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2 Analytical Chemistry Division OVERVIEW The activities of the Analytical Chemistry Division (ACD) of the Chemical Science and Technology Laboratory are focused primarily in two areas―fundamental chemical metrology and the development of measurement methods and standards, including the following: clinical diagnostics and health status markers, environmental monitoring, food dietary supplements and nutritional assessment, industrial commodities and advanced materials characterization, forensics and homeland security, nanoparticle characterization, and the hydrogen economy. The division maintains core expertise in analytical mass spectrometry, analytical separation science, atomic and x-ray fluorescence spectrometry, gas metrology, nuclear analytical methods, nuclear magnetic resonance (NMR) spectrometry, and classical and electroanalytical chemistry. The core expertise resides in four groups or teams (Organic Chemical Metrology Group, Inorganic Chemical Metrology Group, Gas Metrology Group, and Environmental Specimen Bank/NMR Team) and provides the capability for carrying out the division’s broad mission with flexibility so that it can respond to changing and evolving national priorities. The Environmental Specimen Bank/NMR Team is located at the Hollings Marine Laboratory (HML) in Charleston, South Carolina, which is a partnership with the National Oceanic and Atmospheric Administration (NOAA), the South Carolina Department of Natural Resources, the Medical University of South Carolina, and the College of Charleston. The total FY 2008 ACD funding was $21.82 million, of which $4.23 million (19 percent) was other-agency funding and $5.29 million (24 percent) was from standard reference materials (SRMs). As of March 2009, total funding was $21.29 million (including $0.39 million pending), of which $3.89 million (including $0.23 million pending), or 18 percent, was other-agency funding and $4.22 million (20 percent) was from SMRs. The division staffing level is approximately 90 NIST full-time equivalents (FTEs) and 15 visiting scientists and graduate students. The ACD has been meeting its obligations, and its priorities are appropriate. The technical commitment of the staff is high, and the availability of equipment and facilities is generally of a high order. The strong tradition of quantitative measurements within the ACD is very important work that helps many federal and state agencies achieve their goals. Examples include the division’s support of the Consumer Product Safety Improvement Act of 2008 (Public Law 110-314), which addressed the need to detect lead (Pb) in paint on children’s toys; its assistance to the Environmental Protection Agency (EPA) in its mission to regulate mercury (Hg) in emissions from coal-powered-electricity generation; and its development of standards for the Office of Dietary Supplements in the National Institutes of Health (NIH). 5

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RESPONSE TO RECOMMENDATIONS FROM THE PREVIOUS REPORT One of the concerns expressed by the Panel on Chemical Science and Technology during its 2007 review1 centered on the general balance between service work and methods research. The concern is now formulated more precisely, as follows: the development of standard reference materials (SRMs) is a key component of the work of the ACD, and balance is needed between developing SRMs and establishing new analysis methods. The division does an excellent job of developing assays for the quantitative analysis of target analytes in a broad range of matrices—an area in which it excels. However, the panel raised concerns during its 2007 review about a shortage of staff in aerosol science and electrochemistry (listed among the ACD’s areas of core expertise), and those concerns remain unaddressed, as noted elsewhere in this chapter. TECHNICAL MERIT In 2007, division researchers produced 57 publications and gave 163 talks (64 invited). In 2008, division researchers produced 66 publications and gave 162 talks (71 invited). For 2007–March 2009, 8 external awards and 7 internal awards were given to ACD staff. Projects Within the Organic Chemical Metrology Group The Organic Chemical Metrology Group has a long history of excellence in quantitative measurements, particularly in separations. The group has diversified more recently into proteomics, NMR, and other techniques and is applying these techniques to important areas, such as nutritional analysis and marine environmental samples. Standards for conducting quantitative measurements of proteins are not well developed across the community, and the work being done by this project is both timely and important. The linkage of the project with leading proteomics projects through the National Cancer Institute (NCI) Clinical Proteomics Technology Assessment for Cancer (CPTAC) collaboration is especially valuable and connects the ACD staff with strong researchers in the field. Given the number of laboratories now engaged in proteomics, many of which do not have resident mass spectrometry experts, having standards for assessing the operation of the instrument and quality of the results is very important. These results are also being published in significant journals by members of the group as coauthors. However, this group should be leading publications in this area. Furthermore, it should consider the addition of a protein mass spectrometrist and a high-performance mass spectrometer to support its continuing work in proteomics and metabolomics. This group reported that it is expressing its own labeled proteins; it may want to consider working with other projects that do this on a large scale (e.g., structural biology projects), and it would have the infrastructure to do this. The metabolomics work, like the proteomics work, is very important; this project has been using multiple approaches to develop techniques and evaluate standards. 1 National Research Council, An Assessment of the National Institute of Standards and Technology Chemical Science and Technology Laboratory: Fiscal Year 2007. Washington, D.C.: The National Academies Press, 2007. 6

