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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Chapter 4

Chemical Science and Technology Laboratory

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

PANEL MEMBERS

Lou Ann Heimbrook, Lucent Technologies, Chair

Arlene A. Garrison, University of Tennessee, Vice Chair

John L. Anderson, Carnegie Mellon University

Anthony M. Dean, Exxon Research & Engineering Company

Pablo G. Debenedetti, Princeton University

Robert R. Dorsch, DuPont Central Research & Development

Daniel L. Flamm, University of California, Berkeley

Steve M. George, University of Colorado, Boulder

Wayne O. Johnson, Rohm and Haas Company

Helen H. Lee, University of Cambridge

Douglas E. Leng, LENG Associates

Roy Lyon, National Food Processors Association

James W. Serum, Hewlett-Packard Company

Jay M. Short, Diversa, Inc.

Christine S. Sloane, General Motors Corp. R&D Operations

Anne L. Testoni, DEC-Digital Semiconductor

Submitted for the panel by its Chair, Lou Ann Heimbrook, and its Vice Chair, Arlene A. Garrison, this assessment of the fiscal year 1998 activities of the Chemical Science and Technology Laboratory is based on a site visit by the panel on March 12–13, 1998, and documents provided by the laboratory.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

LABORATORY-LEVEL REVIEW

Laboratory Mission

According to NIST 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 U.S. economic growth and the global competitiveness of U.S. industry. Positioning the laboratory as the nation's premier scientific institute for advancing technologies and providing measurement capabilities in chemistry, chemical engineering, and biotechnology are appropriate objectives. In fiscal year 1997, the laboratory's programs led NIST 's efforts in measurement services by producing 73 percent of the NIST Standard Reference Materials (SRMs), providing 69 percent of NIST Standard Reference Data (SRD), performing 12 percent of NIST calibrations, and submitting 25 percent of NIST patent requests. 1

During site visits at NIST, the panel observed that the CSTL staff is dedicated to providing measurement standards that strengthen the vertical traceability structure in the United States and to leading the efforts of global standards organizations for chemical and physical measurements. In 1997, NIST's adequacy to support the U.S. technology infrastructure was benchmarked against other national measurement laboratories in Japan, Germany, and Brazil. The comparison focused on activities related to measurements, standards, and data and looked at the relative levels of effort, total space, specialized facilities, and demand for services. This international benchmarking is to be expanded to include comparisons with six more countries. The initial work shows that NIST covers a broader metrology scope than any other single institution in the three countries already studied2 The CSTL provides fundamental work that allows NIST to assume this leadership position in the area of chemical and physical measurements. In addition, the CSTL maintains numerous programs that, in the panel 's opinion, anticipate and address the next generation of measurement needs of the nation in order to maintain an economic growth position for U.S. industry through technical efforts of the laboratory. Examples of such programs are documented in the divisional assessments.

Technical Merit and Appropriateness of Work

The CSTL's technical efforts in chemical and physical measurement are conducted across strategic scientific areas relevant to the mission of NIST: biotechnology, process measurements, surface and microanalysis science, physical and chemical properties, and analytical chemistry. The panel found that the technical work of all the divisions was of the highest scientific quality and showed consistent programmatic excellence. Over the past year, extensive internal and external prizes recognizing scientific achievement were awarded to laboratory personnel and document

1  

The numbers that correspond to these percentages are 28,644 SRM units sold, 652 SRD units sold, 1,354 calibrations performed, and 13 patents submitted.

2  

The findings of NIST's international benchmarking study were discussed in the presentation made by the laboratory director to the panel on March 12, 1998.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

NIST's continuing ability to perform world-class research. The panel also applauds the laboratory for carrying out state-of-the-art scientific work that is intermediate in scope between longer-range university research and the more immediate goals of industry. Building strong relations with academic institutions can only enhance the strength of NIST programs that occupy this unique niche in the nation's research and development efforts.

The technical merit of each division in the CSTL is well documented in the individual reports. These reports clearly show that the laboratory as a whole has made dramatic progress in the development of the planning process for new and existing scientific programs. Most importantly, the laboratory has begun work on putting in place measurable goals and objectives for the quality and appropriateness of NIST work. When the effectiveness of programs is being determined, it is critical to realize that numbers are only one measure of success. Assessing work on standards will use different metrics than those that are appropriate for evaluating technical projects. Also, suitable external feedback mechanisms will vary depending on the maturity of the technology. An important factor in achieving success is continued reevaluation of programs throughout their existence. The panel observed that there is the opportunity to solicit input from experts at all stages of program review. Such interactions could help assure that the full breadth of applications is realized.

The laboratory continues to work hard to ensure that the core measurement science is balanced by work on new technical opportunities. In the former area, the update of the NIST/Environmental Protection Agency (EPA)/National Institutes of Health (NIH) Mass Spectral Library was released this year. This database contains evaluated spectra and is provided through multiple vendors. The panel continued to be impressed by this work as it is enabling technology for scientific analysis of materials and compounds and the impact will be felt across multiple fields. In the area of technological development, the panel particularly noted the value of interdivisional and interlaboratory collaborations. The benefits of utilizing the variety of unique expertise available at NIST can be seen in the work on standards for Raman spectroscopy and in the project on microcalorimeter x-ray detectors.

The technical programs in the laboratory and the interactions among the various divisions have exceeded the panel's expectations. The breadth of programs covered by the laboratory is reflected by citing just a few of the projects highlighted in the divisional reports. Reference materials have been developed in several diverse areas. For example, in DNA research, there are now SRMs for evaluation of p53 and short tandem repeats (STRs). For the semiconductor industry, there is a new SRM for arsenic implantation in silicon to complement the existing SRM for boron in silicon. And in the health sciences, NIST has provided standards to help determine accurate levels of cholesterol and 12 other biomarkers in blood samples. In addition, the laboratory continues to meet the high demand for calibration services in pressure, humidity, vacuum, temperature, and flow. Finally, it is worth noting the continued expansion of work in computational chemistry to exploit advances in theoretical modeling.

Impact of Programs

The CSTL has disseminated scientific results to a wide audience in industry, government, and academia. In fiscal year 1997, the laboratory employed all conventional dissemination techniques. Personnel authored 327 publications in leading scientific journals, staff organized 31

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

conferences and workshops, 24 CRADAs with industry were in place, and 6 licenses were granted on patents from laboratory work. In the tradition of being the nation's leader in measurement technology, the laboratory activities have resulted in the sale of 28,644 SRMs and 652 SRDs, as well as performance of 1,354 calibrations. An additional 2,354 SRDs have been sold by distribution.

In addition to these formal demonstrations of dissemination and impact, staff also communicated the value of laboratory activities through attendance at conferences and workshops, through interactions with guest researchers, and through posting information on the World Wide Web. In general, the laboratory has increased use of the Internet to disseminate information, and concerns expressed in last year' s assessment regarding proper labeling of materials on the Web databases have been addressed. The divisional reports contain specific comments on how technical results could be disseminated more widely using techniques such as establishing more industrial liaisons. Examples of successful information dissemination include such efforts as the Chemistry WebBook and the Mass Spectral Library, which is now installed in over 60 percent of the mass spectrometers manufactured in the United States.

The CSTL programs affect a wide range of industries including health and safety, environmental, electronics, automotive, and aerospace. Numerous industrial operations are increasing demand for traceability to NIST and for international comparability. The NIST Traceable Reference Materials (NTRM) Program is a key example of the ongoing effort of the CSTL to provide traceable resources to a broad spectrum of industries, as well as to provide economic growth opportunities for those companies producing the NTRM standards. 3 The success of the new NTRM Program will be based on continued proactive management to ensure that the administration of this important program does not interfere with technical activities.

There is worldwide demand from a diverse array of companies for reference materials and physical and chemical measurement databases. The evolution of industries and their products makes it vital that efforts continue on the development of new and advanced reference materials and on ways to ensure worldwide compliance with traceability on product and service quality and safety. The panel notes two CSTL projects that demonstrate how this laboratory contributed to such efforts.

The division's refrigerants research clearly reduced uncertainty about refrigerant properties and fostered the development of new products that are more environmentally safe, energy efficient, and cost-effective. An economic impact study on this project surveyed industrial representatives and calculated that, when industry's gains were compared with NIST 's investment, this program had a benefit-to-cost ratio of 4:1. The second example is in the aerospace industry. A high-temperature alloy is one of the most critical components of jet engine turbine blades, and analysis showed that the adherence of the protective oxide coating on the turbine is enhanced by reducing the sulfur content below 0.5 ppm. The SRM developed in the CSTL has currently become the de facto standard for the measurement of sulfur levels of 1 ppm and below in nickel-based alloys. This work has had an impact on the quality and safety of the aerospace industry and all citizens who rely on the service and quality of aerospace products.

3  

In the NTRM program, the goal is to reduce the burden on NIST of continually producing large quantities of the same SRMs. Instead, for well-established SRMs, NIST establishes a program with appropriate quality assurance that allows a group of commercial reference materials producers to produce and sell NIST Traceable Reference Materials that are based on the corresponding NIST SRMs.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

In addition to the laboratory's work on materials and databases, the fundamental research has also had an impact on industry; examples are cited in the divisional reviews. In many cases, this fundamental work augments specific technical needs in industry for current and long-term measurement capabilities. Recently, the laboratory completed realization of the full extent of the International Temperature Scale of 1990 (ITS-90). The final range completed was from 0.65 to 25 K; this range of temperatures is important for applications in the aerospace and cryogenic fuel industries. The efforts to provide calibration of precision resistance thermometers have been critical in the realization of the accuracy needed for international comparisons in this range.

