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An Assessment of the National Institute of Standards and Technology Chemical Science and Technology Laboratory: Fiscal Year 2007 Analytical Chemistry Division SUMMARY The Analytical Chemistry Division (ACD) has been meeting its obligations, and its priorities are appropriate. The technical merit of the division, the commitment of the staff, and availability of equipment and facilities are of a high order. Future assessments will be facilitated if the ACD presentations to the NRC panel place greater emphasis on separating service activities from development and research activities and if the status of and progress on projects are clearly reported. ADDRESSING NATIONAL PRIORITIES The ACD is involved in new NIST-level programs on standards and methods to address the challenges of the hydrogen economy, climate change, nanotechnology, biofuels, and medical diagnosis. These challenges provide a framework for development of improved metrical methods, standards, and materials. The issues involved in new and renewable energy, environmental stewardship and measurement accuracy, and improvements in health and medical research are important national priorities. The Inorganic Chemical Metrology Group is addressing biology as metal-protein complexes (metallomics); the biogeochemical cycling of sulfur and the formation of sulfate (SO42−) aerosol particles in the atmosphere; the oxidation states of arsenic; organometallic species in marine tissue standard reference materials (SRMs); sulfur at levels of less than a microgram per gram in diesel and gasoline SRMs; and the measurement of small quantities of fissionable nuclides such as 235U and 239Pu. Such projects are in response to requests from outside agencies as well as industrial consortia. The mission of the Organic Chemical Metrology Group includes the development, critical evaluation, and application of methods for the identification and measurement of organic and organometallic species using analytical separation techniques and mass spectrometry. This mission is addressed by the measurement of organic compounds in support of the development of SRMs, quality assurance programs, and other agency activities in clinical, food and nutritional, environmental, forensic, and homeland security areas. This work is in alignment with essential national priorities. The addition of work that addresses nanotechnology would also be aligned with national priorities. The Gas Metrology Group has focused on dynamic dilution for reducing uncertainties in gas standards; global climate studies; a volatile organic compound standard for environmental and hazard monitoring; the development of reference materials based on input from organizations such as the AIGER (Automobile Industry/Government Emissions Research) consortium; and the development of standards and methods to determine and monitor the concentration of ozone in the atmosphere. These projects reflect input from industry and industrial consortia that need high standards for purity and effective methods related to gas and emissions monitoring. The group must prepare itself to play a critical metrology role in any carbon emissions trading system that may be implemented to address global climate change.
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An Assessment of the National Institute of Standards and Technology Chemical Science and Technology Laboratory: Fiscal Year 2007 For over two decades, the ACD has been involved in the banking of environmental specimens and analytical programs to ensure marine quality; these activities are collaborative efforts supported by NIST resources and funding from other federal agencies. The division currently maintains environmental specimen banks at two locations: the National Biomonitoring Specimen Bank at the NIST Center for Neutron Research in Gaithersburg, Maryland, and the Marine Environmental Specimen Bank at the Hollings Marine Laboratory (HML) in Charleston, South Carolina. The banks support important work in medicine and marine chemistry and biology. NIST is the lead agency for metrology in nanotechnology. The accurate and comprehensive assessment of the risks to health and the environment posed by nanoparticles and nano devices is important. ACD staff typically develop methodologies by using and evaluating commercial instrumentation. This is a reasonable approach that gives their work direct impact across the ACD constituent communities. However, the ACD should be more involved in advancing technology to improve environmental monitoring, homeland security, forensic investigation, and clinical diagnosis. As the premiere analytical agency in the United States, it could play a more central role in developing new measurement techniques and in advancing the science of metrology into the biological and nanotechnology areas. Such fundamental studies will, however, require additional funding and should not be done at the expense of the ACD’s current work on developing standards and methods. IMPACT AND INNOVATION ACD supports the mission of the CSTL by adhering to the vision it states as follows: To be recognized as the