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The Analytical Chemistry Division is well known for its fundamental studies on shape recognition using reversed-phase chromatography. Strong progress on these efforts continues, with detailed molecular modeling studies on the three-dimensional structural attributes of these stationary phases. Based on this work and on its recent study on the solvation of perfluorinated octane, the division is now examining new stationary phases that utilize perfluoro functionalities; this should allow even greater molecular recognition. The work on establishing standards for nutritional analysis has very high importance, and it provides good support for other federal agencies and in the arena of public health. A large number of SRMs have been developed—a need that will grow in the future. In addition to standards for nutritional supplement labeling, standards are being established for botanical supplements. This area is also growing quickly, and reliable methods for analyzing these supplements are very important. The development of techniques for the analysis of contaminants in human biofluids builds on long-standing expertise in understanding the impact of matrices on various assays. The forensics and homeland security project, which interacts closely with the Department of Homeland Security (DHS) on the development of SRMs for the analysis of explosives, is one of several such efforts at NIST. The project has developed trace-explosive SRMs for use in portable instruments that are a vast improvement on the use of standards provided by manufacturers. The forensics and homeland security project has also begun to develop metrology and standards for canine detection of trace explosives. It was unclear whether the ACD group’s project has developed sufficient interactions with other groups outside of NIST with relevant experience. For example, the ACD will need to develop increased interaction with a larger project of forensics researchers if it is to optimize its participation in any NIST-wide response to the recent National Research Council report on forensics science.2 Projects Within the Inorganic Chemical Metrology Group The Inorganic Chemical Metrology Group (ICMG) shows excellence in a range of analysis techniques, including inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma optical emission spectrometry (ICP-OES), neutron imaging, and x-ray fluorescence (XRF) spectrometry. The neutron imaging activities are aimed at achieving high-resolution (submicron) imaging. Neutron imaging has the potential to provide a quantum leap for materials research in fuel cell dynamics and hydrogen storage; for biological research, such as in nanomedicine; and for environmental research, including that on global warming. Major accomplishments of this innovative group include the development of new neutron converter prototypes and interesting designs of radiography components. A very important ICMG study examines tissue-banked samples of seabird eggs from different locations in and around Alaska. An important set of new high-precision isotopic reference materials (RMs) containing multiple elements is being developed. Four new isotopic RMs containing Hg, Pb, thallium (Tl), and germanium (Ge) are planned for 2009- 2010 that will provide an important high-precision reference material for the community. This work was enabled by the acquisition of an inductively coupled plasma multicollector mass spectrometer with precision of a few parts in 106. 2 National Research Council, Strengthening Forensic Science in the United States: A Path Forward. Washington, D.C.: The National Academies Press, 2009. 7

