 's research work.

The group, in collaboration with the NIST Electronics and Electrical Engineering Laboratory, continues to play a critical role in understanding the effects of reduced excitation voltages on x-ray emission cross-sections for the development of high-resolution x-ray spectrometers. The measurements of chemical shifts in x-ray spectra using these detectors will provide standard spectra and enable chemical state analyses at very high spatial resolution, which should revolutionize x-ray spectroscopy of nanometer-scale particles and ultrathin films. The group deserves credit for recognizing and developing this important application of technology invented in another NIST laboratory; it is an excellent example of the collaboration that exists across laboratories at NIST. The panel hopes NIST staff will be involved in the commercialization of this technology.

The Microanalysis Research Group has also been active in the development of new applications of existing instrumentation, such as backscatter electron diffraction (BSED) and grazing-angle XPS. BSED is an emerging method for performing crystallography with a scanning electron microscope on particles that are not amenable to analysis by other techniques. This method will have strong impact on the semiconductor and catalysis industries. Grazing-angle XPS shows strong promise for the characterization of ultrathin films (often inhomogeneous) such as gate dielectrics in the semiconductor industry. The research is currently being conducted using synchrotron radiation at the National Synchrotron Light Source in New York, but future work could result in the modification of commercially available instrumentation for onsite analyses.

The Microanalysis Research Group's reference material to validate proficiency in testing asbestos levels is important in the certification of laboratories across the nation. The group is also developing SRMs for critical surface and particle composition for the semiconductor manufacturing, steel, and aerospace industries. The panel encourages the group to continue this sort of work and release more of these standards in the near future.

The Analytical Microscopy Group performs state-of-the-art research on ion and photon microprobe analysis. The staff perform remarkably innovative research into ion microprobe analysis of materials and have very strong collaborations with industries, especially in semiconductor manufacturing and process development. Work in this group provides critical support to monitoring of nuclear materials worldwide.

The premier program within the group is the development of new standard materials and measurement methods for secondary ion mass spectrometry (SIMS). A key accomplishment in 1998 was the installation and start-up of a time-of-flight (TOF) SIMS instrument. The

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

increasing use of this tool to analyze small particles and organic surfaces underscores the importance of NIST's taking a leading role in the development of quantitative measurement methods. Collaboration with the Physical and Chemical Properties Division to incorporate TOF-SIMS data into the mass spectral database would assist industry in obtaining needed data.

Traditional SIMS instrumentation is no longer able to make critical implantation measurements in semiconductor applications. A technical highlight for 1998 was pioneering research into the generation and use of polyatomic primary ion beams to improve SIMS analysis of semiconductor and organic materials. The group collaborated with an instrument company to develop an SF5+ source that can be retrofitted onto common SIMS instruments. This new source doubles depth resolution and reduces overall surface roughness by a factor of 6. The commercialization of this source and the development of new analytical methods will upgrade the large base of instrumentation currently in use, increasing instrument performance, extending instrument life, and saving U.S. industry millions of dollars in new ion mass spectrometry instrumentation purchases. The SF5+ source has also greatly improved the analysis of organic and biological materials. Tests on a model biological system gave yields 10 to 50 times those of traditional SIMS. Successful adaptation of the source for use on TOF-SIMS instruments would produce an extremely powerful method for the static characterization of polymer composition and structure; the panel encourages the group to continue this work.

In collaboration with the Process Measurements and Analytical Chemistry Divisions, the Analytical Microscopy Group has developed a series of candidate frequency and intensity standards for the calibration of Raman spectrometers. Largely because of the recent development of high-aperture Raman spectrometers using charge-coupled device detectors, the use of these instruments has increased greatly, with applications ranging from fundamental science to process analysis and control. The new standards will be increasingly important for comparing results from different instruments.

The work of the Atmospheric Chemistry Group on advanced isotope metrology and chemical measurement processes continues to be the standard for world-class excellence. The group is continuing to develop its unique capability to specify the source of carbon emissions. A result of this effort is the development of techniques for microanalysis of particles, multi-isotopic speciation via gas chromatograph/accelerator mass spectrometry, and compound-specific IR/mass spectrometry are under development. Isotopic profiling brings an interesting new dimension to resolution of fossil fuel emission sources, such as transportation sectors and power generation. The multiagency cooperative Denver Front Range Brown Cloud study completed a field application of fossil/nonfossil fuel particulate discrimination in ambient samples in 1998. The fossil and nonfossil contributions were resolved as a direct result of this group.

The Atmospheric Chemistry Group has also identified and created needed reference materials to provide traceability for environmental measurements. To resolve the fossil and nonfossil origins of CO2, NIST staff developed a novel check on the accuracy of isotope ratio (m/z) measurements by improving the value assignments of isotopic reference materials. This allowed the evaluation of the m/z = 47 isotopic distribution two ways, with the comparison serving as a check on accuracy. Furthermore, the CO2 reference materials provide a check on stable isotope measurements (13C and 18O), which do not themselves discriminate fossil from nonfossil, as does 14C. These developments will allow further discrimination of sources within the fossil and nonfossil classes.

Three events improved traceability of environmental measurements in 1998. Interactive, Web-based standard test data have been established for scientists to evaluate their XPS analysis

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

software and understand the uncertainties in their XPS analyses. The ozone standard reference photometer was upgraded in design, and a parallel system was installed in Spain to provide globally consistent traceability for regulatory compliance. Lastly, techniques were demonstrated to create a reference filter sample for calibration of ambient particulate field measurements, used to evaluate compliance with U.S. ambient air quality standards. A calibration reference is a key need in this area.