This past year the laboratory has continued work on programs critical to industry, has effectively planned for future initiatives, and has improved methods for dissemination of information. The numbers of reference materials and databases sold, of hits on laboratory Web sites, and of calibrations performed clearly reflect the ever-increasing demand for the services this laboratory provides to industry. In addition, economic impact studies completed for some projects in the laboratory demonstrate the effectiveness of the work done in this laboratory in influencing the economic growth of the United States. Such studies are vital, and it would be appropriate for the laboratory to perform these analyses on sample projects from all of the divisions.

Laboratory Resources

Funding sources4 for the Chemical Science and Technology Laboratory (in millions of dollars) are presented below:

 

Fiscal Year 1997

Fiscal Year 1998 (estimated)

NIST-STRS, excluding Competence

37.0

37.1

Competence

1.9

2.0

ATP

2.0

3.0

Measurement Services (SRM production)

2.3

2.3

OA/NFG/CRADA

10.0

10.6

Other Reimbursable

2.8

3.0

Total

56.0

58.0

4  

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 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:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

Staffing for the Chemical Science and Technology Laboratory currently includes 280 full-time permanent positions, of which 242 are for technical professionals. There are also 106 nonpermanent and supplemental personnel, such as postdoctoral fellows and part-time workers.

Clearly, the CSTL is able to perform world-class measurements as a result of the caliber of facilities, equipment, and human resources available at NIST. However, there are still some issues related to these resources of concern to the panel.

Relatively flat budgets coupled with staff retirements have led to difficulties in several areas where the number of projects per staff member is high and many key projects are dependent on nonpermanent personnel. The SRM and calibration programs are growing and take priority, so often permanent staff do not have enough time to continue work on these central laboratory activities as well as to begin new research projects. Therefore, the development of new research is often overly dependent on postdoctoral students and visiting staff, and thus leadership of these growth areas can be divorced from the permanent laboratory organization.

In general, the existing laboratory capabilities have improved over the past year. However, the facilities are still not adequate to allow all of the divisions to perform the current and next-generation measurements needed by U.S. industry. The panel is pleased to see that the new wing at the Center for Advanced Research in Biotechnology (CARB) has been completed and occupied. This addition provides space for the Structural Biology Group and for the new high-field 600 MHz nuclear magnetic resonance (NMR) instrument. The Advanced Chemical Sciences Laboratory (ACSL) should be finished during the first quarter of 1999. This building contains 80,000 sq ft of laboratory and office space, including much-needed clean-room facilities, for several divisions. In Boulder, the NOAA is building a new facility, and the space vacated by NOAA staff currently working in NIST's Building 2 will provide room for the Physical and Chemical Properties Division staff to expand and upgrade their laboratories. The panel was pleased to learn that initial funding for the Advanced Measurement Laboratory (AML) had been allocated by Congress and that further funding for fiscal year 1999 is being pursued so that construction might begin in December of 1998. Construction of this new laboratory is imperative to obtain the quality of facilities necessary for measurements undertaken in the Surface and Microanalysis Science Division and for provision of primary standards and calibration services for pressure measurements in the Process Measurements Division. However, completion of the AML could take 3 or more years, so it is Critical for the CSTL to develop a facility plan to deal with the interim period, as well as to work out contingency plans in case the AML's funding does not come through.

Capital equipment is discussed in detail in the divisional reviews. Overall, the panel felt that funding in this area was adequate and appropriately utilized to exert the maximum impact on U.S. industry.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

DIVISIONAL REVIEWS

Biotechnology Division
Division Mission

According to NIST documentation, the mission of the Biotechnology Division is to provide the measurement infrastructure necessary to advance the commercialization of biotechnology. This is achieved by developing a scientific and engineering technical base along with reliable measurement techniques and data which will enable U.S. industry to produce biochemical products quickly and economically with appropriate quality control.

The conformance of the division programs is, in general, good, ranging from excellent to needing improvement. This is to be expected for a new division focused on a broad and rapidly changing field such as biotechnology. One concern of the panel related to the work being done at CARB. The center, a collaboration between NIST and the University of Maryland, has produced strong technical work, and CARB is a key asset for NIST's biotechnology programs. However, the collaboration does generate a managerial challenge. One of the strengths of CARB is its technical ability to solve protein structures. Although such an activity may not be inappropriate for NIST scientists, it is not clear how such work fits into the NIST mission, which is to advance measurement sciences. A general plan that furthers the mission of NIST needs to be conveyed to the NIST staff who are a part of CARB so as to ensure that the NIST mission is not defocused. However, the benefits of the NIST/CARB collaboration, such as increased strength in recruiting and efficient resource sharing, outweigh the costs of the extra managerial efforts, and the formation of other similar collaborations is encouraged.

Technical Merit and Appropriateness of Work

Overall the division performs appropriate, high-quality research into the development and application of new measurement technologies in the area of biotechnology. One of the strengths of the division is the program in biocatalysis and bioprocessing engineering. The field has significant economic potential for U.S. businesses, and NIST is a recognized technical leader in this area. The panel was impressed by the balance between the need for state-of-the-art technological work and the development of new standards and measures in this area. The NIST efforts are likely to encourage further research and development in a field that currently is only weakly supported by industry. Another group with potential impact is the Structural Biology Group, located at CARB. The group's emphasis on theoretical and experimental approaches to macromolecular structure determination and function will advance analytical and biophysical measurement science, as well as protein engineering and design.

In general, a key element in the success and improvement of the programs is continued vigilance in the definition of critical paths in each of the targeted research areas. For example, the DNA Technology Group has done an excellent job developing the p53 and STR reference materials. Investing further resources in this program might allow fluorescence intensity standards to be expanded to provide other needed diagnostic reference materials; possible candidates range from infectious agents to transgenic plants. Another important aspect of

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

successful projects is focusing on high-priority industrial needs. Leveraging NIST efforts with industrial support can then maximize the value of NIST resources. A particular example can be seen in the beneficial studies and database development in the area of biothermodynamics. The success of this project depends on utilizing input from external experts both to define initially appropriate areas of activity and to review progress of specific projects.

Overall, the division management is to be commended on the substantial progress made in developing broad and appropriate programs in a complex and rapidly changing field. There is some variability between programs that may be related to the selection process. The division outlined an extensive process that is used to define the areas in which the division is active, but the priority-setting process did not appear to the panel to be as clearly defined. In spite of this minor issue, the group activities were well integrated, and the joint efforts between CARB and NIST add substantial strength and increase the overall value of the division. With continued resource planning and appropriate priority setting, the full economic impact of the division's projects will be realized.

Impact of Programs

The panel was impressed by the effectiveness with which the division disseminates its scientific accomplishments. In 1997, its 99 publications covered diverse topics, ranging from applications of membrane channels to mechanisms on DNA topoisomerases. In addition, the group has been active at numerous professional conferences and sponsored workshops, including Self-Assembling Thin Film Materials and Standards for Nucleic Acid Diagnostic Applications. They have also established and maintained a number of Internet databases such as the STR DNA database and the Biological Macromolecule Crystallization Database (BMCD). In addition they have cross-referenced the BMCD with the Nucleic Acid Database. The efforts in this area are outstanding, and the division should continue its dissemination activities at the current level.

It is premature to expect a significant impact on industry resulting from the activities of the Biotechnology Division at this time. However, programs do exist for which such an impact may be expected in the future. One example is the newly created Bioinformatics Group, which has the potential to generate significant economic impact through applications in sequence, functional, and structural data analysis. In fact, the level of need and the size of the effort are so great that it will be essential for the division to narrow its focus to areas of the greatest influence. Biotechnology is expanding its influence into practically every sector of industry; therefore it is essential to invest increasing resources in biotechnology programs.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×
Division Resources

Funding sources for the Biotechnology Division (in millions of dollars) are presented below:

 

Fiscal Year 1997

Fiscal Year 1998 (estimated)

NIST-STRS, excluding Competence

6.9

6.5

Competence

0.5

0.9

ATP

1.3

1.9

Measurement Services (SRM production)

0.1

0.0

OA/NFG/CRADA

0.8

0.9

Other Reimbursable

0.1

0.1

Total

9.6

10.3

Staffing for the Biotechnology Division currently includes 35 full-time permanent positions, of which 32 are for technical professionals. There are also 31 nonpermanent and supplemental personnel, such as postdoctoral fellows and part-time workers.

In addition to the permanent staff, each group within the division has attracted experienced guest researchers. A concern is that there is some difficulty in maintaining qualified individuals in the bioinformatics area because of the competition with industry for talented individuals in this field.

The construction of the ACSL will amply address several critical facility needs of the Biotechnology Division, such as clean rooms for several groups. The 80,000 sq ft ACSL facility will be available by the first quarter of 1999. The recently completed CARB 1-B expansion also has provided modern facilities and has produced much needed additional laboratory space, which now includes a new high-field 600 MHz nuclear magnetic resonance instrument.

Process Measurements Division
Division Mission

According to NIST documentation, the Process Measurements Division develops and provides measurement standards and services, measurement techniques, recommended practices, sensing devices, instrumentation, and mathematical models required for analysis, control, and optimization of industrial processes. The division's research seeks fundamental understanding of, and generates critical data pertinent to, chemical process technology. These efforts include the development and validation of data-predictive computational tools and correlations, computer simulations of processing operations, and provision of requisite chemical, physical, and engineering data.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

The division's goals and projects were found to be generally consistent with this mission statement. In line with the mission statements of NIST and CSTL, programs in this division make highly appropriate contributions to the promotion of U.S. economic growth through work with industry. This close coupling helps direct programs to areas of highest priority to the affected industries. For example, over the last 20 years, many U.S. companies have become global corporations, and simultaneously foreign corporations have rapidly increased their presence and investment in U.S. markets. Therefore international cooperation in standards activities is essential to U.S. competitiveness. The Process Measurements Division's continuing and expanding work on interactive comparisons with measurements and standards made by sister organizations in other countries is highly appropriate and commendable.

