&EPA
                                 United States
                                 Environmental Protection
                                 Agency
                                  Industrial Environmental Research
                                  Laboratory
                                  Research Triangle Park NC 27711
                                 Research and Development
                                  EPA-600/S7-82-036  Sept. 1982
Project Summary
                                 Sampling  and  Data  Handling
                                 Methods for  Inhalable
                                 Particulate  Sampling
                                 Wallace B. Smith,  Kenneth M. Gushing, Jean W. Johnson, Christine T.
                                 Parsons, Ashley D. Williamson, and Rufus R. Wilson, Jr.
                                   The report reviews objectives of a
                                 research program established by the
                                 EPA on sampling and measurement of
                                 particles in the inhalable particulate
                                 (IP) size range in industrial process
                                 emissions, and  discusses methods
                                 and equipment that will be required. It
                                 summarizes research at Southern
                                 Research  Institute  to support  the
                                 development of techniques for mea-
                                 suring and characterizing emissions in
                                 the IP  size range.  Topics studied
                                 include computer  techniques  for
                                 analyzing  cascade impactor data to
                                 recover  information  on IP emissions
                                 available from existing data; concepts
                                 for maintaining  isokinetic sampling
                                 conditions at constant flowrates in
                                 particle-sizing devices; the design and
                                 use of cascade impactors, cyclones,
                                 and elutriators as particle collectors
                                 for IP sampling systems; and a stack
                                 sampling system in which the sampled
                                 gas is diluted under  conditions simu-
                                 lating those in stack plumes.
                                   This Project Summary was developed
                                 by EPA's  Industrial Environmental
                                 Research Laboratory.  Research Triangle
                                 Park, NC. 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
                                   The U.S. EPA  is  considering air
                                 pollution standards  for emission of
                                 inhalable particulate  (IP) matter from
                                 stationary sources. IP matter is defined
                                 in terms of particle size, sincethe extent
                                 of penetration of inhaled particles into
                                 the  lungs depends on their size.
                                   Adequate characterization of a pollu-
                                 tion source requires measurement of
                                 stack or fugitive emissions from the
                                 source and background levels in the
                                 ambient atmosphere as well.  The
                                 concentration and particle-size distribu-
                                 tion of the suspended particulate matter
                                 and, in some instances,  its chemical
                                 composition and biological properties
                                 must be determined.
                                   In December 1978 a workshop was
                                 held at Research Triangle Park, NC, to
                                 discuss the IP sampling and analysis
                                 problem and the EPA research program
                                 on  the subject. The workshop  was
                                 attended by consultants and other
                                 investigators  experienced in aerosol
                                 sampling and characterization.
                                   The consensus of those attending the
                                 workshop was that no methods in use
                                 were adequate for measuring the
                                 amount of material in the IP size range
                                 in process emissions. Thus they recog-
                                 nized the need for information on
                                 methods that could yield such data or
                                 that could be adapted to yield it, and for
                                 the  research necessary in the develop-
                                 ment of instruments and procedures for
                                 that purpose.
                                   This report contains recommendations
                                 resulting from that workshop  and
                                 summarizes related research at Southern
                                 Research Institute  on the  problem,
                                 under contract with the EPA.

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Recommendations for the
EPA Research Program

  The workshop participants recognized
that the greatest problem to be faced in
developing adequate measurement
methods  would  be  the  lack of time
available. They  concluded that  3 to 5
years would likely be required  before
reliable methods would be available for
obtaining the  detailed data needed.
They also  concluded that the only
practical  course would be the  use of
available  survey techniques to obtain
less  comprehensive data as soon as
possible while research programs were
initiated to develop  more accurate
methods for future use.
  Specific needs and problems recog-
nized at the workshop included the fact
that, in sampling ambient atmospheres
and  fugitive emissions,  inlets were
needed for the available samplers to
equip them for measuring mass con-
centrations in the IP size range.
  The lack of  realistic  and rational
strategies for sampling fugitive emis-
sions  was also  seen as a serious
problem.
  In  sampling stack emissions, the lack
of cyclones and inertial impactors
calibrated for recovery of the  IP size
range was noted. It was also recognized
that dilution and cooling  sampling
systems were needed that could simulate
the behavior of stack plumes, especially
the behavior of condensable vapors.
  Advanced techniques for extrapolation
of particle-size  distribution  curves to
larger  particle sizes  to yield additional
information on the IP size range were
noted as conceptually feasible but  not
yet in use.


Recommendations

  It  was  recommended  that the EPA
adopt a standard mathematical  perfor-
mance curve with specified tolerances
for sampling devices used to collect and
measure  IP matter. Figure 1 isthecurve
which was actually adopted. Any newly
developed device would have to be
calibrated and shown to agree with the
curve, within the tolerances specified.
The  shaded area was constructed by
plotting two log-normal curves through
the (13 /jm, 50 percent) and (17//m, 50
percent) points with geometric standard
deviations (crB)of  1.0 and 1.7, respectively,
and  allowing 10 percent for wall losses
of small  particles and 10 percent for
penetration of large  particles.
  Other tasks recommended for prompt
action were:
  • Analysis of existing  particulate
    emission data, using the Southern
    Research Institute curve-fitting
    procedure and the University of
    Minnesota modal analysis.
  • Calibration of  inlets for the hi-vol
    and  dichotomous samplers. This
    would also include the development
    of a  total mass sampler  (lo-vol)
    with the same f lowrate and inlet as
    the dichotomous sampler for use
    in ambient  measurements com-
    paring total mass  samplers with
    the dichotomous sampler.
  • A modified EPA Method 5 sampling
    train  was suggested  that would
    include in-stack cyclones with
    suitable cut points  (Dso values) for
    covering the IP size range.