The Surface Dynamical Processes Group continues to perform excellent work in the development and application of molecular spectroscopy methods to the study of surface-mediated processes. The studies of gas-surface dynamics are now emphasizing selective generation of radicals and ions and their interactions with surfaces of technological importance. Initial measurements of the reactions of hyperthermal hydrogen and deuterium atoms with silicon surfaces have demonstrated the power of the approach. This work provides reaction mechanisms and rate constants for the continuing development of process models for chemical vapor deposition and plasma etching in the semiconductor and other materials synthesis industries.

The group has initiated a pioneering effort to develop complementary vibrational spectroscopies with subwavelenth spatial resolution. The panel believes that the group is ideally suited to meet the many challenges of this high potential payoff project and that its approach, to develop both IR and Raman near-field scanning optical microscopy (NSOM), is a good strategy. Even if both methods are completely successful, they will be applied to different sets of problems. The collaboration with a DuPont Fellow is typical of the division's improved level of interaction with industry. The development of a broadband IR source is an excellent example of the group's ability to design instrumentation that serves several applications. The source is used for both the IR NSOM and the sum-frequency generation experiments and is a technical accomplishment that should prove useful to the community.

Overall, the panel continues to be impressed with excellence of the division's work and with the degree of collaboration it has established between groups and with other CSTL divisions and NIST laboratories. The panel encourages the division to seek out collaborations with the NIST OMP on projects related to metrology needs of the semiconductor industry. The Surface and Microanalysis Science Division expertise in microscopy, spectroscopy, and data analysis could be leveraged to reduce the time required to deliver key composition and critical dimension standards for the semiconductor industry.

Impact of Programs

The division has changed the focus of metrics it uses to measure its impact; in the past, the metrics addressed its output: papers, presentations, number of new SRMs, and so on. Now the metrics also examine the outcome of the work by recording citations of papers, numbers and types of industrial collaborations (instrument manufacturers versus end users), Web page hits, and national/international acceptance of SRMs. The panel believes that these new metrics are of higher quality and will provide a more realistic measure of impact. The panel also recommends that the division request its industry and government collaborators to provide feedback on the benefit of their interaction. This direct feedback is the highest-quality impact measurement.

The division has used the Internet in its telepresence microscopy activities and in the promotion of the XPS Standard Data Set, but a redesign of the division's Web site could greatly

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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enhance dissemination of its results. It is difficult to locate information known to be posted, and there was no uniform sense of information flow or design. The site could also be updated in a more timely manner. A dedicated resource to design and manage the Web site would greatly assist the division's industrial, academic, and governmental customers.

There were many collaborations during 1998 with instrument manufacturers and members of the semiconductor, oil, biotechnology, and aerospace industries. Expanded use of telepresence microscopy methods will further enable the division to collaborate with and support industrial partners by providing advanced analytical methods without a significant capital equipment investment.

The Surface and Microanalysis Science Division is conducting research that will have a direct impact on many U.S. industries. For example, a significant achievement of the past year was the development and release of SRM 2806: Medium Test Dust in Hydraulic Fluid. This standard was the result of collaboration between the Analytical Microscopy and Microanalysis Research Groups, and it has been accepted by the international standards community. NIST work in this area began in direct response to a request from the National Power Fluid Association, and the resulting SRM fulfills the industry's need for a realistic standard to calibrate particle levels in real hydraulic systems. The ability to perform accurate measurements will benefit the power fluid industry worldwide through improved accuracy and reproducibility of particle measurements, more effective contamination control programs, lower operating and maintenance costs, less system downtime, and increased system reliability. The development of this standard is a significant achievement and would be an excellent candidate for a CSTL economic impact study. The Atmospheric Chemistry Group released SRM 1922, a refractive index standard for the calibration of refractometers. This SRM will aid the sugar industry and any other area that depends strongly on refractometer measurements for process control or materials characterization.

In the Surface Dynamical Processes Group, the development of NSOM-based vibrational spectroscopies is important work, and the results will have a major impact on industry when implemented. Applications of this unique approach range from defect analysis in semiconductor manufacturing to the examination of nanometer-scale structures in heterogeneous biological systems.

The microcalorimeter x-ray detector program, when commercialized, will revolutionize nanoscale particle and ultrathin film analysis for the many industries already involved in this spectroscopy. The panel hopes that a formal collaboration with an analytical equipment manufacturer is established as soon as possible. In the Analytical Microscopy Group, the commercialization of the polyatomic ion sources for SIMS will likewise increase the capability of existing instrumentation and enable new analytical methods to be developed, especially for polymer thin film characterization. This project presents an easy and quantitative means for measuring impact through monitoring the number of sources sold by the industrial research partner.

The panel notes that the Atmospheric Chemistry Group's activities have the potential for even higher impact on U.S. industry and government activities. Recent changes in federal emission standards point to the importance of distinguishing the impact of combustion products from transportation, power generation, agricultural clearing, wood stoves, and cooking. The carbon isotope measurement techniques developed in the division offer more definitive resolution of emission sources within those categories. The coordination with the EPA and

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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environmental laboratories that was utilized in the field studies and reference material development should be extended to the regulatory process and implementation of results.

