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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).
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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.
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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.
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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
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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.
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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.
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