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4
Chemical Science and Technology Laboratory
35
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36
AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003
PANEL MEMBERS
James W. Serum, SciTek Ventures, Chair
Alan Campion, University of Texas, Austin, Vice Chair
John Ball, U.S. Army Primary Standards Laboratory
Jeffrey B. Bindell, University of Central Florida
Ulrich Bonne, Honeywell Laboratories
Douglas C. Cameron, Cargill, Inc.
John W. Kozarich, ActivX Biosciences, Inc.
Max G. Lagally, University of Wisconsin at Madison
R. Kenneth Marcus, Clemson University
Mack McFarland, Dupont Fluoroproducts
James D. Olson, The Dow Chemical Company
Athanassios Z. Panagiotopoulos, Princeton University
Gary S. Selwyn, Los Alamos National Laboratory
Michael L. Shuler, Cornell University
Christine S. Sloane, General Motors Corporation
Peter Wilding, University of Pennsylvania Medical Center
Jerome J. Workman, Jr., Argose Inc.
Submitted for the panel by its Chair, James W. Serum, and its Vice Chair, Alan Campion, this
assessment of the fiscal year 2003 activities of the Chemical Science and Technology Laboratory is
based on site visits by individual panel members, a formal meeting of the panel on February 25-26,
2003, in Gaithersburg, Maryland, and documents provided by the laboratory.
1U.S. Department of Commerce, Technology Administration, National Institute of Standards and Technology, Chemical
Science and Technology Laboratory: Annual Report FY2002, NISTIR 6954, National Institute of Standards and Technology,
Gaithersburg, Md., February 2003.
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CHEMICAL SCIENCE AND TECHNOLOGY LABORATORY
LABORATORY-LEVEL REVIEW
37
The Chemical Science and Technology Laboratory (CSTL) is the nation's reference laboratory for
chemical measurements. Its mission is to provide a chemical measurement infrastructure to support and
enhance U.S. industry's productivity and competitiveness; assure equity in trade; and improve public
health, safety, and environmental quality. The laboratory is organized in five divisions: Biotechnology,
Process Measurements, Surface and Microanalysis Science, Physical and Chemical Properties, and
Analytical Chemistry (see Figure 4.1~. Following the panel's major observations from this year's
review, this chapter presents an overall assessment of the laboratory. Chapter 11 provides division-level
assessments, with detailed discussions of some of the more noteworthy projects.
Major Observations
The panel presents the following major observations from its assessment of the Chemical Science
and Technology Laboratory:
· CSTL's research and standards programs are technically excellent overall, with many considered
to be world-class by the scientific and technical community in general and by international standards
Chemical Science
and Technology
Laboratory
1 1 1
Biotechnology
Division
· DNA
Technologies
· Bioprocess
Engineering
· Biomolecular
Materials
· Structural
Biology
Process
Measurements
Division
· Fluid Flow
· Fluid Science
· Process
Sensing
Thermometry
Pressure and
Vacuum
· Thermal and
Reactive
Processes
Surface and
Microanalysis
Science Division
· Microanaly-
sis Research
· Surface and
Interface
Research
· Analytical
Microscopy
Physical and
Chemical
Properties Division
· Computational
Chemistry
· Experimental
Kinetics and
Thermo-
dynamics
· Chemical
Reference Data
and Modeling
· Experimental
Properties of
Fluids
(Boulder)
· Theory and
Modeling of
Fluids
(Boulder)
· Cryogenic
Technologies
(Boulder)
.
Analytical
Chemistry
Division
· Spectro-
chemical
Methods
Organic
Analytical
Methods
· Gas
Metrology
and Classical
Methods
· Molecular
Spectrometry
and
Microfluidic
Methods
· Nuclear
Methods
FIGURE 4.1 Organizational structures of the Chemical Science and Technology Laboratory. Listed under each
division are its division's groups.
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AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003
organizations in particular. The laboratory's outstanding performance in the Key Comparisons of Na-
tional Metrology Institutes (NMIs) conducted under the auspices of the CIPM (Comite International des
Poids et Mesures) is a particularly fine example of CSTL's capabilities.