Technical Merit and Appropriateness of Work

The technical merit of the programs is demonstrated in many ways. For example, in this fiscal year, personnel from the division have received more than nine awards and citations for their work, including a Department of Commerce Silver Medal, a Department of Commerce Bronze Medal, and the Allen V. Astin Measurement Science Award. In addition, continuing and widespread demand for calibration services in pressure, humidity, vacuum, temperature, and flow speaks highly for the quality of the division's work.

The panel was impressed to note that a number of their past suggestions have been adopted and implemented in laboratory programs. For example, the physical property databases now include extensive citations describing the data sources, type (experimental or calculated), and reliability. Also, division scientists have expanded the use of computational fluid dynamics (CFD) to complement experimental data, thereby reducing the amount of data required to quantify models. Finally, NIST's traceability programs are essential, and the panel was pleased to see this work continuing. Comments on the technical merit of each group's programs are below.

Information about the division's research is disseminated through meetings, publications, information posted on the Internet, symposia, guest researchers, personal contacts, and workshops. It is important not only for the division to publicize the results of its work but also to educate the relevant communities about the availability of this information.

One area of dissemination that the panel focused on was the laboratory 's use of the Web to publish updated and evaluated data for the technical community. The level of this effort could be raised, and the value of this data might be increased by supplementing the Web releases with production of permanent archival media such as CD-ROM. Leverage could be gained for this activity by publishing the archival data in the form of HTML files, which are accessed by a standard browser. Another way to expand the impact of this division's work would be to include evaluation and/or property estimation codes in both Web-based and CD-ROM formats via coding in a machine-independent form such as JAVA.

Within the Fluid Flow Group, the work on modeling gas-metal atomization flows to improve particle size distribution of finely divided metal products has progressed nicely over the past year. CFD simulations are in close agreement with experimental observations, and the simulations demonstrate that cooler gas flows produce increased momentum that results in better particle-size distributions. However, current industry systems are based on the opposite belief: the assumption that adding enthalpy to the gas flow improves powder yield. NIST is now

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

transferring this technology and these results to its industrial partners and could consider which other industries might benefit from this knowledge.

A multiyear program has been initiated to improve primary gas flow standards. The value and importance of such work were discussed in last year's assessment. Better standards in this area will raise the capability of NIST to a level that commands the highest international respect. Another valuable new program is the validation of ultrasonic flow measurement, which could become the technique of choice for future flow measurement. A deeper understanding of its technical nuances and development of a standard ultrasonic calibration methodology are crucial.

In the High Temperature Processes Group, the panel was particularly impressed by the cooperative work with the Analytical Chemistry and Surface and Microanalysis Science divisions on a new project addressing key needs for Raman spectroscopy standards. If a low-cost automated Raman instrument becomes available, it has the potential to be used as a process tool. This effort, initiated in response to industrial and institutional demand, includes the development of measurement standards for intensity and frequency as well as provision, over the long run, of key reference data. These standards are critical to assuring the accuracy and utility of data collections. The cooperative nature of this project is an excellent example of interdivision collaboration.

The High Temperature Processes Group also manages a specialized spray combustion research program. The facility for this work has recently been modified to enable total material balances and gas analyses to be done. In line with the mission, staff members are preparing for an industry-wide workshop to identify emerging needs in this field. Another project has targeted heat transfer data for supercritical fluids, with emphasis on carbon dioxide. A new facility is nearing completion where flows can be measured by laser Doppler anemometry and other advanced instrumentation. Since critical point densities are very sensitive to changes in temperature, heat transfer is subject to high local convective flows. Hence it is important to consider the orientation of the equipment because thermal convection will have a large influence on the flows. CFD modeling should enable heat transfer calculations to be made from the flow and temperature fields.

The Reacting Flows Group continues to disseminate results effectively over the Internet. CKMech, the chemical kinetic mechanisms database, now includes data sources and clearly indicates the most reliable data value if the information is available. Also, publications of NIST researchers are being made available on the Web. The group has completed a CFD model for gas behavior in a rotating disk chemical vapor deposition (CVD) reactor and is now awaiting experimental data. These data, such as information on the chemical profile in the gas phase above the disk, will be used to validate and provide parameter information for the models. The new experimental reactor is located in a new laboratory and is nearing completion. The laser-based analytical methods require clean air, which staff hopes to arrange by curtaining off portions of the room. Other work in this group addresses the development of new technology for low-temperature CVD. The technology is based on the reaction of sodium vapor with metal halides to produce very high purity coatings of metals. Particle growth takes place on solid substrates. Current experiments have verified the theoretical predictions for the coating of titanium on metals. Conditions have been identified where salt deposition can be avoided. With additional development, the technique could be applicable to the preparation of metal films on polymeric substrates. There remains much to be proven in this project.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

The Process Sensing Group has made good progress in the microhotplate gas sensor project. Since the researchers have improved the consistency and successfully demonstrated continuous operation, they are now focusing on industrial applications. A partnership has been established to identify and develop applications. Challenges that remain include difficulties with the quantitative analysis of gas mixtures and uncertainty about the long-term stability of the probes. Complete desorption of certain gaseous species could limit some applications. This work is supported by a Defense Special Weapons Agency contract, which demonstrates that the sensing of chemical warfare agents is perceived to be a vital national need. The self-assembled monolayer sensor research team is developing a good understanding of DNA hybridization reactions with surface substituents. Technologies that provide spatial resolution in the needed dimensions have provided key insights to this growing field of process sensors.

The Thermometry Group completed the realization of the ITS-90. The standard definitions in this scale range between 0.65 and 1234 K, and NIST is the first laboratory in the world to have realized the full extent of ITS-90, an amazing feat. The panel was pleased to note that the spherical resonator previously used for the determination of the Boltzmann constant is now being applied to determine thermodynamic temperatures. Another key accomplishment in this group is a new low-frost-point generator (LFPG), which was developed at NIST and extended the state of the art by three orders of magnitude. This LFPG can provide stable humidity levels down to 5 nm/mol, equivalent to a frost point of –100º C. This technology is needed in the field of semiconductors. As part of the extensive testing planned for the year, stable long-term operation of the generator may allow an extension of the lower limit of the device by an additional order of magnitude.

The Pressure and Vacuum Group has demonstrated excellent synergy in the merger of the former vacuum and pressure groups. One example of their development of natural areas of cooperation is the view that leaks are low flow rates and should be studied as such. This research group has actively sought outside funding and has been successful in obtaining support for studies that are well aligned with the division mission. The evaluation of microelectronic mechanical pressure sensors will provide valuable information about their failure mechanisms and should help quantify the characteristics of these inexpensive (approximately $15) sensors to facilitate appropriate use. In another project, the group is addressing the possibility of developing a new generation of spinning rotor gages in order to extend the current pressure range by about two decades. Such gages could potentially serve as primary measurement devices. Because the capabilities of current gages are limited by a lack of understanding of the physics that describes these devices, current research in related fields at NIST should prove beneficial to this project.

In an aggressive cycle of program planning, the Process Measurements Division continuously reallocates resources with careful attention to the mission. All projects are reviewed annually. This process encourages creation of critical new technologies while trimming programs that no longer appear to be useful. At the same time, care is taken to preserve the infrastructure essential for supporting work in calibrations and standards. Two examples of the turnover in projects in this fiscal year are the termination of research on supercritical oxidation of wastes and the adoption of new interdivision work on Raman standards.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×
Impact of Programs

Various groups in the Process Measurements Division participate in intercomparability activities and collaborations with national and regional standards laboratories. These activities are essential for global commerce between companies based around the world. One focus area this year was the development of partnerships with South American countries for pressure and vacuum measurements.

The panel found abundant evidence that divisional programs have a broad and valuable impact on industry. The many publications, workshops, consortia, industrial visits, use of the Web sites, and extensive utilization of NIST calibration services are all solid indicators that this division reaches out to industry and forms close relations. However, counting these indices does not reflect the full value and impact that division programs have on the economy. For example, more nuanced information on Internet use could be acquired by providing log-in access and tracking. Appropriately, NIST has begun to commission external groups to independently assess the value of its work. This activity is very important, and initial efforts to assess the value of the NIST thermocouple calibration program through an economic impact study are to be commended. However, this study only included input from wire suppliers and from a limited group of thermocouple manufacturers. This neglect of the end-users resulted in an underestimation of the impact. NIST needs quantitative data to determine which programs have the greatest value in order to use its limited resources most effectively, and therefore quality evaluation must include end-user assessment. Still greater effort to get honest and meaningful assessments of customer value will improve quality and attract long-term funding.

Division Resources

Funding sources for the Process Measurements Division (in millions of dollars) are presented below:

 

Fiscal Year 1997

Fiscal Year 1998 (estimated)

NIST-STRS, excluding Competence

8.0

8.0

Competence

0.9

0.6

ATP

0.2

0.3

Measurement Services (SRM production)

0.1

0.1

OA/NFG/CRADA

0.3

0.4

Other Reimbursable

1.2

1.2

Total

10.7

10.6

Several years ago, funding from other agencies, service fees, and industry grants supported about three-fourths of the activities within the division. Today, internal support (NIST-STRS) accounts for approximately 75 percent of the budget. This shift in policy has

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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enabled programs to proceed efficiently from year to year with an emphasis on technical activities, rather than on promotional activities and the search for uncertain funding. The disadvantages of the increased dependence on internal funding sources include fixed budgets that do not provide much flexibility to respond to new needs. In addition, the division, rather than the laboratory, is now burdened with the responsibility of demonstrating the value of its activities in order to assure continued funding.