Division Resources

Funding sources for the Surface and Microanalysis Science Division (in millions of dollars) are presented below:

 

Fiscal Year 1998

Fiscal Year 1999 (estimated)

NIST-STRS, excluding Competence

4.5

4.9

Competence

0.4

0.4

ATP

0.4

0.4

Measurement Services (SRM Production)

0.0

0.1

OA/NFG/CRADA

2.1

2.5

Other Reimbursable

0.3

0.1

Total

7.7

8.4

As of January 1999, staffing for the Surface and Microanalysis Science Division included 36 full-time permanent positions, of which 33 were for technical professionals. There were also 17 nonpermanent and supplemental personnel, such as postdoctoral research associates and part-time workers.

The division continues to rely heavily on other government agencies (OA) for its capital equipment, and external support accounts for a major portion of the budget increase for the division in fiscal year 1999. This is appropriate, as long the division is able to use these resources to fulfill its mission.

There were major changes in the leadership and management of the division this year; there is a new division chief, along with two new group leaders in 1998. Although it would have been preferable to avoid so many leadership changes in a single year, the panel notes that the division remained active and productive and that the transitions were made smoothly and successfully. The attitude of the scientists is very positive; they feel empowered to make a positive impact on the development of new methods and standards for U.S. industry.

In general, the staffing of the division seems appropriate for its mission. There is some concern that the personnel change in the Surface Dynamical Processes Group will have an impact on the group's ability to achieve its technical goals. Also, the panel again observes that the division has limited technical support staff. Skilled scientists are performing equipment and computer maintenance and working on Web pages, and the division's Web site has suffered from the lack of dedicated attention to its upkeep. The Surface and Microanalysis Science Division or perhaps the CSTL should consider hiring a full-time Web site developer.

The instrumental resources of the division are excellent. The Analytical Microscopy Group received the state-of-the-art TOF-SIMS instrument necessary to become a leader in this important new analytical method. The division's suite of instruments will be complete once a high spatial resolution AES system is acquired; the panel encourages the division to finalize this

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

important purchase as soon as possible. Also, the panel recommends that the division develop a multiyear capital equipment plan to match its technology roadmap to help ensure that its critical instrumental resources are sufficient to allow the division to remain best-in-class.

The panel is concerned about the general short-term adequacy of the division's facilities and believes that division and CSTL management need to make basic improvements to the current laboratory space. Although construction of the AML will provide the Analytical Microscopy, Surface Dynamical Processes, and Microanalysis Research Groups with the state-of-the-art laboratory space they require to fulfill their mission, it will be at least 5 years before this space is available. Continuous and prompt investments in basic building systems (HVAC, electricity, air quality, vibration control, water, and safety) should be made in the near future.

The Atmospheric Chemistry Group is not slated to move into the AML with the rest of the division. Its undefined future location and separation from the rest of the division are elements for concern. Further, the continuing air-quality problem constrains technical progress. For example, the 10 µg lower limit on 14C isotope samples is imposed solely by air quality in the NIST laboratory. The panel encourages CSTL management to search for a way to include this group in the AML. If this is not possible, then improved laboratory space should be acquired as soon as possible.

Physical and Chemical Properties Division
Division Mission

According to division documentation, the mission of the Physical and Chemical Properties Division is to be the nation's reference laboratory for measurements, standards, data, and models for the thermophysical and thermochemical properties of gases, liquids, and solids, both pure materials and mixtures; the rates and mechanisms of chemical reactions in the gas and liquid phases; and fluid-based physical processes and systems, including separations, low-temperature refrigeration, and low-temperature heat transfer and flow.

The programs of this division comply with NIST's mission to promote economic growth by working closely with industry. Every group in the division has ties to appropriate industries, but the division maintains a desirable balance between supporting short-term industrial needs and longer-term national science and technology needs. An example of such balance is the recently initiated project on fluid-solid equilibrium modeling by the Theory and Modeling of Fluids Group. Likewise, fundamental studies of fluid flow and heat transfer in microgeometries by the Cryogenic Technologies Group have long-term scientific relevance and important medical applications. The work on the Next Generation Chemical Kinetics Database project accurately reflects industry's need for reliable databases to support detailed process modeling and is consistent with the needs articulated in the chemical process industry's Vision 2020 roadmap.

An appropriate priority-setting process is in place to help laboratory and division management systematically forecast industry needs. This system includes participation in workshops and service to professional societies and standards committees; attendance at conferences and symposia; activities with trade organizations; use of industry roadmaps; and communications with guest researchers, NIST industry fellows, CRADAs, and direct customer contacts. The Physical and Chemical Properties Division uses such input to select and continue projects by considering the magnitude and schedule of the industrial need, match with the

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

division's mission and resources, and the impact that NIST's response would have. The panel believes this mechanism provides excellent and effective priority-setting and project assessment criteria.

Technical Merit and Appropriateness of Work

The Physical and Chemical Properties Division conducts work that is unsurpassed in making fundamental measurements of thermodynamic properties. The research skill level of the scientists and engineers in the division continues to be unexcelled. This is exemplified by several areas in which the laboratory methodology is clearly Best in the World. An example is the multifaceted application of acoustic resonator physics in the Fluid Science Group. The division's activities are split between Gaithersburg and Boulder, and the staff are organized into eight technical groups: Process Separations, Fluid Science, Experimental Kinetics and Thermodynamics, Chemical Reference Data and Modeling, Computational Chemistry, Experimental Properties of Fluids, Theory and Modeling of Fluids, and Cryogenic Technologies.