nation’s reference laboratory for chemical measurements, providing traceability through measurement technology, reference materials, reference data, and other measurement services required to meet science and technology needs. This vision is being realized through a strategy to conduct research on the qualitative and quantitative determination of chemical composition; develop and maintain state-of-the-art chemical analysis capabilities; disseminate tools for measurement traceability and quality assurance (such as reference materials, reference data, and other services); and demonstrate comparability of U.S. standards for chemical measurement with those of other national metrology institutes. These core competencies allow the ACD to carry out its broad mission and give it the flexibility to respond to changing and evolving national priorities. In 2007 these competencies reside in three main groups: the Inorganic Chemical Metrology Group, the Organic Chemical Metrology Group, and the Gas Metrology Group. The organization was recently restructured to improve efficiencies and manage specific activities through multidisciplinary teams better able to address the changing landscape of analytical sciences. The three primary groups collaborate in a number of high-priority program areas, including reference measurement methods and standards for environmental quality; clinical diagnostics; food, dietary supplements, and nutritional assessment; forensics and
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An Assessment of the National Institute of Standards and Technology Chemical Science and Technology Laboratory: Fiscal Year 2007 homeland security; commodities characterization; and advanced materials characterization. Internationally recognized reference methods support the division’s infrastructure for providing traceability for the chemical measurements used in programs of national and international importance through SRMs, NIST traceable reference materials, measurement quality assurance programs in critical areas, and comparisons of NIST chemical measurement capabilities and standards with those of other national metrology institutes. The technical merit of scientists within ACD has been acknowledged in a number of different ways. During 2006, research in the division resulted in 60 peer-reviewed publications with an additional 28 manuscripts in press, down from an average of 106 publications per year over the preceding 4 years. In addition, staff gave 137 scientific technical talks, which is also fewer than the 196 talks in 2005. The status of the division with respect to other metrology communities at home and abroad is demonstrated by staff participation in 127 scientific committee assignments, up from 100 in 2005, and at the average of 128 over the preceding 4-year period. In the area of fuel cell imaging technology, an exploratory research project has led to the conception and design of a new neutron-radiation-based imaging system that, when implemented, will allow the observation of the chemical actions in a fuel cell or across single biological cells. Applications such as biological cell imaging then become possible with this high resolution, as well as the ability to map the flow characteristics of hydrogen species across the proton exchange barrier of a hydrogen fuel cell. The development of SRMs for use in the biofuel industry should receive continued support, given the explosion of industrial activity in biofuels over the last year. The electrochemistry activity is now down to one person. This calls into question the future viability of this program, and ACD must consider the intellectual losses that would result from the disappearance of this group. In the area of nanoscience metrology, the collaboration with the National Cancer Institute and the Nanotechnology Characterization Laboratory (NCI/NCL) creates a natural link, especially given the topics—for example, gadolinium (Gd) and quantum dots. NIST is an ideal partner for NCI in this work. Gd and quantum dots have significant implications for many industries. Projects at the HML continue to be relevant, effective, and impressive in quality. The work on contamination of waterways by flame retardants and on illicit and prescription drugs is worthwhile and appears to be progressing in a satisfactory manner. Dietary supplements are an expanding field being explored by numerous agencies and governments. International collaboration is essential to prevent duplication of effort. The list of compounds being investigated by the division was proposed by the National Institutes of Health and the Food and Drug Administration. Given the wide diversity of both domestic and imported compounds and the multi-billion-dollar industry they support, this work could result in new mandated SRMs for controlling imports. Work on the detection of trace explosives was very impressive. Given the current relevance and rapid growth of homeland security efforts, this and related work deserves even greater emphasis. To the extent possible, ACD should position itself as the leading metrology group for new methods of analysis applicable to homeland security.