Successful completion of the competency phase of several programs will force difficult funding decisions about whether to maintain these projects and where to find the funding for them. The Cavity Ring-Down Spectroscopy (CRDS) project is an example of one that must be continued. The staff have clearly demonstrated the utility of CRDS and have identified state-of-the-art laser diode instrumentation that will allow substantial miniaturization of the equipment, a key to widespread industrial use of this measurement technique.

Staffing for the Process Measurements Division currently includes 59 full-time permanent positions, of which 53 are for technical professionals. There are also 18 nonpermanent and supplemental personnel, such as postdoctoral fellows and part-time workers.

Personnel attrition has taken some research programs below critical mass, and there do not seem to be plans to hire new permanent staff. NRC postdoctoral fellows, although temporary, seem to be the chief source of new or replacement staffing. The panel was told that it is increasingly difficult to attract new postdoctoral fellows, perhaps because salaries are too low to attract a large pool of high-quality candidates in this field.

Over the past few years, there has been significant personnel attrition because of promotions, retirements, deaths, and other factors. If this 5 percent annual attrition rate continues for 10 years, the net reduction will be 40 percent, which seems unacceptable. This division's work in calibrations and standards is vital, and the present level of effort can only be maintained if lost personnel are replaced. This problem could be addressed via longer-term budgeting from Congress.

The quality of the physical plant has been a problem for some research projects and is appropriately being addressed by the construction of new laboratory facilities. This year the panel saw an improvement in laboratory conditions and less crowding than on previous visits. The equipment in the Process Measurements Division is of very high quality. Through the use of a variety of resources, essential laboratory refurbishments have occurred in many areas. New laboratory facilities were provided for research in low-temperature CVD, for housing the thermal CVD spinning disk reactor, for research in diagnostic and sensing applications of self-assembled monolayers, and for housing the new 300 mm plasma reactor and the high-density gaseous electronics conference radio-frequency reference cell. In addition to new instruments, dated equipment, such as an Fourier transform infrared (FTIR) spectrometer used in combustion monitoring, was replaced with high-quality new equipment.

Despite these important improvements, in many of the laboratories temperature control and the presence of particulates in the air continue to be problems. Some laboratories have been renovated and curtained zones placed around certain pieces of equipment to provide smaller areas with the required level of environmental control. Environmental problems are limiting the work in numerous groups, such as the pressure and vacuum laboratory. Many concerns cannot be addressed piecemeal and will require new facility construction to maintain the state-of-the-art nature of the NIST laboratories.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Surface and Microanalysis Science Division
Division Mission

According to NIST documentation, the Surface and Microanalysis Science Division serves as the nation's reference laboratory for chemical metrology research, standards, and data to characterize the spatial and temporal distribution of chemical species and 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 in general agreement with the NIST mission. The mission statement would be improved if the mission or the supporting documentation, such as the division vision and strategic plan, included quantifiable goals and objectives that represent the implementation of the mission. Such objectives would describe a vision of successful research. Similarly, the division will benefit from continuing work on articulating goals and on a roadmap embodying those goals. The mission statement could also mention that the division is an important asset as a national resource in measurement capability.

To be more in compliance with its stated mission statement and the general NIST mission, the division needs to continue to examine national needs. In addition, it is important for the division staff to look beyond their particular current area of expertise to define future research directions. Division management also could benefit from continued definition of quantitative objectives to be used to determine and assess the technical merit of the research.

Technical Merit and Appropriateness of Work

The Surface and Microanalysis Science Division conducts extremely high-level research that defines the spatial and temporal distribution of chemical species and improves the precision and sensitivity of surface and microanalysis techniques. The division is continuing a process of evolution and development of new research efforts. Research efforts that have reached successful conclusion have been terminated, and the staff has moved to work in new areas. It is a rarity for a research staff to demonstrate this level of confidence and vision. The positive impact of the divisional reassessment activities complements the laboratory-level annual reallocation objectives.

The Atmospheric Chemistry Group's work in advanced isotope metrology and chemometrics continues to set the standard for world-class excellence in this area. Methods to measure 14C isotopes in small quantities (< 10 µg) have led to the only technique by which scientists can discriminate unambiguously between emissions from fossil fuels and from biological sources in time-resolved atmospheric samples. The significance of this method has been demonstrated by the work resolving soot from fossil and biomass burning in local effects, such as the wintertime “brown cloud” in the Rocky Mountain front range, and global effects, such as the migration of combustion plumes from North America into the polar atmosphere. This represents the first time that 14C has been measured in the polar snow and is the first combined application of satellite tracking and polycyclic aromatic hydrocarbon fire tracers with particulate carbon isotopic tracers. This combination represents a powerful new complement of independent measures.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

In the gas-phase arena, the capability to resolve emission sources of carbon monoxide through analysis of 14C and stable 13C and 18O isotopes was improved in precision by a factor of six. The technique was also demonstrated to be applicable in the field for the resolution of seasonal and latitudinal variations in carbon monoxide emission sources and atmospheric sinks. Such field data will be critical in understanding and finding ways to reduce overstepping the Clean Air Act's National Ambient Air Quality Standards (NAAQS) for carbon monoxide and ozone. In related work, the Atmospheric Chemistry Group is developing an urban dust particle filter reference material and standard test data to evaluate analysis protocols, thereby improving the accuracy and precision of atmospheric measurements required to establish compliance with NAAQS targets.

The Surface Dynamical Processes Group has excellent expertise in surface spectroscopy and is developing a new effort in near-field scanning optical microscopy (NSOM). This technique potentially can detect chemical species nondestructively and in situ with nanometer resolution. Recent work has concentrated on NSOM images of 100 nm colloidal gold particles and the development of a surface-enhanced Raman scattering tip. If successful, the Raman proximal probe would lead to significant improvements in the sensitivity of surface Raman spectroscopy. In an attempt to understand the complicated surface chemistry occurring during semiconductor processing, the group is also working on understanding TiSi2 growth and the reaction of radicals on silicon surfaces. Another research effort within the group is that involving novel spectroscopy of model membrane surfaces using broadband vibrational sum frequency generation (SFG) at interfaces. This cutting-edge SFG research exploits the group's world-class expertise in femtosecond laser technology and infrared light generation. This effort is complemented nicely by additional scanning probe microscopy studies of these “soft” surfaces.

The Microanalysis Research Group performs state-of-the-art electron and x-ray beam microanalysis. The group focuses on some of the most widely used microanalysis instrumentation in use by industry: scanning electron microscopes, transmission electron microscopes, energy dispersive x-ray spectrometers, wavelength dispersive spectrometers, Auger electron spectrometers (AESs), and x-ray photoelectron spectrometers (XPSs). Pushing the quantitative analysis and spatial resolution capabilities of these methods will have broad and important impacts. The successful completion of the telepresence microscopy project is exciting. This project startup was funded by the NIST director's office and was a collaboration with the Manufacturing Engineering Laboratory intended to facilitate the support of industry by NIST's unique skills and instrumentation. The project used low-cost, easily accessible hardware and Web-based software to facilitate the implementation of the NIST methodology by many laboratories both for intracompany communication and also for effective collaborations with external entities such as NIST.

Several other group activities will have broad impact. The Surface Analysis Data Center will provide a central resource for improved use of AES and XPS. The XPS database, released in September 1997, provides a centralized, evaluated set of reference data for aid in data interpretation. This standard XPS data set will allow analysts to test their ability to identify changes in chemical states using peak fitting algorithms, a large source of misinterpretation of data. The use of the World Wide Web to publicize the availability of this data set and to distribute it free of charge should increase the visibility and therefore the impact of this work.

Of particular note is the group's work in support of the development of high-resolution x-ray spectrometers in collaboration with NIST's Electronics and Electrical Engineering Laboratory

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

in Boulder. The expertise of CSTL's microscopists and spectroscopists is critical in developing a useful spectrometer from the original microcalorimeter research. This research is nearing commercialization and will revolutionize the way that practical microanalysis is performed.

The Analytical Microscopy Group performs state-of-the-art ion and photon microprobe analysis research. Its main focus is on developing new measurement methods and standards for secondary ion-mass spectrometry (SIMS) microprobe material analysis. This group also conducts photon microprobe analysis of materials. Research results are excellent, and the group is extensively involved with industry. The release of the new SRM 2134 for arsenic implants in silicon is very important to the semiconductor industry and supports the metrology needs outlined in the Semiconductor Industry Association Roadmap. This new SRM is an excellent complement to the established reference for boron implants in silicon (SRM 2137). The availability of these two standards will produce more accurate SIMS-depth profiles of real semiconductor materials, resulting in faster transistors via more accurate process/device correlation, more accurate semiconductor process simulators through the production of more accurate calibration data, and better intralaboratory comparisons within companies having multiple SIMS instruments and multiple locations.

Overall, the panel noted that the technical quality, timeliness, and enthusiasm evidenced in numerous projects have been markedly enhanced by cross-division collaboration. Examples include complementary chemical measurements in atmospheric aerosols and the boron and arsenic in silicon implant SRMs.