The Process Separations Group researches industrially important separation unit operations, including distillation, supercritical fluid extraction, adsorption, and membrane separations through carefully designed laboratory measurements and correlation of measured and retrieved data. This work provides critically evaluated data and models needed to design more efficient and cost-effective separation processes. Current activities include developing solvatochromic screening procedures for alternative solvents; compiling databases for chromatographic analysis of natural gas mixtures, odorants, and alternative refrigerants; and improving methods for chromatographic analysis of the C6+ fraction of fuel gas condensates. The group also measures vapor-liquid equilibria of reactive mixtures and mixed-waste model systems and membrane diffusion by attenuated total reflectance spectroscopy. The panel looks forward to data measurement from the azeotropic distillation equipment, which has been under development for several years.

The Fluid Science Group uses acoustic resonators, capacitors, and other novel methodologies to measure thermodynamic and transport properties of fluids. These state-of-the-art extraordinarily high-precision techniques are also investigated as potential next-generation primary standards for temperature, pressure, and low flow rates. Current activities include development of acoustic transducers for use in primary thermometry up to 700 K; measurement of the speed of sound of semiconductor process gases to derive ideal-gas heat capacities, volumetric virial coefficients, and transport properties to support process modeling and accurate calibration of flow-metering devices; development of laboratory standards for accurate measurement of the viscosity and Prandtl number of industrially important gas mixtures; and development of an ultrastable cross capacitor for use as a primary pressure standard from 0.4 to 4 MPa.

The Experimental Kinetics and Thermodynamics Group uses a wide range of state-of-the-art measurement techniques to obtain kinetic and thermochemical data on industrially important chemical species. It also certifies SRMs for thermodynamic properties. Current activities include development of a broad database for advanced oxidation technologies used for waste treatment; measurement of the effects of industrial compounds in the environment; study of the thermodynamics of industrially important materials and processes; and development of new capabilities, such as use of ring-down spectroscopy, to characterize surfaces and thin films.

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

The group also has proposed a new initiative, the Next Generation Chemical Kinetics Database, to support detailed chemical modeling of gas-phase chemical processes. This proposal will supplement experimental data with extrapolation and prediction tools.

The Chemical Reference Data and Modeling Group compiles, evaluates, correlates, and disseminates SRDs. It also develops and disseminates electronic databases and software for thermodynamics, chemical kinetics, mass spectroscopy, and IR spectra. The group, in collaboration with EPA and NIH, supports the Mass Spectral (MS) Library and added the Automated MS Deconvolution and Identification System to allow more systematic evaluation of spectra. It has also continued development of the NIST Chemistry WebBook.

The NIST Chemistry WebBook is one of the premier projects in the CSTL and this division. It was developed as a tool to provide a flexible, easy-to-use interface for access to chemical data on the Internet and makes NIST reference data quickly available to the widest possible audience. An increasing user base has paralleled the WebBook's evolution through five editions, and the current version contains data on over 31,000 chemicals (up from 11,000 in the first edition). Data coverage has been greatly extended in 1998; new classes of information include heat capacity in the condensed phase, vapor pressure (both single boiling points and as a function of temperature), IR- and ultraviolet-visible spectra, and energy levels associated with small-molecule and radical electronic and vibrational spectra. Data on mass spectra and water solubility of organic compounds have also been added. In parallel, NIST-evaluated data collections have been added, such as proton affinity, equations-of-state on a number of industrial fluids, and data for diatomic molecules.

Improvements in user access have continued. Searching by substructure and complete structure have been added to searching by name (with a very extensive list of synonyms and common and trade names), formula, and Chemical Abstracts Registry Number. In addition, drop-down menus now define functional groups for which data are sought. The panel believes that one of the recently added sections in the NIST Chemistry WebBook labeled “water solubility” should be labeled “Henry's law constant.” The panel suggests that when resources permit, the WebBook should gain a new section labeled “water solubility” that contains composition data on coexisting saturated aqueous and organic liquid phases (liquid-liquid equilibrium).

The Computational Chemistry Group develops and applies computational chemistry methods for estimation and prediction of the chemical and physical properties of molecules. Last year's formation of this group has resulted in a substantial enhancement in NIST's ability to provide critical evaluation of existing literature data and construction of readily accessible databases. It has also developed chemical methodology for calculating transition states, including application of Density Functional Theory, and for total cross sections for electron impact ionization, which builds on existing expertise in the NIST Physics Laboratory. The group has had close interactions with the Experimental Kinetics and Thermodynamics and Chemical Reference Data and Modeling Groups, providing theoretical guidance for evaluation of thermochemical and kinetic properties.

The Experimental Properties of Fluids Group measures high-accuracy comprehensive thermophysical and transport property data on technically important pure fluids and mixtures, including hydrocarbons, organic and inorganic chemicals, refrigerants, and aqueous systems. In addition, the group develops unique, state-of-the-art apparatus to measure thermodynamic and transport properties of fluids and fluid mixtures over wide ranges of temperature, pressure, and composition. Current activities include development and construction of a low-vapor-pressure-

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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effusion apparatus and heat-of-vaporization calorimeter; construction and validation of an apparatus for the simultaneous measurement of vapor-liquid equilibrium and interfacial tension; and application of vibrating-wire, torsional-crystal, and capillary viscometers to precision measurements of fluid viscosities over broad ranges of temperature and pressure. The current generation of the vapor/liquid equilibrium-surface tension apparatus has been under development for several years. The panel looks forward to data measurement from this unique equipment.

