United States
 Environmental Protection
 Agency
Environmental Sciences Research
Laboratory
Research Triangle Park NC 27711
 Research and Development
EPA-600/S4-81-006  Mar. 1981
Project Summary
Aerosol  Analysis  for  the
Regional  Air  Pollution  Study

Final  Report

J.M. Jaklevic, R.C. Gatti, F.S. Goulding, B.W. Loo, and A.C. Thompson
  From May 1975 through April 1977
a total of 35,000 individual ambient
aerosol samples were collected at 10
selected sampling sites in the vicinity
of St. Louis, Missouri, as part of the
Regional Air Pollution Study (RAPS).
The  samples  consisted  of  aerosol
particles  in  the coarse  and fine
fractions  deposited on  membrane
filters using automatic dichotomous
air  samplers.   The samples were
returned to  Lawrence  Berkeley
Laboratory (LBL) for  analysis
following collection at the field sites.
Particulate mass was determined by a
beta-ray attenuation method, and the
concentrations for 27 elements were
determined using energy dispersive X-
ray fluorescence analysis.
  This Project Summary was devel-
oped by  EPA's  Environmental
Sciences  Research Laboratory. Re-
search Triangle Park. NC 27711, to
announce key findings of the research
project that is fully documented in a
separate report of the same title (see
Project Report ordering information at
back).

Introduction
  An automatic dichotomous sampler
was equipped with a two-stage virtual
impactor which separates particles into
two size fractions: above and below 2.4
ftm aerodynamic diameter. The upper
particle size  cutoff  for the coarse
particle fraction was determined by the
inlet configuration and is estimated to
be 20 /um. The coarse and fine particle
size fractions were collected separately
on 1.2 //m pore size cellulose ester
membrane filters. The normal sampling
schedule  consisted  of  twelve-hour
sample periods at eight of the stations
and six-hour sample periods at two of
the stations.
  The  procedures  followed  in  the
sampling  program   were carefully
controlled  to ensure  valid data.
Individually  numbered clean  filters
were loaded into separately numbered
36-sample  cartridges at LBL.  The
sample identification numbers  and the
corresponding  tare   weights  were
recorded on magnetic tape at the time of
the initial beta-gauge measurements.
The samples were then shipped to St.
Louis for exposure in the samplers. The
location and times of sampling were
recorded both on the cartridge labels
and in a separate sampling log. This log
also contained checklists  for site visits
and notes of any irregularities in the
sample  routine. The  exposed filters
were returned to  LBL,  where final
masses were determined, and the data
pertinent to the sampling conditions
were entered into the computer system
for subsequent data processing.

Mass Measurements
  The total mass of particlescollected in
each size fraction was measured using
an automated beta-ray   attenuation

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   method.  The  method  relies on  the
   exponential dependence of transmitted
   beta-ray  intensity upon mass, when a
   sample is placed between a 147Pm beta-
   ray source  and a  suitable  detector.
   Although  the  measurement  is
   straightforward,  the use  of  beta-ray
   attenuation  in  the  present  study is
   complicated   by  the  high  precision
   required. A typical  measurement
   consists  of  determining  the  mass
   accumulated on a 4 mg/cm2 filter to an
   accuracy of ± 10/ug/cm2. This requires
   that  each  mass   measurement   be
   accurate  to  0.1%. The elapsed time
   between  the measurements of the tare
   weight and the exposed weight might be
   several months.  Frequent  calibrations
   were  made  using a set   of  carefully
   weighed  polycarbonate films   as
   standards.

   X-Ray Fluorescence
   Measurements
     The elemental  composition  of  the
   particulate  deposits  was  measured,
   using  an  energy  dispersive  X-ray
   spectrometer.  The   particular  X-ray
   spectrometer employed was  an LBL-
   constructed  pulsed   X-ray excitation
   system, computer controlled for sample
   sequencing  and analysis. The  X-ray
   excitation was provided by a  series of
   three  secondary  fluorescent targets,
   which were irradiated with the output of
   a pulsed X-ray tube.  The precision and
   accuracy  of the method depended upon
   many components in the system, each
   of which  was carefully controlled.
     Several thin films  containing copper
   were  used as the primary calibration
   standard. Each film consisted  of a layer
   of copper deposited on a mylar  substrate
         and  were obtained from Micromatter,
         Inc. These standards were accurate to
         better than 2%.
           The relative excitation efficiencies for
         other elements were obtained using
         thin  film  standards prepared  by
         depositing an aerosol generated from a
         carefully prepared solution in which the
         relative concentrations  of elements
         were known. Where possible, the ratio
         of elements  was established  by the
         stoichiometry   of  the  chemical
         compound. In other cases, solutions
         contained individual elements mixed in
         known ratios. The accuracies  of the
         ratios  obtained  by this  method  are
         estimated to be less than 1%.
           Because of the importance of sulfur in
         this  program, exceptional  care was
         taken  in  its  calibration. Thin film
         standards were prepared by collecting
         an aerosol deposit of 0.3 [im diameter
         particles  in  order to  eliminate
         absorption  effects. Attenuation
         corrections were  made   for   coarse
         particles based on the assumptions of
uniform  spheres  of  composition
approximately that  of typical aerosol
particles.
  The  reproducibility  of  the aerosol
samples was checked by collecting side-
by-side  samples at  LBL,  using  three
automatic dichotomous samplers. The
root  mean square  deviation for  the
coarse particle fraction was  approxi-
mately 5%, whereas for the fine parti-
cles, it was about 1.5%. The precision of
the XRF analysis was checked by the
repeated analysis of the  same  filters
over an extended period  of time. The
reproducibility of the major  elements
indicates a stability of approximately
+ 1% over a three-month period.
  The analytical results were written on
magnetic  tape  that was sent to the
Environmental  Sciences  Research
Laboratory, Research Triangle Park, NC
27711,  from  which copies  may  be
obtained.  Arrangements  are  being
made  to  have  the tapes  available
through  the  National  Technical
Information Service, Springfield,  VA.
            J. M. Jaklevic, R. C. Gatti, S. F. Goulding, B. W. Loo, and A. C. Thompson are with
              the Lawrence Berkeley Laboratory, Berkeley, CA 94720.
            Thomas G. Dzubay is the EPA Project Officer (see below).
            The complete report, entitled "Aerosol Analysis for the Regional Air Pollution
              Study," (Order No. PB 81-157 141: Cost: $8.00, subject to change) will be
              available only from:
                   National Technical Information Service
                   5285 Port Royal Road
                   Springfield, VA  22161
                   Telephone: 703-487-4650
            The EPA Project Officer can be contacted at:
                   Environmental Sciences Research Laboratory
                   U.S. Environmental Protection Agency
                   Research Triangle Park,  NC 27711
                                                                                        & US GOVERNMENT PRINTING OFFICE. 1961-757-012/7029
United States
Environmental Protection
Agency
Center for Environmental Research
Information
Cincinnati OH 45268
                 Postage and
                 Fees Paid
                 Environmental
                 Protection
                 Agency
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Official Business
Penalty for Private Use $300
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