Impact of Programs

The Surface and Microanalysis Science Division is conducting research needed by many U.S. industries. One prominent example is the semiconductor industry, where decreasing feature sizes continue to force constant improvements in spatial analysis and surface sensitivity. Although it appeared to be well positioned for future developments, the division should be encouraged to continue to reevaluate its goals and assess how well its research is helping U.S. industry. In addition to its many publications, the division might consider what other efforts could be made to disseminate research results more widely. For example, to provide additional industrial guidance, the division could establish more industrial liaisons and promote industrial fellowships for younger staff.

Industry is significantly affected by environmental regulations that require expensive control of emissions to meet NAAQS. When emissions are correctly identified, regulations are effective and economic competitiveness is enhanced. The carbon isotope measurement techniques developed in this division clearly improve the resolution of fossil and biogenic contributions to emissions exceeding the carbon monoxide and particulate standards, a significant and unique capability.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

As global warming emerges as a potential concern, it will be critical that emissions that affect the global radiative energy balance be accurately measured and distinguished. Byproducts of such emissions are often airborne carbon particles that scatter and absorb light. Therefore, the ability to discriminate between various emission sources of such particles, which include transportation, power generation, agricultural clearing, wood stoves, and cooking, will be required to develop sound environmental policies. The division's program to develop techniques for the measurement and analysis of carbon isotopes in the atmosphere shows excellent foresight in anticipating requirements to distinguish and monitor carbonaceous particles in the atmosphere either to define the nature of the environmental impact or, in the event of preventative action, to evaluate its effectiveness. It is important that all interested parties within the United States be made aware of NIST's capabilities in this area.

The Surface Dynamical Processes Group has made recent progress in developing NSOM techniques for chemical resolution at the nanometer scale. These new NSOM techniques are widely embraced by U.S. industries. The fundamental understanding of NSOM emerging from the Surface Dynamical Processes Group will facilitate the quantitative application of this important new optical technique. The new surface-enhanced Raman scattering tip also promises increased sensitivity for surface vibrational spectroscopy. This higher sensitivity will also aid many surface microanalysis problems relevant to a variety of industries. Examples of programs directed at specific industries include the study of soft surfaces and model membrane surfaces, which is relevant to biological research and the ever-expanding biotechnology industry, and the research on TiSi2 interface formation and radical reactions on silicon surfaces, which is very applicable to the semiconductor industry. This latter industry will benefit from NIST SRMs such as SRM 2134 (arsenic in silicon) and SRM 2137 (boron in silicon). Although the sales of these items may not be high in numbers, the impact will be broad.

Industrial collaborations are particularly evident in the Microanalysis Research and Analytical Microscopy groups, which possess an especially valuable set of instruments designed to carry out research funded by the U.S. Air Force. This collection of tools is an effective arsenal to tackle many questions of interest to industry. In addition, these instruments are often identical to those used in industrial laboratories; as a result, companies can benefit from NIST's expertise in the use and calibration of these instruments.

That the division does not perform formal assessment of its impact on industry is of concern to the panel. Such evaluations are necessary to provide the management team and research staff with feedback on the division's importance to U.S. industry and to allow them to direct their research into appropriate new areas. Appropriate metrics are needed to focus research efforts effectively on industrial needs.

Division Resources

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

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×
 

Fiscal Year 1997

Fiscal Year 1998 (estimated)

NIST-STRS, excluding Competence

4.4

4.5

Competence

0.4

0.4

ATP

0.2

0.4

Measurement Services (SRM production)

0.1

0.0

OA/NFG/CRADA

2.9

2.8

Other Reimbursable

0.4

0.3

Total

8.3

8.4

As the panel noted in last year's assessment, the division depends heavily on funding from other government agencies (OA) for its major capital acquisitions. In the future, such reliance could inhibit the division's ability to pursue new ideas in surface and microanalytical research that are not in line with the needs of other government agencies.

Staffing for the Surface and Microanalysis Science Division currently includes 37 full-time permanent positions, of which 34 are for technical professionals. There are also 15 nonpermanent and supplemental personnel, such as postdoctoral fellows and part-time workers.

The entire research staff is excellent. The personnel include three NIST Fellows who are active in a wide range of research projects. In addition, division staff members are to be congratulated on the outstanding accomplishments that resulted in the awarding of a Department of Commerce Bronze Medal and a Department of Commerce Gold Medal. Morale is high throughout the division. An examination of program staffing levels shows that the distribution of human resources is appropriate. In general, there are no personnel problems, and important projects do not lack key people. Leadership is good in the four groups. The panel was pleased that an official group leader for the Atmospheric Chemistry Group has been identified and that he has assumed a leadership role. The CSTL management faces the challenge of ensuring continued strong leadership at the divisional level, as the division chief plans to retire in the next year or so.

The panel observed that the division has limited technical support staffing, which forces the technical professionals often to engage in activities outside of their expertise. For example, scientists with PhD degrees are building Web pages, designing computer networks, and changing pump oil. Alternative methods, such as service contracts for equipment and computers or hiring dedicated support staff, might address this problem. The instrumental resources in the division are excellent. The Analytical Microscopy Group will soon receive a state-of-the-art time-of-flight SIMS instrument, which will enable NIST to assume the lead in the definition of proper measurement practices for this new analytical technology. The decision to pursue the acquisition of a high spatial resolution AES and the related staff expertise in the Microanalysis Research Group is very appropriate and will allow the division to address pressing and increasingly difficult problems with quantitative analysis in this popular analytical area.

In last year's assessment, the panel emphasized various difficulties encountered by the division resulting from the low quality of experimental facilities. This year, NIST personnel noted that initial funding for construction of the AML has been obtained and that, if additional funding commitments can be obtained for fiscal year 1999, construction is slated to begin in December

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

1998. Given that the length of such construction is estimated at 44 months, it is critical that the division also develop and fund a short-term facility improvement plan as well as a contingency plan in case the building is not constructed. Also, the division is encouraged to work with NIST site facilities staff to improve the quality of power supplied to their equipment. Although the purchase of uninterruptible power supplies can provide backup in a few areas, it is not a cost-effective solution for the Chemistry and Physics buildings. Finally, the Atmospheric Chemistry Group is not slated to move into the AML with the rest of the division. Laboratory and division management may want to prepare for organizational problems and productivity deficits that could result from this split.

Physical and Chemical Properties Division
Division Mission

According to NIST documentation, the Physical and Chemical Properties Division is 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 division provides technical research and services, SRD, SRMs, and calibrations to promote U.S. economic growth and to assist U.S. industry, other government agencies, and academia in solving problems of national importance.

The programs of this division remain firmly rooted in the central NIST mission to promote economic growth by working closely with industry. Although every group in the division has ties to appropriate industries to some degree, this division as a whole maintains a desired balance between research directed toward industrial concerns and work motivated by a more long-term view of the nation's science and technology needs.

Technical Merit and Appropriateness of Work

As has been noted in previous assessments, the skill set of the personnel in this division is complementary, unique, and highly valued. The mix of expertise covers the range from experiment to theory and includes thermodynamics, transport properties, and chemical kinetics. The staff form virtually the only teams left in the world who are actively involved in making precise and fundamental measurements of thermodynamic properties and who have the expertise to critically evaluate their own and existing literature data in order to build databases of usable information. The capabilities of this division have been further enhanced in the past year by the creation of the Computational Chemistry Group.

The merit of the work done by the division is high, and the research is definitely relevant to the needs of industry. An important feature is the strong synergism between experiment and theory, as evidenced by the interactions within and between the various groups. Division management has done an excellent job of directing the groups located at the NIST facility in Boulder in support of the laboratory and NIST missions and of clearly articulating programmatic

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

goals. In addition, the Gaithersburg and Boulder groups are well coordinated, but not overlapping. For example, the distinctive identities of the Experimental Properties of Fluids and Fluid Science Groups have now been clearly defined.

Formation of the Computational Chemistry Group has strengthened the division, and this group should substantially expand the division 's work on providing evaluated databases. For example, the additional computational capabilities should improve evaluators' ability to identify erroneous rate-constant measurements. The availability of such a theoretical tool makes it feasible to include evaluated rate-constant data in the gas phase kinetics database. This improvement will enable scientists to include more reliable rate constants in kinetic models of reaction systems.

A continuing concern is that the gas phase kinetics database has not been updated since November 1994. The utility of the previous release of this database continues to diminish as more and more information becomes available in the literature without being captured and disseminated in an update. The panel strongly supports the rapid completion and release of the update.

In the future, the division is well placed to make significant contributions to several national budget initiatives for fiscal year 1999. In the initiative on global climate change, the division's expertise will be valuable to studies on membrane-based alternatives to distillation and on alternative working fluids for energy-efficient and environmentally benign processes. Also, the division's expertise and capabilities in thermophysical property determination of gases and chemical kinetics will be important components in the initiative on research relevant to semiconductors.

The program planning process is well coordinated with personnel development. Staff members are required to develop a performance plan at the beginning of each fiscal year, in concert with the division's leadership. This process not only requires the staff to assess their goals for the coming year but also provides a source of ideas for new initiatives. The year-end review of staff and other reviews during the year provide a mechanism for comparing stated goals with achievements. This process is commended.

Two projects in this division were particularly noteworthy, and details of the merit and impact of these programs are described below. The first such project is the NIST/EPA/NIH Mass Spectral Library with associated algorithms, and the second is the work on thermophysical properties of next-generation refrigerants.