The Theory and Modeling of Fluids Group performs theoretical and computational research on the thermophysical properties of fluids and fluid mixtures, including regions of fluid-fluid and fluid-solid phase separation. It develops high-accuracy models and correlations to describe and predict the thermophysical properties of fluids and fluid mixtures. It also provides comprehensive and evaluated SRD and electronic databases. The group has begun fundamental theoretical studies of the fluid-solid transition. Additional studies include structure evolution and rheology of gelling colloidal silica by neutron scattering and rheometry and computer simulation of shear-induced restructuring of colloidal silica gels. The staff are using an extended corresponding states model to develop standard thermodynamic surfaces for fluids. In October 1998, the group published a new tabulation of the thermodynamic properties of water from the International Association for the Properties of Water and Steam 1995 Formulation.

The Cryogenic Technologies Group develops improved measurement and modeling techniques for characterizing basic cryocooler components and processes and state-of-the-art cryocoolers for specific applications. The group also provides measurement methods, standards, and services for flow under cryogenic conditions and assists U.S. industry in the development of new and improved products utilizing cryogenic processes. Current activities include achievement of technology transfer status for the cryogenic catheter for treatment of heart arrhythmia and abnormal uterine bleeding and measurement and correlation of microscale heat transfer for cryogenic applications.

In collaboration with the Mathematical and Computational Sciences Division, group staff have developed a computer model of the behavior of regenerative heat exchangers, which has become the standard model in the field for predicting the behavior of cryocoolers. The group has measured the performance of several types of cryocoolers, including the new pulse tube refrigerator. The miniature pulse tube refrigeration unit was used on the April 1998 Space Shuttle mission, and NASA intends to continue use of such pulse tubes to cool IR sensors. NIST is currently working with NASA's Johnson Space Center on developing methods for liquefaction of atmospheric oxygen on Mars for use in rocket liftoff from Mars to return rock samples to Earth in the year 2007. Plans are now under development for NIST to assist the National Radio Astronomy Observatory in the development of pulse tube cryocoolers for detector cooling in the Millimeter Array telescope to be built in the Andes Mountains. Over the past 10 years, the pulse tube technology has been transferred to dozens of companies through publications and short courses, as well as contracts and CRADAs. A cryogenic grinding unit designed to increase friability and retention of volatile toxic compounds was completed in 1998.

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
Impact of Programs

All the groups in the Physical and Chemical Properties Division are making a strong, well-directed effort to convey their results to the scientific and engineering communities through a variety of mechanisms. During fiscal year 1998, the staff published 190 papers (31 percent of CSTL output), delivered 104 talks (17 percent), served on 122 committees (23 percent), and presented 59 seminars (36 percent). In the 240 days since it was released, the fourth edition of the WebBook was visited from over 129,000 distinct hosts, each of which may have served a number of users. On average, the WebBook has between 5,000 and 10,000 users per week, and 40 to 50 percent of these hits are from returning, i.e., serious, users. Many sites access the WebBook daily.

The division uses multiple approaches to identify industry needs and develop programs to assure that its work will have impact. Significant evidence of the value of divisional programs is also seen in industrial funding of projects, either through corporate grants or purchase of data products. Examples of close interaction with industry and/or responses to an industry problem include the proposed measurement of phase equilibria for ethylene glycol/water for aircraft and runway deicer recovery systems, the development of cryogenic catheters, and the measurement and modeling of flow boiling heat transfer rates in microgeometries for use in catheters to cool blood flow to the brain.

Division Resources

Funding sources for the Physical and Chemical Properties Division (in millions of dollars) are as follows:

 

Fiscal Year 1998

Fiscal Year 1999 (estimated)

NIST-STRS, excluding Competence

8.7

8.7

Competence

0.1

0.1

ATP

0.4

0.3

OA/NFG/CRADA

4.0

4.2

Other Reimbursable

0.1

0.2

Total

13.3

13.5

The panel is encouraged to see that the percentage of OA funding has decreased from 35 percent in fiscal year 1997 to 30 percent in fiscal year 1998, but the large amount of external support still causes problems throughout the division. OA money is becoming more difficult to acquire, and the funding agencies and companies are requiring unreasonable levels of cost-sharing. Although division management would prefer the level of external support to be closer to the CSTL average of 17 percent, competing for grants and other funds is a healthy process that ensures the division research teams remain at the forefront of their fields.

As of January 1999, staffing for the Physical and Chemical Properties Division included 65 full-time permanent positions, of which 54 were for technical professionals. There were also 24 nonpermanent and supplemental personnel, such as postdoctoral research associates and part

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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time workers. The division staff are split approximately equally between Gaithersburg and Boulder.

The skills of the personnel in the Physical and Chemical Properties Division are complementary, unique, and highly valued. NIST personnel form virtually the world's only remaining teams actively involved in making fundamental measurements of thermodynamic properties. The strong synergism between experiment and theory, made possible by the interactions within and among the various groups, improves the quality of the work. A specific example is the rapidity with which the Computational Chemistry Group has become tightly integrated with both the experimental and reference data groups at Gaithersburg. Similar strong connections had previously been established in Boulder and continue to work well.