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An Assessment of the National Institute of Standards and Technology Chemical Science and Technology Laboratory: Fiscal Year 2007 In the area of proteomics and biomarker standards, health status markers have been identified as having high priority for immediate studies. Because protein biomarkers occur naturally with considerable heterogeneity (i.e., with glycosylation, acetylation, phosphorylation), the group has developed liquid chromatography and mass spectrometry techniques for chemical characterization of the target species, particularly the protein-based markers such as troponin I and prostate-specific antigen. This work is critical to continued biotechnology efforts. TECHNICAL MERIT Overall the technical merit of the division is excellent. Increased effort could be expended in developing analytical technology as well as methods and SRMs. Research in new technologies to advance the analytical sciences in any particular field seems to be left somewhat up to the individual group leaders and their views on how assertively to investigate such new measurement technologies. If the group leader exhibits leadership and is motivated to move an analytical technique forward, then that technique is included in the group’s activities. The technical merit of the Inorganic Chemical Metrology Group projects is, overall, very good to excellent. The emphasis on isotopic metrology for elemental isotopic measurements is highly appropriate. This is in many ways a breakthrough project leading to improvements in fundamental understanding of geological eras and origins of Earth and the planets. It enables improved understanding of biological processes such as kinetics and life cycles. The work on sulfur in diesel fuel is good, and the work on arsenic in drinking water is first rate and will result in additional reductions in detection limits and increased identification of specific arsenic species. The work associated with the various programs and projects in mass spectrometry, x-ray fluorescence, optical spectrometry, and sample preparation is proceeding well and underpins the productive role of this group in creating, developing, and maintaining the SRMs that constitute nearly three-fourths of ACD’s products. The Organic Chemical Metrology Group is developing standards and methods to determine the levels of specific proteins and other biomolecules in blood as indicators of certain disease states. This effort is largely motivated by proteomic biomarker discovery research supported in part by the NCI. There is currently enormous government and industry investment in developing protein biomarkers for specific disease states, and the results of this ACD group have shown a dramatic need for improved metrology. Needed to establish a quality assurance infrastructure for protein biomarker measurements are reference materials of known composition and stability; reference measurement procedures; and reference data libraries. Efforts are under way at ACD in each of these areas to establish measurement traceability and reliability. The group’s research activities in separation science continue to investigate the physical and chemical processes that influence retention in liquid chromatography, gas chromatography, supercritical fluid chromatography, capillary electrophoresis, and capillary electrochromatography. Results from these fundamental studies are used to design stationary phases tailored to solve specific separation and analysis problems and to assist in method development and optimization. Additionally, during the past 2 years, the
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An Assessment of the National Institute of Standards and Technology Chemical Science and Technology Laboratory: Fiscal Year 2007 group has measured a number of SRMs of importance to the clinical, environmental, and food and nutritional communities. The metrology sciences applied by the Gas Metrology Group are state of the art for this industry and have generally served as a benchmark for other domestic standards and gas measurements. The group has been conducting important projects in dynamic dilution, reference standards for the automotive industry, and ozone measurements. The balance between services work and advanced technology or methods research is the key distinguishing characteristic of the programs of this division. The programs having a high service load relative to SRMs and international comparisons do not have the resources of time or personnel to pursue cutting-edge or proactive research. This disturbing aspect of the project planning process greatly reduces opportunities to perform the research necessary to address future—as opposed to present—customer needs. The scientific expertise within NIST is a national resource that should be valued highly. The scientists must have enough time to incorporate cutting-edge research into their portfolio. A number of programs have indeed been successful in obtaining extramural funds and are fulfilling the vision and mission of NIST—that is, meeting future challenges. INFRASTRUCTURE The division employs approximately 88 scientists, technicians, and administrative/clerical support staff. It has an annual budget of about $21 million, about $5 million of which supports programs of other federal and state government agencies and/or American industry on a cost-reimbursable basis. The division recently experienced a reduction in full-time positions. Over the last 4 years there has been a steady decrease in personnel, specifically in the permanent lines. Eleven permanent professionals were lost from this division mostly owing to their transfer to the Biochemical Science Division. Reductions in scientific personnel have particularly profound consequences in this division because its SRM program and international activities result in a very high service load, and it is tasked with a leadership role in nanotechnology as well as support roles in homeland security, global climate change studies, and the new hydrogen economy. In particular, the Gas Metrology Group has been constrained in developing new gas measuring technologies and associated methods because it does not have enough