· CSTL has clearly demonstrated both the relevance and effectiveness of its programs to its cus-
tomers, primarily U.S. industry, government, and academia, but also to international science, technol-
ogy, and commerce. Evidence of the impact of its work includes customer feedback from symposia and
workshops, formal economic impact studies, and documented leadership in the international standards
community.
· Even during an extended period of flat budgets, the laboratory's innovative practices and suc-
cessful partnering have sustained exceptional productivity and the continuation of its high visibility,
recognition, and world leadership in the development of measurement standards. In particular, the panel
cites significant advances in the clinical in vitro diagnostics (IVD) and NIST-Traceable Reference
Materials (NTRM) programs. Having commercial facilities produce NIST-traceable gas standards is an
excellent example of creative leveraging of CSTL's efforts.
· CSTL has implemented an excellent strategic planning process that is closely aligned with the
goals and objectives of the overall NIST strategic plan (the NIST 2010 plan) and that has enabled it to
effectively anticipate future customer needs. Linking the annual operating plan tightly and transparently
to the strategic plan has been an excellent management decision that allows the laboratory to effectively
plan its ongoing programs while responding to unanticipated needs and opportunities.
· The panel encourages the development of a coherent plan for responding to the explosive growth
of onnortunities for the Biotechnolo~v Division. In particular. it is not clear that there currently exists
~ ~ ~7, ~ , ,
1 · 1 ,. · ,1 1 · 1 · 1 · , · 1 1 , ,1 1 1 , r
enough In-house expertise In the biological sciences to guide and support the development ot programs
in this field.
· Standard Reference Material (SRM) productivity could be enhanced by building stronger in-
house collaborations.
· The Analytical Chemistry Division continues to be central to the laboratory's standards develop-
ment. The panel is concerned, however, that declining support for personnel and equipment will ulti-
mately erode both quality and productivity and encourages the laboratory to develop a plan to ensure the
successful continuation of the important work conducted by this group.
· CSTL has made great progress in Web site design and information dissemination; as indicated in
last year' s report, however, there remain lapses in data updates that detract from the utility and value of
these sites. Also, the panel recommends that over the course of the next year the laboratory develop
common entry points for all of the chemical information available on its site, perhaps using a search
engine format similar to that of the Chemical Abstract Services Syfinder.
· While the panel is encouraged with the small increase in laboratory funding over the past year, it
is concerned that proposed federal reductions in Advanced Technology Program funding will require
nontrivial repositioning of the laboratory programs. CSTL should address this issue explicitly in its
strategic and operational planning processes.
Technical Merit
The technical merit and quality of CSTL's work continue to be excellent, in many cases world-class.
Its performance in the CIPM Key Comparisons is probably the finest single example of its stature in the
national measurements community. The panel also wishes to draw attention to several other examples
that illustrate the outstanding, ongoing quality and technical merit of CSTL projects, including these:
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CHEMICAL SCIENCE AND TECHNOLOGY LABORATORY
IVD;
39
· Significant advances in clinical markers technologies and the completion of several SRMs for
· Significant advances in the rigorous validation of biomarkers for health diagnostics;
· Significant advances in the research on properties and equation-of-state of fluid mixtures near the
critical point, and the release of an updated version of the NIST database REFPROP (alternative
refrigerants);
· Development of the extensible markup language (XML) data format for spectroscopic hyperdata.
This general data format enables very impressive methods for spectral data storage and analysis and is
destined to become a nationally accepted standard format;
· Demonstration of a 10,000-fold improvement in the sensitivity of microfluidic sensors;
· A major update of the NIST Mass Spectral Database, which is among NIST's most widely
disseminated Standard Reference Databases (SRDs); and
· Successful completion of a Johnson Noise Thermometer prototype and documentation of a noise-
to-power accuracy ratio of better than 0.1 percent over the range considered. The panel views the ability
to recalibrate these sensors remotely for example, for space station applications as very significant.
Program Relevance and Effectiveness
CSTL continues excellent practices to ensure that its technical programs are relevant to the needs of
its customers. Various mechanisms are used to gather outside input on current or planned activities;
these include participation in standards committee meetings, technical conferences, benchmarking and
roadmapping activities, professional society meetings and committees, and trade organization events.