In Gaithersburg, division staff are generally satisfied with the physical facilities, although in certain laboratories, the mechanisms to ensure air cleanliness, dust control, and air filtration are insufficient; the quality, capacity, and reliability of the power supply are problematic; and the exhaust and ventilation systems are inadequate. Future laser-based optical studies will require cleaner rooms and better vibration control. However, the current quality of the laboratories is comparable to that of facilities at research-oriented universities.

In Boulder, the division's laboratory space in Building 2 is generally adequate; the two most significant infrastructure problems have recently been addressed by installing a new HVAC system for this building and increasing power capacity and quality. However, Building 2 is currently overcrowded because laboratory space in Building 3 is inadequate. Problems associated with Building 3 include practically no temperature control; extremely poor air cleanliness, dust control, and air filtration; unreliable, low-quality, low-capacity power; poor lighting; and a leaky exterior shell. The situation is expected to improve when NOAA personnel vacate the site and space in Building 2 is made available for NIST researchers. However, the timing for this transition remains uncertain. Meanwhile, these facilities problems are having a strong negative effect on the division's work and ability to carry out its mission.

Analytical Chemistry Division
Division Mission

According to division documentation, the mission of the Analytical Chemistry Division is to serve as the nation's reference laboratory for chemical measurements and standards to enhance U.S. industry 's productivity and competitiveness; assure equity in trade; and provide quality assurance for chemical measurements used for assessing and improving public health, safety, and the environment.

The Analytical Chemistry Division is the fundamental chemical metrology component of CSTL and NIST, and the division mission is fully and effectively integrated into the overall mission and goals of both. Divisional programs provide measurement standards, accurate and reliable compositional data, and research in measurement science. CSTL has placed a priority on international comparability of measurements, and the staff of this division is taking a leadership role in this intercomparability effort. The division continues to be well managed and is clearly focused on fiscal responsibility.

The division programs demonstrate the fundamental role that maintaining U.S. standards and standard methodology play in the division's mission. There is, however, a delicate balance

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

between a commitment to develop and to supply new SRMs and the need to maintain and resupply existing SRMs. The panel remains concerned that the standards maintenance program appears to be overshadowing the research into measurement science and new standards development. The breadth of coverage of measurement standards must remain a priority to assure the competitiveness of U.S. industry.

All division research and service projects are reviewed on an annual basis to assess the quality of work and fit with the mission and industry needs. The division is using a formal system to assess relevancy and to prioritize programs and projects. The panel encourages continuous attention to the process to assure that the best projects are supported. The Analytical Chemistry Division needs to continue strategic evaluation to determine those technical competencies for which it should be best-in-class, state-of-the-art, or a nonparticipant. They cannot and should not attempt to be best-in-class in all areas. The driving force for developing or maintaining best-in-class capability should be based on critical needs of U.S. industry.

Project effectiveness may be better demonstrated by clear comparison of objectives and milestones to demonstrated results. Indicators of success may include new SRMs, NTRMs, publications, and leadership involvement in international comparability studies. Although industry roadmaps are not available for this laboratory, the division does conduct industry focus groups to provide similar inputs.

Technical Merit and Appropriateness of Work

Overall, the technical merit of the work in the Analytical Chemistry Division was exceptional, and the results produced in the division are of vital importance to U.S. industry. The entire staff is dedicated to a quality process that drives much of their activities. Programs of particular note include the expansion into microfluidic measurements, expansion of high-precision optical emission spectrometry (OES) methodology to support spectrometric NTRM programs, novel methods to isolate and identify proteins and biomarkers in biological matrices, continued development of techniques and methodologies focusing cold neutron beams for analytical applications, and the revitalization of the division's classical chemistry capability.

Research activities in the division focus on chemical measurements as made by high-performance analytical tools such as mass spectrometry, microsampling/detection technologies, state-of-the-art separations methods, classical analytical methods, gas metrology, nuclear analytical methods, organic analytical methods, and spectrochemical measurement methods. These programs are carried out within five groups: Spectrochemical Methods (newly renamed), Organic Analytical Methods, Gas Metrology and Classical Methods, Molecular Spectrometry and Microfluidic Methods, and Nuclear Methods. The division is nearing the end of a 3-year restructuring that includes establishing a strategic plan for division research and service activities, adjusting the funding profile, and improving the division's delivery of standards.

The Spectrochemical Methods Group focuses on the development, critical evaluation, and application of methods for the identification and measurement of inorganic chemical species using x-ray, optical, and mass spectrometry. This group continues to make considerable investments in capital equipment; this year's major purchase is a glow discharge optical emission spectrometer (GD-OES). One of last year's acquisitions, a wavelength-dispersive x-ray fluorescence (WD XRF) spectrometer, will be used to expand this group's presence in the standards program and was recently used to renew three new standards for the $4 billion cement

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

industry. This group continues to expand the application of high-precision inductively coupled plasma-optical emission spectrometry (ICP-OES) methodology. The performance of high-precision ICP-OES rivals classical methods and will continue to have a favorable impact on group effectiveness. The ICP-OES technology is well suited for transfer to the private sector and is being used in the development of an NTRM Program for spectrochemical solutions. The resulting outsourcing of the routine certification of spectrochemical solutions will enable the spectrochemical group to spend more time on the advancement of measurement science and the development of new standards.