Ph.D. staff. Recent research in organic chemical metrology within the division has focused on techniques for characterization and quantitative determination of organic compounds, including proteins, in biological matrices. In FY05 and FY06, several new instruments were purchased that significantly increased the division’s capabilities for the determination of trace-level analytes of health, nutritional, forensic, and environmental importance, as well as its ability to characterize proteins and other biomolecules and natural products. The acquisition of an ultra-high-pressure, high-performance liquid chromatograph should be considered soon. This instrument is used routinely in the pharmaceutical industry to achieve improved separation efficiency and faster analysis. Maintaining state-of-the-art core competency requires this addition. New SRMs for both organic nanoparticles and atmospheric aerosols will likely be needed to support the fast growth of nanoscience and nanotechnology and the increasing interest in climate change. The
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An Assessment of the National Institute of Standards and Technology Chemical Science and Technology Laboratory: Fiscal Year 2007 addition of personnel with expertise in the mass spectrometry of environmental aerosols and the characterization of nanoparticles is recommended and is consistent with NIST’s interests. ACD’s interest in nanoparticle characterization logically overlaps with that of other NIST divisions. Reconfiguration of the ACD has brought some improvement, particularly with the integration of the Nuclear Analytical Methods Group and the Inorganic Chemical Metrology Group and the transfer of the microfluidics activity to another division. Also the direct reporting of the HML specimen bank team to the Division Chief is a reasonable change that promotes efficiency. Both the Gas Metrology Group and the electrochemistry program within the Inorganic Chemical Metrology Group are short-staffed by several positions, given current and potential future needs in these areas. ACD has made commendable efforts to combat increased operating costs while still allowing for new projects to be mounted and existing projects to be continued. The increased charges for SRMs have alleviated some problems, and new funding by Congress is predicted to allow most activities to continue. In the face of increasing overheads, the division should critically assess the cost of maintaining such a large inventory of SRMs and determine the consequence of eliminating those in very low demand. CONCLUSIONS Additional Ph.D.-level staff should be recruited to prevent the loss of critical expertise and to allow the NIST knowledge pool to expand into critical areas such as proteomics, environmental aerosol mass spectrometry, and nanoparticle characterization. The potential loss of expertise in the following areas is of concern: gas metrology; electrochemistry; glass mixing, cutting, and polishing with the high precision required for SRMs; and precision machining for SRM quality fixtures. With the high skill levels required in the production quality of SRMs, neglect of these functions could seriously jeopardize future SRM quality or costs of production. These important support services are of vital interest to the entire CSTL. ACD program design and planning are very good. The new cross-divisional planning exercise (addressing program opportunities in nanoscience metrology and in bioscience, including biomarkers and systems biology) conducted at the CSTL has had a positive impact on ACD and should also help ACD to integrate its work with other divisions within and outside CSTL. The mechanisms for determining project priorities and urgencies come from government directives and funding of projects as well as feedback from industry and committee interactions. ACD has not promoted its contributions and accomplishments at a level commensurate with the magnitude of its contributions to the field of analytical chemistry. The result of this underpublicized activity is that industry, academia, and other government laboratories may not be aware of some cutting-edge standards and methods and may be applying antiquated techniques for their own operations. The laboratory should carefully consider the real costs of SRM development and recertifications for specialized industries where only a few SRM samples are purchased. ACD should reconsider its pricing for SRMs where high-profit industries are requesting
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An Assessment of the National Institute of Standards and Technology Chemical Science and Technology Laboratory: Fiscal Year 2007 only a few SRM samples. Indeed, its current SRM pricing structure does not reflect the cost of producing such standards and the supporting infrastructure required to maintain world leadership in standard materials. In such cases, it could impose a surcharge based on actual costs. Specimen banking and marine quality assurance activities should be maintained. These banked specimens might one day be used to address issues of marine environmental quality and ecosystem changes through retrospective analyses and as such constitute a critical national resource. Additional time and effort must be expended in mentoring and guiding the staff of other NMIs not having the skill sets and training of the ACD scientists. The participation of ACD staff in international comparison activities is vital to its own mission and function. Resource constraints could eventually begin to limit these necessary interactions. The constraints include time available to perform comparisons, generate reports, and travel; and staff shortfalls, especially in the Gas Metrology Group. Efforts should be made to reduce the burdensome tasks of SRM maintenance, which is currently performed by the most highly qualified staff. The division should also help to make its scientists more visible in their respective scientific communities. A strong molecular spectroscopy effort should be built within the ACD, because this capability was transferred to the Biochemical Science Division but is still needed within the ACD.
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