This division is responsible for the NIST/EPA/NIH Mass Spectral Library, a widely utilized, comprehensive collection of reference mass spectra used for the identification of unknown compounds. This library is sold with 60 percent of all new mass spectrometer data systems and has been installed on more than 20,000 data systems overall. On January 1, 1998, the most significant new release in its 25-year history took place. With a directed measurement program and incorporation of high-quality collections from external sources, the number of compounds in the library was increased by 75 percent, bringing the total to 130,000 spectra of 108,000 compounds. Even more significantly, an 8-year program of intensive, spectrum-by-spectrum evaluation was completed in which each spectrum was examined for quality and consistency with chemical structure. As a result, thousands of lower-quality spectra were replaced by higher-quality spectra, and many hundreds of incorrect spectra were deleted. This evaluation also led to substantial improvements in the correctness and consistency of chemical names and to the completion of drawings of chemical structures for virtually all compounds. For the first time in 25 years, the library is now fully evaluated. Future efforts will focus on

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

continuing to ensure the reliability of spectra of important compounds, especially by adding confirming replicate spectra.

Since the utility of the library depends on the effectiveness of library search algorithms, significant effort has been devoted to testing, refining, and optimizing these algorithms. In fact, NIST algorithms are now available on most new systems employing the NIST/EPA/NIH Mass Spectral Library. Important progress has also been made in the development of algorithms for extracting pure component mass spectra from complex gas chromatography/mass spectrometry (GC/MS) data files and for using these spectra to identify target compounds. This work was performed specifically for the Department of Defense to assist in the verification of the Chemical Weapons Convention (CWC), a major international treaty ratified by the U.S. Senate in 1997. To prevent the loss of confidential information, a fully automated system was required that could identify compounds related to chemical weapons with very low risk of making false positive identifications. Such a capability was developed, thoroughly tested, and implemented in a software package that has passed stringent treaty requirements to become a central component in CWC verification. These algorithms will also find wide use in other areas of chemical analysis and are provided with the new release of the NIST/EPA/NIH Library.

The next example of very high quality work within this division is also from a long-term project. For more than 10 years, this division has been providing U.S. industry with the thermophysical properties data and models needed to identify and implement environmentally acceptable alternatives to the chlorofluorocarbons (CFCs) and hydrochlorofluorocarbons (HCFCs) in air-conditioning and refrigeration equipment. After the 1987 signing of the Montreal Protocol on Substances that Deplete the Ozone Layer, industry faced the formidable challenge of shifting from tried-and-true products to new refrigerants and new technology in a short period of time. Relying extensively on high-accuracy thermophysical properties measurements and models provided by the division, industry succeeded in producing a new generation of refrigerants and energy-efficient equipment that will save billions of dollars a year while creating a healthier global environment.

During the past year, development has been completed on a major new version of the REFPROP (refrigerant properties) database and computer program. The new version implements the most accurate pure fluid and mixture models currently available and provides a separate graphical user interface for accessing the models. REFPROP serves as a major mechanism for transferring the results of the division's entire program on alternative refrigerants to its customers in industry.

With the ongoing concern about global warming, the division continues to focus on providing industry with the properties, data, and models needed to maximize the energy efficiency of refrigeration equipment. Interest is growing in natural refrigerants, including hydrocarbons and ammonia, and also in novel compounds, such as fluorinated ethers, which have much lower greenhouse warming potentials than the hydrofluorocarbon (HFC) refrigerants. Finally, HCFC-123, which is used in many large central-plant chillers, must be phased out by 2030 under the Montreal Protocol, and NIST is prepared to provide data on HFC-245fa and other promising alternatives to assist industry in selecting the best replacement.

There are eight groups in the Physical and Chemical Properties Division; brief descriptions of their programs follow.

The Fluid Science Group uses acoustics and other novel approaches to develop state-of-the-art techniques for measuring the thermodynamic and transport properties of pure fluids and

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

mixtures, such as alternative refrigerants and semiconductor processing gases. Another research focus is on 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 heat capacity, thermal conductivity, and viscosity of semiconductor process gases in order to develop more accurate flow-metering devices; development of laboratory standards for accurate measurement of viscosity and Prandtl number of industrially important gas mixtures; and development of a primary pressure standard in the 500 to 2000 kPa range based on the measurement of the dielectric constant of helium.

The Chemical Reference Data and Modeling Group compiles, evaluates, correlates, and disseminates SRD. It also develops and disseminates electronic databases and software for thermodynamics, chemical kinetics, mass spectroscopy, and infrared spectra. A major activity is the NIST/EPA/NIH Mass Spectral Library, which is highlighted separately above. Other activities include the compilation of kinetics data for chemical reactions in the gas phase and the development of the NIST Chemistry WebBook, which is a searchable compilation of chemical data designed for Internet access.

The Computational Chemistry Group was formed in November of 1997. It develops and applies computational chemistry methods for estimation and prediction of the chemical and physical properties of molecules. It evaluates new theories, models and estimation methods, and computational techniques for rate constants and thermochemical properties. Future plans include development of resources to provide guidance to nonexperts in the use of computational chemistry methods. Current activities include work in computational thermochemistry, methods for vibrational analysis of large molecules, improved methods for geometry optimization, computational chemistry in solution, and transition state theory.

The Experimental Kinetics and Thermodynamics Group uses a wide range of state-of-the-art measurement techniques to obtain kinetic and thermochemical data on species that are important in the chemical and related industries. It also certifies SRMs for thermodynamic properties important to science and industry. Current activities include development of a broad database for advanced oxidation technologies used for treatment of hazardous and some nonhazardous wastes; measurement of environmental fates and impacts of industrial compounds; thermodynamics of industrially important materials and processes; and development of new capabilities, such as ring-down spectroscopy for studying chemistry near surfaces and thin films.

The Process Separations Group performs basic and applied research on a variety of separation processes including distillation, supercritical fluid extraction, adsorption, and membrane separations. It also provides critically evaluated data and models needed to design and/or select more efficient separation processes. Current activities include development of systematic screening procedures for alternative solvents; vapor/liquid equilibria studies on azeotropes and near azeotropes; database development for properties of membrane materials; databases for chromatographic analysis of natural gas mixtures, odorants, and alternative refrigerants; and development of improved chromatographic methods driven by new industry standards for gas-line condensate analysis.

The Experimental Properties of Fluids Group performs experimental research and develops and maintains high-accuracy apparatus for measuring the full complement of thermodynamic and transport properties of fluids and fluid mixtures over wide ranges of temperature, pressure, and composition. It also provides comprehensive thermophysical property measurements for technically important pure fluids and mixtures, including common organics and

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
×

inorganics, hydrocarbons, refrigerants, and aqueous systems. Current activities include development and construction of a new apparatus for the simultaneous measurement of vapor-liquid equilibrium and interfacial tension; development and construction of a new high-temperature adiabatic calorimeter for isochoric heat capacity measurements of gases and liquids; and new vibrating-wire, torsional crystal, and capillary viscometers for precision measurements of fluid viscosities over broad ranges of temperature and pressure.

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 models and correlations of high accuracy to describe and predict the thermophysical properties of fluids and fluid mixtures. It also provides comprehensive and evaluated Standard Reference Data and electronic databases for the properties of technically important fluids and fluid mixtures. Current activities include development of standard thermodynamic surfaces for fluids using extended corresponding states, fundamental studies of fluid-solid phase transitions, studies of surfactant adsorption on clays by neutron scattering, and structure evolution and rheology of gelling colloidal silica by neutron scattering and rheometry.

The Cryogenic Technologies Group develops improved measurement and modeling techniques for characterizing basic cryocooler components and processes. It develops state-of-the- art cryocoolers for specific applications. It also provides measurement methods, standards, and services for flow under cryogenic conditions. Research on the pulse-tube refrigeration system is supported by the National Aeronautics and Space Administration (NASA). This group is also developing a cryogenic catheter for the treatment of arrhythmias and abnormal uterine bleeding. The liquid nitrogen flow calibration facility is being upgraded to allow more accurate measurement of low flow rates. Current activities include the work on advanced refrigeration systems and cryogenic catheters.

Impact of Programs

All groups in this division make a strong, well-directed effort to communicate their results to the scientific and engineering communities. An example of their success is the widespread recognition NIST received for providing U.S. industry with the data and models needed to identify and implement environmentally acceptable alternatives to CFCs and HCFCs in air-conditioning and refrigeration equipment. The impact of the Chemistry WebBook on the chemical industries and on university researchers is also considerable. In the 5 months after the August 1997 update, the number of data pages generated for users per month averaged well over 200,000. Many small businesses that cannot afford expensive data resources of their own will benefit from the availability of inexpensive databases over the Web.

There are several examples of fundamental work that have direct impact on industry. One is the development of models and databases for thermophysical properties of fluids and fluid mixtures to enable faster, more accurate, and reliable design and simulation of chemical processes. In the Cryogenic Technologies Group, the development of cryogenic catheters for cryosurgical procedures has resulted in a CRADA with CryoGen, Inc., a medical device company. The device uses a Joule-Thompson cycle for refrigeration and can be used as a cardiac catheter for the treatment of heart arrhythmia and as a uterine catheter. Joint patents have been issued to NIST

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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and CryoGen, Inc. With Lockheed Martin of Denver, the Cryogenic Technologies Group has developed the world's smallest pulse-tube refrigerator. This refrigerator is scheduled to fly on the Space Shuttle in April of 1998 and will be used in future cooling applications in space. The group is also working with NASA to develop a pulse-tube refrigerator for use in future missions to Mars.