The Organic Analytical Methods Group focuses its research and application efforts on the areas of clinical, nutritional, environmental, and forensic analysis, with priority given to national and international measurement comparability. There is a heavy emphasis on high-resolution mass spectrometric methods to unequivocally identify species isolated at low concentrations by various separation techniques. Because of the difficulty of working with small samples, the group has used supercritical fluid extraction to assure homogeneity in the extraction of organic contaminants in natural environmental matrices such as air and diesel particulate. Solid-phase microextraction has been developed to concentrate and purify trace amounts of methylmercury and alkyl tins in fish, mussel, and oyster tissue and blood. Methods to extract drugs quantitatively from within human hair samples have confirmed that residues from drug users are enriched in the nonnaturally occurring enantiomer of the drug, whereas residue on the surface of the hair from casual exposure to smoke contains both enantiomers. Hyphenated high-resolution mass spectroscopy has been used to detect and quantify proteins and biomarkers in biological matrices (troponin-I, a marker for myocardial infarction; glycohemoglobin, a marker for diabetes; serum thyroxine, a marker for thyroid function; and cortisol, a marker for endocrine function). Capillary electrochromatography methods have been developed to separate isomers of beta-carotene and other carotenoids of significance in food.

In fiscal year 1998, the Organic Analytical Methods Group recertified or redeveloped 11 environmental SRMs, 14 chemical/pesticide SRMs, 5 clinical SRMs, 4 food/nutritional SRMs, and 8 miscellaneous SRMs in addition to developing 7 new SRMs and renewing 3 SRMs in the above categories. Staff in this group published seven significant papers in their field this year, and collaborations are ongoing with the NOAA, EPA, National Cancer Institute, College of American Pathologists, National Institute of Justice (OLES), Defense Special Weapons Agency, Department of Defense, and a number of international metrological agencies.

The Gas Metrology and Classical Methods Group focuses on a variety of activities, including gas metrology, classical wet chemical methods (such as gravimetry and titrimetry), coulometry, ion chromatography, optical spectroscopy, and maintenance of the theoretical infrastructure for pH and conductivity measurements. One of the very significant accomplishments by this group in 1998 has been the successful conclusion of a long-standing debate over the pH scale. NIST staff provided leadership on the adoption of a singular approach to measuring pH. Research has continued on development of an open-path, Fourier transform IR (FTIR) database for quantitative measurements of EPA-designated hazardous air pollutants. A CD-ROM containing 21 compounds, including 525 spectra, has been developed. This group is actively involved in international comparisons with European collaborators on measurement standards in such areas as primary gases for the automotive industry and conductivity for water quality. This program is designed to allow bilateral use of local standards in making regulatory and trade agreements with the United States. The group is actively involved in the NTRM

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

Program and continues to successfully manage certification programs for specialty gas vendors that provide NIST traceable gas standards for end users.

The Molecular Spectroscopy and Microfluidic Methods Group (formerly Chemical Sensing and Automation Technology Group) conducts research on the metrology of molecular spectrometry, develops standards for calibration, validates performance of instruments for measuring molecular spectra, and conducts research on microfluidic devices. In collaboration with the Process Measurements Division, this group has begun a project on microfabricated analytical devices that will receive NIST competence funding for 5 years beginning in 1999. This area is critical to U.S. industry for a wide range of applications in the environmental, pharmaceutical, forensic, and health care areas and has a potentially broad impact for the reduction of solvent usage (which would lower environmental contamination), the development of remote and portable measurement devices, and development of integrated sampling/measurement devices for faster analysis.

In addition, the group has responsibility for development and certification of optical transmittance and wavelength standards. It continues to provide optical filters to calibrate the transmittance and wavelength scales of visible and ultraviolet spectrophotometers. In 1998, staff certified 124 solid absorbance filter SRMs and recertified 203 optical filter sets. The NTRM Program for optical reference material filters was expanded, and two additional workshops were conducted. A new dispersive Raman instrument was installed, and a calibration source was put together for a new project to develop Raman intensity standards.

The Nuclear Methods Group continues research on the use of neutron beams as analytical probes with both prompt gamma activation analysis and neutron depth profiling. Long-term research includes development and application of cutting-edge neutron focusing technology to provide three-dimensional compositional mapping of thin film semiconductor materials. This technique has been used for nondestructive chemical characterization of metals. In addition, because of its multielement nature, it is used for analysis of chemical contaminants in the NIST specimen backing program and for compositional mapping of advanced materials, e.g., semiconductors. The development work on neutron activation mass spectrometry and measurement support for superconductivity were terminated in 1998.

Impact of Programs

NIST provides nearly 1,300 different types of SRMs and in fiscal year 1998 sold 37,000 SRM units to approximately 6,650 separate customers. Roughly 21,000 of these units were from the 850 different types of materials certified for chemical composition by the Analytical Chemistry Division. In addition, the division certified 73 batches of NTRMs. The combined number of types of SRMs and NTRMs available from the division has increased from 193 to 216; the number of NTRMs alone rose by about 20 percent this year. Currently, each technical group within the division manages its respective SRM and NTRM standards programs, although the division is not able to fully recover the cost of administering the NTRM Program. Recertifications of optical filters and cylinder gas standards remained constant at 325 in 1998.

The panel continues to be concerned about the proportion of resources dedicated to the division's SRM and NTRM activities. Currently almost $8 million (an increase of $1.2 million from 1997) of the Analytical Chemistry Division's budget is devoted to maintenance and

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

development of standards, whereas the budget for new standards development increased by only about $200,000 over the same period.