Staff members take lead roles in organizing these gatherings and often hold them at NIST. Researchers
maintain informative relationships with a large number and wide variety of guest researchers and
collaborators in industry and at universities to support and leverage their work.
Overall, the programs of CSTL have a strong impact on a wide array of industries and research
communities. CSTL' s contributions often provide critical bridges between research directed toward the
short-range goals of industry and the long-range, open-ended inquiries pursued in universities. Particu-
larly noteworthy for their relevance and effectiveness are the laboratory's efforts in SRMs, SRDs, and
international standards activities. These services and activities rarely garner headlines, but they under-
pin many critical measurements in the chemical, pharmaceutical, medical, and other industries and are
therefore very highly leveraged investments. Finally, CSTL responded quickly and decisively to recent
national crises and is actively assessing its current capabilities and planning for possible future contribu-
tions to the national homeland security effort. The panel wishes to highlight the following programs for
their significant impact:
· Widely recognized leadership in the development of clinical standards and diagnostic devices,
ensuring continued U.S. dominance in an area fostering more affordable health care at home and abroad.
New methods developed by CSTL for the amplification and automated detection of DNA fragments
served a critical need in the identification of victims of the World Trade Center disaster. This technology
could be the basis of a multitude of applications existing in the military and supporting homeland
security requirements.
· The frequency of visits to the NIST Chemistry WebBook site (an increase of 43 percent in 2002)
and the inclusion of databases in commercial instrument packages. Roughly one-half of all gas chroma-
tography/mass spectrometry instruments sold worldwide include the CSTL Mass Spectral Database,
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AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003
enabling the application of these techniques to problems that span nearly every area of science and
technology.
· The pursuit of DNA diagnostics for the detection of human disease in the NISTINational Cancer
Institute (NCI) Biomarker Validation Laboratory. This NIST component of the NCI Early Detection
Research Network (EDRN) serves to refine recently discovered cancer biomarkers and to format new
research tests for field trials in EDRN clinical laboratories. Significant advances are now being made in
the areas of breast and prostate cancer and in the identification of clinical markers for radiation damage
and processes involved in aging.
· The development of an XML data format for spectroscopic hyperdata in the transmission electron
microscope (TEM) laboratory is extremely important work. This general data format supports very
powerful methods of spectral data storage and analysis and is destined to become a nationally accepted
standard format. These data are critically important in almost every area of science, technology, and
manufacturing.
· Developments in microheater sensors have reduced detection limits to as low as 20 to 200 ppb for
satin; these sensors can also detect mustard gas and GA-tabun with a response time of approximately 50
seconds. A new, monolithic preconcentrator may further increase sensitivity by an additional factor of
10. Carbon nanotubes have been grown on MEMS micro-ho/plates, enabling the evaluation of their
performance as gas sensors. This project is relevant to both homeland security and Chemical Weapons
Convention defense technologies.
Laboratory Responsiveness
CSTL provided a detailed, written, point-by-point response to the observations and recommenda-
tions made in the FY 2002 assessment. The panel is, in general, quite satisfied with the laboratory's
response. Many recommendations were implemented, and thoughtful replies were provided in cases in
which management either could not implement a suggested change (usually for resource or NIST-wide
structural reasons) or chose a different solution based on its own programmatic priorities and resources.
A few examples of the kinds of laboratory responses include the following:
· Determined efforts to bring all calibration programs into compliance with ISO/IEC 17025 have
resulted in significant progress and already rate highly in the eyes of calibration service customers. It
would be especially beneficial for NIST to publish its ISO-compliant quality manual and other relevant
quality documents on the Web. Commercial and government calibration and testing laboratories could
use such documents for a variety of purposes, including use as guides and templates for their own
documents.
· The panel is pleased to note that the laboratory has started to address the issue of management
training for group leaders; this is an important issue, given the broad range of responsibilities now
assigned to group leaders and the general lack of training in these areas in the careers of scientists and
engineers.
· The panel was pleased to see the reorganization of the effort in atmospheric chemistry in the
Surface and Microanalysis Science Division in response to repeated suggestions by the panel over
several years.
