United States Environmental Protection Agency	Office of Research and Development

National Exposure Research Laboratory
FY02 Research Abstract

Government Performance Results Act (GPRA) Goal 1
APM23

Significant Research Findings:

Guidelines for the Application of SEM/EDX Analytical
Techniques to Particulate Matter Samples

In July 1997, the U.S. Environmental Protection Agency (EPA) promulgated
a new National Ambient Air Quality Standard (NAAQS) for particulate
matter (PM). The new standard is aimed at regulating ambient concentrations
of PM10 and PM25, particles with aerodynamic diameter <10 fj.m and <2.5
fj.m, respectively. The new NAAQS was developed in response to studies
that showed a significant association between human morbidity and mortality
and PM concentrations. Additional studies indicate that transition metals may
play a significant role in the health consequences of particle exposure. These
studies coupled with the new NAAQS have generated increased interest in
analytical techniques capable of measuring the size, morphology, and
chemical composition of individual aerosol particles. These data are
essential to the understanding of particle formation, transport and transforma-
tion, and deposition mechanisms as well as the impact of particles deposited
in the respiratory system. Furthermore, chemical and physical characteriza-
tion of individual particles can reveal source information that cannot be
determined through bulk chemical characterization such as X-ray fluor-
escence (XRF). Individual particle analysis is thus a complement to bulk
elemental analysis techniques as well as a potentially powerful tool in
source apportionment research.

Research	The National Exposure Research Laboratory (NERL) of the U.S. EPA has

Approach	been developing and evaluating the use of scanning electron microscopy

(SEM) combined with energy-dispersive x-ray analysis (EDX) to
characterize coarse and fine ambient and source-derived particles. With the
SEM/EDX analysis technique, particles can be imaged by SEM, providing
information on the physical properties of particles including size, shape, and
surface morphology, while EDX provides information on the chemistry of
individual particles. SEM/EDX can be conducted both manually and in a
computer-controlled fashion (CCSEM).

Results of this research and development work are presented in an EPA
report entitled "Guidelines for the Application of SEM/EDX Analytical

Scientific
Problem and
Policy Issues

National Exposure Research Laboratory — November 2002


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Techniques to Particulate Matter Samples. The document provides an
introduction to the SEM/EDX techniques, including basic concepts and
hardware, and a description of the NERL SEM/EDX facilities. Procedures
are recommended for sample preparation and analysis. Research related to
SEM/EDX data validity and quality assurance and quality control issues
conducted by the NERL and others is presented, with recommendations
specific to the air particle analysis application. Finally, examples of research
applications are presented.

Results and	The present document, which evolved over several years as a product of

Implications research carried out in support of the U.S. EPA/NERL SEM/EDX

Laboratory, provides guidelines for researchers using SEM/EDX in both a
manual and computer-controlled fashion for aerosol characterization and
source apportionment. The document fulfills the requirements of Annual
Performance Measure (APM) 23, which helps to attain Annual Performance
Goal (APG) 24 under Government Performance Results Act (GPRA) Goal
1.1.8.

APM 23 contributes to GPRA 1.1.8 goal and objectives by 1) providing
techniques to improve understanding of the relationship among PM sources,
ambient concentrations, and human exposure and 2) enhancing receptor
modeling capabilities, thus improving the chances for successful SIP
strategies and NAAQS compliance.

Results of this research and development work (conducted by the NERL
principal investigator for SEM/EDX and by scientists of ManTech
Environmental Technology, Inc. under contract to NERL) are presented in the
following EPA report: "Guidelines for the Application of SEM/EDX
Analytical Techniques to Particulate Matter Samples," R. Willis, F.
Blanchard, T. Conner, EPA Report No. 600/R-02/070, September 2002.

Future Research Future development and applications of SEM/EDX will directly support the
NERL long-term research goals. SEM/EDX techniques will be used to
support the application of source apportionment techniques to personal and
indoor air samples. In addition, SEM/EDX analyses will be used to confirm
multi-variate source apportionment model results as well as demonstrate
limits of the models using ambient data. To further enhance source
apportionment modeling techniques, individual particle data obtained by
SEM/EDX will be applied directly in one or more multi-variate source
apportionment models.

Research
Collaboration
and Publications

National Exposure Research Laboratory — November 2002


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Contacts for

Additional

Information

Questions and inquiries can be directed to:
Teri L. Conner, Ph.D.

U.S. EPA, Office of Research and Development
National Exposure Research Laboratory (D205-03)

Research Triangle Park, NC, 27711

Phone: 919/541-3157
E-mail: conner.teri@epa.gov

Federal funding for this research was administered under EPA contracts 68-
D5-0049 and 69-D-00-206.

National Exposure Research Laboratory — November 2002


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