The division entered into five CRADA agreements in 1998, up one from 1997. Although such formal agreements are useful, the panel supports the division's approach of also promoting informal partnerships with industry. The division's publication record is excellent and continues to make strong contributions to the peer-reviewed literature. The project on international comparability of chemical measurements provides worldwide leadership in the development of SRMs, NTRMs, proficiency testing programs, and international intercomparisons. The panel is particularly pleased by this division's international work, as intercomparisons become more vital as trade becomes more global.

The division is supporting the NIST-wide initiative to play a leadership role in intercomparability programs among national and regional standards laboratories to facilitate international trade. These activities remain the basis for formal establishment of equivalence among primary methods and standards important for global commerce. The panel applauds the group's leadership in this area. However, although the division is well situated in the international reference material community, it is lacking a coordinated effort that could have an impact on international measurement science, particularly with respect to world trade.

Division Resources

Funding sources for the Analytical Chemistry Division (in millions of dollars) are as follows:

 

Fiscal Year 1998

Fiscal Year 1999 (estimated)

NIST-STRS, excluding Competence

8.1

8.0

Competence

0.0

0.3

ATP

0.0

0.1

Measurement Services (SRM Production)

2.2

1.9

OA/NFG/CRADA

2.2

3.2

Other Reimbursable

1.4

1.4

Total

13.9

14.9

External funding now appears to be sufficiently low to allow independence in the division's implementation of strategic measurement science research programs. The panel encourages the division to maintain this independence and supports management's continuing efforts to reengineer delivery of SRM services.

The panel welcomes the division's efforts to reduce SRM backlog, increase the ratio of new to renewal SRMs, and develop a new quality classification document for its SRM value assignment process. The panel also applauds the division's conducting bi- and multilateral comparisons of chemical measurement standards and methods with other national metrology institutes. The panel considers the NTRM Program to be excellent work and applauds its continued expansion beyond the area of gas standards. The panel recognizes that each NTRM

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×

Program is unique but believes that the administrative burden that NTRMs place on the scientists would be eased by placing the standard processes within a dedicated organization. Another concern of the panel is the apparent proprietary nature of company-specific NTRMs. Either the cost of development and certification for these NTRMs needs to be more fully recovered or the licensed company should provide these standards to the industry for a reasonable price.

As of January 1999, staffing for the Analytical Chemistry Division included 66 full-time permanent positions, of which 61 were for technical professionals. There were also 31 nonpermanent and supplemental personnel, such as postdoctoral research associates and part-time workers.

The division hired four new personnel in 1998, but because of attrition, the programs are still understaffed. Several experienced personnel retired in 1998, and more are anticipated to retire shortly. Postdoctoral research associates are used efficiently to conduct research and as a source for permanent hires. The panel is also pleased that critical vacancies have been filled in the area of classical analytical chemistry and that necessary personnel have been added to the Gas Metrology and Classical Methods Group to support the SRM Program.

The division is moving into new facilities in the Advanced Chemical Sciences Laboratory (ACSL) in 1999. The panel is pleased to note that plans are in place that will hopefully produce a smooth transition to the new space with as little disruption to current activities as possible. On a longer time scale, division management needs to continue to maintain and revise its 5-year capital plan to adequately address future needs and analytical capabilities.

MAJOR OBSERVATIONS

The panel presents the following major observations.

  • The technical merit of the work in the focus areas of the Chemical Science and Technology Laboratory (CSTL) continues to be of a very high level and quality. Benchmarking activities determined that several of the technical efforts in the areas of chemical and physical measurements, such as the CSTL standards in temperature, moles, pressure, humidity, and flow rate, are the Best in the World or at least at the state-of-the-art level.

  • The technical results produced and the services performed at the CSTL continue to be of vital importance for the advancement of U.S. industry.

  • The process for project/program assessment put in place by CSTL is well documented and provides a good example for other NIST laboratories. The true value of this tool is the way managers use it to focus discussions and decisions on project initiation and conclusion.

  • The operational lifetime of scientific hardware is limited. A long-term capital equipment plan should be developed and reexamined regularly.

  • The facility's inadequacy for performing state-of-the-art measurement work remains an issue. Funding appears to be in place for the Advanced Measurement Laboratory, but the anticipated occupancy is at least 5 years away. Therefore it is important to develop a plan for upgrading the present facilities and to determine an implementation schedule for that plan.

  • The Web-based data dissemination is of vital importance and must be carefully reviewed for uniformity among divisions regarding standardization of data presentation, ease of use, and maintenance of user privacy.

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
  • The laboratory overall continues to address topics raised by the panel in a timely and receptive manner; the panel was especially pleased to note that the update to the gas-phase kinetic database has finally been released by the Physical and Chemical Properties Division. In the spirit of continuous improvement, the panel encourages the laboratory to continue to carefully consider the recommendations documented in the detailed divisional reports. In particular, the panel remains concerned about the costs associated with the NTRM Program and the commercial distribution of the reference materials. This activity is an excellent approach to efficiently providing industry with reliable reference materials, but the panel would like to see a proactive management plan to appropriately allocate the costs and responsibilities within NIST and at commercial companies.

Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Page 77
Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Page 78
Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Page 79
Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Page 80
Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Page 81
Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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Page 82
Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
Page 83
Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
Page 84
Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
Page 85
Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
Page 86
Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
×
Page 87
Suggested Citation:"Chapter 4 Chemical Science and Technology Laboratory." National Research Council. 1999. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories: Fiscal Year 1999. Washington, DC: The National Academies Press. doi: 10.17226/9685.
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