NIST has commissioned economic impact assessments for six programs in the CSTL, two of which are from the Physical and Chemical Properties Division: Alternative Refrigerants to Replace Ozone-Depleting CFCs and Advanced Refrigeration Systems for Cryogenic Applications. The analysis of the former project is complete and concludes that NIST research in this field has resulted in a social rate of return (SRR) of 433 percent, an implied rate of return of approximately 21 percent, and a benefit-to-cost ratio of 3.9:1. This SRR represents relatively high economic impact when compared with that of SRRs for other NIST projects for which economic impact studies have been performed. These results were computed by an outside organization and were based on detailed surveys of major producers of refrigerants and refrigeration equipment. The assessment considered direct benefits only; it did not include such indirect benefits as the effects of NIST's program on the energy efficiency of refrigeration equipment.

Note that a very different example of work with direct impact on industry is the release of the NIST/EPA/NIH Mass Spectral Library, which was described in detail in the section on technical merit.

Division Resources

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

 

Fiscal Year 1997

Fiscal Year 1998 (estimated)

NIST-STRS, excluding Competence

8.6

8.7

Competence

0.1

0.1

ATP

0.1

0.4

OA/NFG/CRADA

4.2

4.4

Total

13.0

13.6

The high level of OA funding is a problem throughout the division. This division is only one of five within CSTL, yet in fiscal year 1997, it produced 42 percent of all OA funding within the laboratory. Such funds are difficult to acquire and are usually earmarked for very specific work. Although currently most of the externally supported projects are consistent with the division's mission, this situation cannot be expected to continue indefinitely. The present level of OA funding, more than one-third of the division's budget, is too high and imposes on the division management and staff a heavy burden of fundraising and administrative activities, which can be detrimental to the technical mission of CSTL. The excessive reliance on OA funding also distorts the strategic planning process by locking the division into projects that require long-term effort,

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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which can result in lost opportunities. For example, although the NASA-supported project on critical-point viscosity measurements has resulted in excellent scientific work, the long-term nature of this project has forced the staff member leading this work to devote himself exclusively to this project and forego additional scientific opportunities.

Data collection and evaluation as well as database development and dissemination are important to the general scientific community, especially to industry, over the long term. Because such projects represent a core element of the NIST mission, they should be directly supported through base funding rather than be dependent on OA support. NIST walks a fine line between universities and industry and acts as a unique bridge between the often short-term interests of industry and the longer-term, more fundamentals-based approach of universities. A lack of outside funding for connective projects would not be a problem if sufficient support were available from NIST's direct congressional appropriations.

Staffing for the Physical and Chemical Properties Division currently includes 68 full-time permanent positions, of which 58 are for technical professionals. There are also 17 nonpermanent and supplemental personnel, such as postdoctoral fellows and part-time workers. The NIST staff in this division is split approximately equally between Gaithersburg and Boulder.

The Physical and Chemical Properties Division has more guest researchers and contractors (approximately 60 full-time equivalents) than most divisions of the laboratory. The panel supports the continuing presence of these visitors who bring a wide range of expertise and provide additional external input into the divisional planning process.

The division's laboratory space in Boulder is currently inadequate. However, this situation is expected to change shortly when the new building for NOAA personnel is completed and additional space in Building 2 becomes available to the division.

Analytical Chemistry Division
Division Mission

According to NIST documentation, the mission of the Analytical Chemistry Division is to conduct research concerning the qualitative and quantitative determination of chemical composition; develop and maintain state-of-the-art chemical analysis capabilities; provide measurement quality assurance through reference materials, data, and services; and provide a basis for U.S. chemical traceability and international comparability.

The Analytical Chemistry Division is the fundamental chemical metrology component of the CSTL and NIST. The division mission is fully and effectively integrated into the overall mission and goals of both the laboratory and NIST. Divisional programs provide chemical measurement standards, accurate and reliable chemical compositional data, and research in chemical measurement science in support of NIST and laboratory missions. The mission includes the development and maintenance of state-of-the-art chemical analysis capabilities.

The dedication of the personnel and their commitment to quality were very evident. The entire staff had a clear sense of the division 's mission and their individual roles. The programs demonstrated that providing standards and standard methodology to the United States and international community was a division priority and a fundamental part of the mission. The panel was particularly pleased by the division chief's fiscal responsibility and determination to meet the

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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division's commitments. There is a healthy balance between a commitment to develop new SRMs and the need to maintain existing SRMs. However, the panel was concerned that the standards program appears to be competing for the resources that are also needed to conduct necessary measurement science research.

The panel was satisfied with the planning processes used within the division. It was evident that the entire organization utilizes the quality processes required to control their business and research activities including project prioritization and resource allocation processes. All division research and service projects are reviewed on an annual basis to assess the quality of the work and fit with the mission and with industry needs.

Technical Merit and Appropriateness of Work

Research activities in the Analytical Chemistry Division are focused on the chemical measurement sciences using high-performance analytical tools such as mass spectrometry (MS), sensing technologies, classical analytical methods, gas metrology, nuclear analytical methods, organic analytical methods, and spectrochemical measurement methods. These programs are carried out by five groups: Spectrochemical Methods, Organic Analytical Methods, Gas Metrology and Classical Methods, Chemical Sensing and Automation Technology, and Nuclear Methods. A 3-year restructuring plan is under way. This activity aims to establish a strategic plan for division research and service activities, adjust the funding profile for division research and service activities, and reengineer the division's delivery of standards to reduce backlog, increase the ratio of new to renewal SRMs, and establish an infrastructure for NTRMs and International Comparability for Chemical Measurements.

The Chemical Sensing and Automation Technology Group develops and applies new technologies, techniques, and standards for chemical sensing, sample preparation, and laboratory automation for chemical analysis. In 1997, the group terminated its work on laboratory automation standards and formally closed down the Consortium on Automated Analytic Laboratory Systems. Therefore, this group expects to be renamed in the near future to more accurately reflect its current focus on advanced measurement methods. This team has historically provided optical filters to calibrate the transmittance and wavelength scales of visible and ultraviolet (UV) spectrophotometers. Recently, they have initiated development of an NTRM program for optical filter reference materials to augment the current “calibration program” in which filters are returned to NIST every 2 years for revalidation. Such NTRM programs allow some of the routine standards activities to be conducted by external organizations, thereby enabling NIST personnel to focus on new topics. For example, this group has been exploring several techniques for use in quality control of incoming raw material in the pharmaceutical industry. These new methods include the use of Raman spectroscopy as well as fiber-optic technology for making remote measurements. This group has also been conducting research on microfabricated measurement devices including the creation of microchannels in plastic (microfluidic devices). The development of such tools will enable U.S. industry to make remote measurements with handheld devices, and this new technology has profound implications within the pharmaceutical, biotechnology, medical, and forensic communities.

Research in 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 MS instruments. This group has enhanced its

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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measurement capability in several areas; new tools include two inductively coupled plasma mass spectroscopy (ICP-MS) instruments (one is a high-resolution magnetic sector instrument) and a wavelength dispersive x-ray fluorescence (WD-XRF) spectrometer. The ICP-MS is a workhorse of the laboratory for certification of inorganic chemical SRMs, and the team working in this area leads the international community in the development and implementation of protocols for international comparisons such as lead in water. The team working in the XRF area has revitalized its focus on the metals industry, particularly on the accurate measurement of alloys.

This group has developed a new inductively coupled plasma-optical emission spectrometry (ICP-OES) method based on a drift correction algorithm with performance that rivals classical methods in terms of precision (relative precision of 0.02 to 0.2 percent). This new technique will have a dramatic impact on the spectrochemical solution SRM business. The spectrochemical SRMs are by far the highest volume standards with several thousands sold every year. This high-precision ICP-OES technology is well suited for transfer to the private sector and will permit the development of a 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.

The Nuclear Analytical Methods Group continues research on the use of neutron beams as analytical probes both with Prompt Gamma Activation Analysis and with Neutron Depth Profiling. NIST recognizes the value of using two complementary methods for validation of SRMs. Neutron Activation Analysis is well suited to provide one of these methods because of the normal lack of interference found in conventional analytical techniques. New methods for analysis of methyl mercury without extraction are being explored. Long-term research includes development and application of cutting-edge neutron focusing technology to provide three-dimensional compositional mapping of thin film semiconductor materials. As a result of the heavy investment in capital for the accelerator facility, this group will not move into the newly constructed facilities as planned for the rest of the Analytical Chemistry Division.

The Organic Analytical Methods Group focuses its research and application efforts on the areas of health care, nutrition, environmental monitoring, and forensic analysis. There is a heavy emphasis on MS because of its specificity and inherent sensitivity. The group has developed several external collaborations, such as monitoring environmental contaminants in marine species with NOAA scientists in South Carolina. Within NIST, staff work with the Office of Law Enforcement Standards in the Electronics and Electrical Engineering Laboratory on the development of new and effective forensic measurement tools. One of the key challenges for all these types of measurements is “microhomogeneity,” and hence this group has been exploring methods to assure necessary homogeneity for accurate small-size SRMs. Studies are under way to assess and eliminate laboratory-to-laboratory variances in DNA fingerprinting. Liquid chromatography (LC) coupled to MS methods and standards will enable the accurate identification and quantification of important biological compounds in baby foods, infant formula, and human serum albumin. Capillary electrophoretic methods are being developed to characterize the structure and effectiveness of liposomes (phospholipid micelles) in selectively delivering bioactive agents across cell membranes to active enzyme sites. New reference methods are under development using biomarkers such as Troponin I in blood employing various methods including capillary electrophoresis, LC, and LC/MS. Several new SRMs have been developed to support measurement activities in the environmental, health care, and foods sectors. These new materials certify a wide variety of analytes including contaminates, vitamins, and trace elements.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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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. Routine applications for which SRMs are maintained include stack gas analysis and automobile emissions. Real-time analysis of oxygenated hydrocarbons is considered a priority. Research is being conducted to develop a standard, open-path, FTIR database for making quantitative measurements of EPA-designated hazardous air pollutants. New programs involve primary standards for trace atmospheric species, air standards for the California Air Resources Board, and volatile organic analyses for the EPA program. This group is actively involved with international intercomparisons via a European collaboration on measurement standards in such areas as primary gases for the automotive industry, conductivity for water quality, and pH standards. This program will allow mutual recognition of European and NIST Certified Reference Materials for quality assurance and in making regulatory and trade agreements with the United States. The group is enthusiastic about the value of this activity, but the international alternative approach to measuring pH makes this method more complex to implement. The group pioneered the NTRM program and has implemented programs with 10 specialty gas venders certifying 61 NTRM batches resulting in 100,000 NIST traceable gas standards for end-users over the past 3 years.