· Some responses to the FY 2002 recommendations were not as strong as those noted above. For
example, progress in providing timely Web updates and more interactive site designs continues to be
slow. The dissemination of new knowledge and data generated by the laboratory is critical to its
continued success and utility; now that the Web is the dominant point of contact between NIST and its
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CHEMICAL SCIENCE AND TECHNOLOGY LABORATORY
41
customers, it is imperative that the Web site be an efficient and easy-to-use interface. If resource
limitations at the laboratory level are indeed the constraint to more rapid progress, the panel urges
management to work collaboratively with the directors of the other laboratories and with the NIST
Director's Office to address this NIST-wide issue of great importance.
Laboratory Resources
Funding sources for the Chemical Science and Technology Laboratory are shown in Table 4.1. In
January 2003, staffing for the laboratory included 271 full-time permanent positions, of which 234 were
for technical professionals. There were also 81 nonpermanent or supplemental personnel, such as
postdoctoral research associates and temporary or part-time workers.
Although there is a small increase in CSTL funding for FY 2003, mandatory salary increases will
translate once more into an essentially flat budget. Within this environment, hard choices have had to be
made, involving trade-offs between personnel and laboratory equipment. The loss of five professional
staff in one division during 2002 has heightened the panel's concern over the trend in reduction of full-
time-equivalent personnel. As in the previous assessment, the panel observed too many priority projects
with subcritical resources devoted to them. Given that an era of flat budgets has taken hold, the panel
strongly advises the laboratory to take a hard look at its priorities and examine areas in which potential
TABLE 4.1 Sources of Funding for the Chemical Science and Technology Laboratory (in millions of
dollars), FY 2000 to FY 2003
Fiscal Year Fiscal Year Fiscal Year Fiscal Year
2000 2001 2002 2003
Source of Funding (actual) (actual) (actual) (July 2003 estimate)
NIST-STRS, excluding Competence 37.7 36.9 38.3 45.1
Competence 2.4 1.9 2.7 2.7
ATP 3.3 3.2 2.5 2.1
Measurement Services (SRM production) 2.2 1.9 2.6 2.2
OA/NFG/CRADA 14.2 14.3 12.4 10.7
Other Reimbursable 3.4 5.8 6.1 6.3
Total 63.2 64.0 64.6 69.1
Full-time permanent staff (totally 275 264 273 271
NOTE: Funding for the NIST Measurement and Standards Laboratories comes from a variety of sources. The laboratories
receive appropriations from Congress, known as Scientific and Technical Research and Services (STRS) funding. Compe-
tence funding also comes from NIST's congressional appropriations but is allocated by the NIST director's of lice in multiyear
grants for projects that advance NIST's capabilities in new and emerging areas of measurement science. Advanced Technol-
ogy Program (ATP) funding reflects support from NIST's ATP for work done at the NIST laboratories in collaboration with or
in support of ATP projects. Funding to support production of Standard Reference Materials (SRMs) is tied to the use of such
products and is classified as "Measurement Services." NIST laboratories also receive funding through grants or contracts from
other [government] agencies (OA), from nonfederal government (NFG) agencies, and from industry in the form of cooperative
research and development agreements (CRADAs). All other laboratory funding, including that for Calibration Services, is
grouped under "Other Reimbursable."
aThe number of full-time permanent staff is as of January of that fiscal year.
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AN ASSESSMENT OF THE NIST MEASUREMENT AND STANDARDS LABORATORIES: FY 2003
in-house funding resources may exist. One area suggested is charges for database use. Such an activity
would require backing from comprehensive evaluations of cost and usage issues. Another area sug-
gested for examination is optimization of professional-to-support staff ratios. Also in the line of re-
strained budgets, the laboratory director should exert even greater effort to keep researchers informed of
pending programmatic realignments and perhaps even to invite their input as decisions are being made.
This would not only serve to increase morale but would also be a resource for new ideas based on the
experiences of the staff.
Facilities and instrumental infrastructure in CSTL are very good overall. Updates in the elevators
and exhaust hoods in some buildings have improved the working environment. The panel was pleased to
hear that some funding has at last become available to begin repairs on the Boulder facility. Two
important pieces of equipment, the electron microprobe and the Auger spectrometer, remain in need of
attention to be brought online. It is still not clear when the CSTL equipment will be moved to AML.
Representative terms from entire chapter:
technology laboratory