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Quantification of deoxyribonucleic acid (DNA) at the trace and ultratrace levels is of increasing importance in bioanalysis connected to applications such as nanoparticle drug delivery and disease monitoring. The ICMG is using ICP-OES to monitor the phosphorus emission signal from DNA. Plans to move to high-resolution ICP-MS from this project are a productive extension of this research project. Handheld XRF devices have been manufactured to determine whether lead is present in the paint on imported toys. SRMs are needed to support these screening assays for low levels of lead. ICMG staff are developing new SRMs for this purpose and are benchmarking the new handheld instruments to determine if they can actually meet the performance standards of the Consumer Product Improvement Act of 2008. This group has also developed a number of new standard reference materials since the panel’s 2007 review. Those of significant interest include the newly collected soil sample polluted with 500 parts per million (ppm) hexavalent chromium, the renewal of the San Joaquin soil, and urban dust. The use of nanoparticles in medical and other applications continues to increase, and the ICMG has been working to establish capabilities for analyzing nanomaterials such as gadolinium-based magnetic resonance imaging (MRI) contrast agents, carbon nanotubes, and gold (Au) nanoparticles. One study on separating free and ligated-gadolinium-based MRI contrast agents is an important effort. However, this effort may not be at the leading edge of this technology, and more interaction with leaders in this area would be valuable to the project. The project on the development of a carbon nanotube SRM in collaboration with national laboratories in Canada demonstrated good scientific rigor. Ultimately, the impact of this standard will require the NCI and other health regulatory bodies to adopt it as a standard for carbon nanotube toxicity tests. The work on ICP-MS of Au nanoparticles and argon (Ar) gas electrospray ionization explores important scientific issues and is interesting; nevertheless, this work might benefit from interaction with a broader array of outside experts in these areas. Inorganic electrochemistry is a capability that is missing in this group. Because this area is central to both the hydrogen economy and growing research and development activity in battery technologies, there is a clear need to hire a new PhD-level electrochemist, as was noted in the panel’s 2007 review. Projects Within the Gas Metrology Group The Gas Metrology Group is fulfilling the current standardization needs of several industrial and federal regulatory communities. It provides gas standards that will be required for monitoring all of the established greenhouse gases. This group is also well prepared to move into the realm of gases likely to come under regulation in future years, such as the halocarbons. The project effectively plays a central role among the national metrology institutes (NMIs) on various aspects of monitoring global warming gases. The project is also preparing the laboratory and SRM infrastructure needed for the hydrogen economy. The Gas Metrology Group’s close interaction with the Environmental Protection Agency and instrument manufacturers will soon complete scientifically sound and legally defensible protocols for monitoring Hg emissions from coal-fired electricity generation plants. These efforts have been critical to the Mercury Demonstration Project and the EPA’s mandate to regulate Hg emission from coal combustion, which constitutes a major national 8

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environmental problem as the dominant anthropogenic source of environmental Hg contamination. Related standards projects support important international atmospheric monitoring activities such as the World Metrology Organization’s Global Atmosphere Watch Program. For example, the NIST Standard Reference Photometer is critical to ozone measurement traceability. The addition of two permanent BSc-level scientists to this unit since 2007 has improved the ability to support the activities of the Gas Metrology Group. However, there remain two significant, looming shortcomings in this group. The first is one of succession— the project has not yet recruited any new PhD-level permanent staff scientists needed to ensure continuity in this project in the coming decades. This short-staffing could quickly become dire if cap-and-trade schemes for controlling global warming gas emissions are mandated nationally. The second shortcoming is the absence of expertise in the area of atmospheric aerosols, which arguably account for the largest uncertainty in models of global warming and are the subject of increasing activity by the scientific community. As opportunities in this area quickly develop, the ACD should strategically evaluate the direction of this group and the recruiting strategies required to ensure the group’s future success. For example, the division should consider adding scientists experienced in aerosol mass spectrometry and high-resolution gas phase spectroscopy, among other areas. SUMMARY The Analytical Chemistry Division continues its high-impact contributions in key areas of importance to industry, federal agencies, and researchers across the nation and around the world. The staff’s work is well aligned with NIST’s core missions. Over the years, the ACD has evolved from instrumentation research to focusing more on establishing standards and analytical methodologies. This is a reflection of the field in analytical chemistry in general. The division must continue to implement and evaluate state-of-the-art technology in analytical chemistry. It also needs to maintain awareness of new developments in the field so that it can adapt quickly to new techniques as well as develop them in-house. The ACD has been reaching out to collaborate with many research groups, both inside and outside NIST. With its valuable expertise, the ACD should take action to be leading more of these collaborations. Cutting-edge work with potentially high impact is highly evident within the ACD, including the neutron imaging work and the Hg isotope ratio work on marine tissue. The division is doing an excellent job of generating standards and trace analysis methodologies using commercial instrumentation, which is congruent with its mission. In a few areas, the methods being used may not be leading-edge. The ACD has highly recognized strengths, yet it must be careful that over the long term it does not evolve to having primary expertise in its currently strong areas of separation science and inorganic analysis. Maintaining new perspectives is critical for the division’s future. ACD management should reinforce hiring practices that bring in new people with new perspectives, including perspectives that result from training in other organizations. Having the division’s young environmental scientist from Charleston, South Carolina, receive further training in France is a good example of broadening perspectives by bringing in people with multidisciplinary backgrounds. 9

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An important aspect of this division’s output is its reporting of results to the scientific community. At present, the rate is about one publication per scientific FTE. It is recommended that the ACD work with its staff to increase its publication rate, with more publications in high-impact journals such as Analytical Chemistry, Nature Methods, and others, where the work of the division would be read by a broader audience of the analytical chemistry community. In addition, more attention should be given to having ACD staff become more visible in the scientific community. 10