In regard to the technical merit of future work, this division has proposed that work begin on microfabricated analytical devices and has applied for Competence funding in 1999 to support such a project. This area is critical to U.S. industry for a wide range of applications in the environmental, pharmaceutical, forensic, and health care areas. Investigation of this technology 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.

The division has created 4 CRADAs in 1997 compared with 12 in 1996. However, the division remains highly dedicated to informal partnerships with industry which can have a positive impact for U.S. companies, an approach supported by the panel, which believes it to be a healthy direction. Overall, publications by this division have increased from 133 in 1996 to 172 in 1997. Publications provide individual recognition for NIST scientists within their peer groups while also enhancing NIST's reputation internationally. 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 such intercomparisons become more vital as trade becomes more global.

Calibrations or recertifications have increased to 350 in 1997. The combined numbers of SRMs and NTRMs have remained constant at approximately 190, but the balance has shifted as the number of 1997 NTRMs has increased by 20 percent over 1996. The division continues to improve these programs. Some directions that are particularly appropriate include the efforts to reduce SRM backlog, increase the ratio of new to renewal SRM effort, evaluate modes for SRM value assignment, and establish infrastructure for traceability and comparability for chemical measurements through intercomparison of primary standards among international laboratories. The panel considered the NTRM program to be excellent work and applauds its continued expansion beyond its success in the area of gas standards. One concern is whether NIST management will establish a single system to administer NTRM activities across organizational

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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units, which would ensure that individual divisions are not unduly burdened with administrative tasks at the expense of valuable research activities.

Impact of Programs

This panel was satisfied that the Analytical Chemistry Division programs produce a broad and effective impact on industry. The new NTRM activities have provided greater availability of SRM and new business opportunities for the companies producing the NTRM standards. The focus on a broad spectrum of applications results in new measurement capabilities and important SRMs and NTRMs that meet industrial needs in chemicals, electronics, automotive research, petroleum refining, instrumentation, biotechnology, environmental technologies, health care, and aerospace. Measurement methods derived from division research activities are also used to establish and maintain chemical measurement traceability links for producers of commercial reference materials (such as gases, optical filters, and spectrometric solutions) and measurement comparability links with chemical metrology laboratories worldwide. The capabilities gained from these activities establish and maintain the national infrastructure that provides U.S. industry with the tools necessary to achieve international comparability of chemical measurements.

The division actively participates in intercomparability programs among national and regional standards laboratories to facilitate international trade. Structured intercomparison programs with other national metrology laboratories remain the basis for formal establishment of equivalence among primary methods and standards important for global commerce. The amount of resources dedicated to international comparative methodology increased significantly in 1997. Such activities include research collaborations with the North American Metrology Organization, the Inter-American System for Metrology (SIM), and the Consultative Committee on Amount of Substance, as well as strategic collaborations with other national metrology laboratories.

An example of this division's impact on a specific industry can be seen in the work to establish NIST traceability for important health markers. Already, isotope dilution MS methods have been used to provide standards for the analysis of cholesterol with a large impact on the cost of health care. Further work is under way to establish reference methods for other important biomarkers. Development of accurate methods for two of these analytes is an important component of the ongoing collaboration with the College of American Pathologists. Several other new SRMs are being developed to support measurement activities in the environmental, health care, food, and nutritional labeling arenas.

The division has been responsible for the successful implementation of the NTRM Program. NIST provides nearly 1,300 different types of SRMs and in fiscal year 1997 sold nearly 40,000 SRM units to approximately 5,000 different customers; approximately two-thirds of these units require certification of chemical composition by the Analytical Chemistry Division. In fiscal year 1997, 61 batches of NTRMs were certified by the Analytical Chemistry Division (double the number certified in fiscal year 1994).

The quality of the standards provided through SRMs and NTRMs is outstanding, and it is essential that NIST keep control over the standards process to assure continued quality of production and accuracy of certifications. Demand for these reference materials is global, and there is a growing need to develop new reference materials to meet industry and regulatory compliance needs. The need for the continued traceability of products in commerce and

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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regulatory compliance to assure acceptance on a worldwide basis is critical. However, there is a growing concern over the proportion of resources dedicated to the synthesis and recertification of SRMs and the development of new SRMs. Currently about one-half of the Analytical Chemistry Division's budget, roughly $6.5 million dollars, is devoted to maintenance and development of standards. This level of involvement may have a negative impact on the division's ability to perform cutting-edge measurement research.

To assess its impact on industry, the division solicits input from U.S. companies on their technological needs. These interactions drive divisional planning and program prioritization. Extensive ties to industry and participation in national and international committees and professional organizations permit direct community assessment of NIST programs. In addition to these personal contacts, the division seems to have made an attempt to determine the economic impact of its activities and plans to evaluate the mechanisms used to assess its impact in several areas, such as health and food standards and gas NTRMs. However, the laboratory does not yet have a general set of metrics that can be used to evaluate the economic impact of future activities.

Division Resources

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

 

Fiscal Year 1997

Fiscal Year 1998 (estimated)

NIST-STRS, excluding Competence

7.3

8.0

ATP

0.2

0.0

Measurement Services (SRM production)

2.1

2.2

OA/NFG/CRADA

1.9

2.3

Other Reimbursable

1.1

1.4

Total

12.5

13.9

Recently, the division has aimed to change its funding profile and reengineer delivery of SRM services. Over the past few years, a plan to accomplish these goals has been carefully implemented as the division has successfully adjusted its structure and personnel in response to budgetary pressures. The panel strongly supports and endorses the division's strategic plan. Continued reduction of the division dependency on OA funding is also supported by the panel. It should be noted that approximately $1.2 million of the estimated fiscal year 1998 STRS funding is specifically earmarked for the development of new SRMs and NTRMs and for providing international comparability of measurements.

At the beginning of 1999, the division plans to move into new facilities in the ACSL. The efficiency of the move will be critical to the division 's productivity this year. The panel was impressed by the plans in place to implement a phased move and is confident that it will be accomplished with as little interruption as possible. On a longer time scale, division management

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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has developed a 5-year capital plan that adequately addresses the need to upgrade the analytical capabilities and has increased their capital budget by 50 percent over the past 3 years. The general focus of the research and measurement service activities within the division is expected to be stable over the next year. However, some resources will be redirected to address analytical instrument calibrations and transfer issues.

Staffing for the Analytical Chemistry Division currently includes 67 full-time permanent positions, of which 61 are for technical professionals. There are also 23 nonpermanent and supplemental personnel, such as postdoctoral fellows and part-time workers.

The division continues to make excellent use of postdoctoral fellows and visiting scientists. Nonetheless, the division still has too few scientists. Several experienced personnel were lost during 1997, and in certain areas such as traditional wet analytical chemistry, these people have proven to be difficult to replace. Clear succession planning and cross training would enhance staff retention and recruitment. The work in wet chemistry provides vital support to the NIST mission, and staff vacancies in this area need to be filled.

MAJOR OBSERVATIONS

The panel presents the following major observations.

  • Overall, the technical merit of the work was excellent, and the results produced in the CSTL are of vital importance to U.S. industry. In particular, the panel was pleased to note the release of the updated Mass Spectral Library. Also, the panel was impressed by the projects on standards for Raman spectroscopy and on the microcalorimeter x-ray detectors, which are excellent examples of the value to be gained from interdivisional or interlaboratory collaborations.

  • The CSTL continued to have exemplary management at the senior level as well as in numerous divisions. Over the past year, the planning process has shown significant improvement. The laboratory is working on setting measurable goals and objectives, an activity encouraged by the panel. Suitable external feedback mechanisms will vary depending on the maturity of the technology; also, standards and technology efforts require different measures of success.

  • The facilities available to the Chemical Science and Technology Laboratory are improving. This year the addition to the Center for Advanced Research in Biotechnology was occupied, and the Advanced Chemical Sciences Laboratory will be finished by the spring of 1999. Although the panel was pleased to hear about funding allocations for the Advanced Measurement Laboratory, such a building will not be completed until well into the future, and it is important to develop and implement a plan for upgrading the present facilities to prevent impedance of the laboratory's ability to perform state-of-the-art measurement work.

  • Personnel levels are steady or declining as a result of flat budgets and retirements. The number of projects per staff member is high, which makes it harder for the laboratory to maintain its work on new measurement technologies. The programs that produce SRMs and perform calibrations are also growing, and these services take priority. Therefore, the panel applauds the development of NIST Traceable Reference Materials, although proactive

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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management of this program will be necessary to ensure that it does not become an administrative burden for the technical staff.

Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Page 80
Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Page 81
Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Page 82
Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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Page 83
Suggested Citation:"4 Chemical Science and Technology Laboratory." National Research Council. 1998. An Assessment of the National Institute of Standards and Technology Measurement and Standards Laboratories, Fiscal Year 1998. Washington, DC: The National Academies Press. doi: 10.17226/9515.
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