Research at Southern
Research Institute  on the IP
Problem

Analysis of Cascade Impact or
Data
  Because of the lack of information on
the concentration of IP matter at particle
sizes larger than about 10/um (the upper
                           limit of the particle-size range covered
                           by an  impactor, i.e., the first-stage cut
                           point or Dso), a computer technique of
                           extrapolation of the impactor data to 15
                           A/m has been developed. The full report
                           discusses improvements in accuracy of
                           the extrapolation obtained by using a
                           first-order osculating polynomial for
                           fitting the cumulative mass curve
                           between the first stage Dso value andan
                           assumed maximum particle size.
                             The function is a third-degree poly-
                           nomial which uses the known charac-
                           teristics of the cumulative mass curve
                           for its solution over the range of particle
                           sizes. Tests of the  technique  on a
                           number of theoretical  unimodal and
                           bimodal size distributions demonstrated
                           a high degree of accuracy in recovering
                           the true cumulative particle concentra-
                           tion. Figure 2 shows an example of the
                           extrapolation  technique applied to
                           actual data  in which the  measured
                           distribution may have been distorted by
                           losses in a buttonhook nozzle or by an
                           improperly calibrated  cyclone.  It is
                           possible to suppress the fit through
                           upper stages to compensate for these
                           errors.  From  such  studies, it  was
                           concluded that the technique could be
                           used for recovering  IP  concentrations
                           from  existing impactor data within a
                          4     6   8 10       20
                             Aerodynamic Particle, um
                                                     60  80 100
Figure 1.
Recommended specifications for collection efficiency of samplers of
inhalable particulate matter.

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factor  of about  three, even when no
information was available .on the type of
nozzle or precollector that was used. If
the effects of these devices are known,
the errors  in the IP  data are probably
within the experimental error of sampling.
  Impactor data were also subjected to
a modal analysis in which the data were
fitted with multi-component log-normal
distributions by a simplex minimization
method. Data were extrapolated to 100
/urn  particle  diameter by  fitting the
portion of the size distribution for which
data  were available, Results were
similar to those obtained with the curve-
fitting polynomial procedure. IP concen-
trations could be estimated within a
factor of two or better.

Isokinetic Sampling by
Particle-sizing Devices
  Isokinetic sampling of a gas stream is
necessary if a representative sample of
suspended particles,  notably those
larger than 2 /urn in diameter, is to be
obtained. This presents the problem of
maintaining  isokineticity in a  sizing
device such as a cyclone or an impactor,
in which the particle-sizing characteristics
are a function  of  flowrate. Several
techniques and devices for solving this
problem are suggested in the full report.
                                                                -r/o1
     ro4-,-
8
10
1
                                2nd Oso Omitted

                                 •6
                                  
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EPA Source Assessment  Sampling
System (SASS), operated at 185 l/min
and 204°C, and  the EPA Fugitive
Ambient  Sampling Train (FAST), ope-
rated at 5,282 l/min and 23°C.
  For the actual field sampling systems
for  IP measurement, it was  decided to
                           develop trains using cyclones for the IP
                           sampling collector. This decision was
                           based on  the  fact that cyclones  are
                           proven field sampling devices  without
                           the damaging problems of particle
                           bounce  or reentrainment.  The  only
                           particular design difficulty is the lack of
 Thermocouple
                                 Stack
                                 Wall
                                       Temperature
                                       Controller
                                             Remote Actuated
                                             Valve   I
                                Dilution Air
               Sizing
               Device
                      ^Condenser
                       .and
   1 Nozzle
 Figure 4.
                                    [Dry,
                                        •er
                                                     Micro Processor
 Figure 3.    Cool gas recycle concept.
                    Theory (Rectangular)
                    Experiment
                2    34     6   8  10        20

                   Aerodynamic Particle Diameter, um
                                          30  40    60  80 100
Theoretical and experimental collection efficiencies for a horizontal
elutriator with rectangular cross-section, plate length 38.1 cm, average
gas velocity 70 cm/sec.
a reliable theory for cyclone performance.
Although  many attempts have  been
made to predict the behavior of cyclones
from their geometry,  or at  least to
describe their performance by empirical
mathematical expressions,  it is still
necessary  to  calibrate them  experi-
mentally with laboratory-generated
aerosols over a range of temperatures
and flowrates similar to those likely to
be encountered in field use.
  Several commercially available cyclones
and  some  especially fabricated  were
calibrated to provide a basis for design
of cyclones for use in an IP sampler. The
individual  cyclones  of the Southern
Research Institute's five-stage  cyclone
system were thus calibrated as part of
this empirical design  process.
  Under laboratory conditions (temper-
ature 22°C, flowrate 28.3 l/min, and
particle density 1.0 g/cm3) the cut
points of the individual cyclones are 5.6,
2.1,1.4, 0.63, and 0.33um, as shown by
the calibration curve of efficiency vs.
aerodynamic particle diameter in Figure
5.
  From design parameters developed in
the previous cyclone calibration studies,
geometries for the  IP  cyclones  were
selected. Two  cyclone systems  were
designed, and evaluated: a cyclone to be
used  as a precollector  for cascade
impactors, and a system of two cyclones
(Figure 6) and a filter in series, to be used
as the primary system for measuring IP
and fine particle concentrations. Both
systems were designed for high-
temperature operation  in process
streams. The  precollector for impactors
and the first cyclone in  the series train
had collection efficiency curves satisfying
the specifications for IP samplers
shown in Figure 1. The second  cyclone
in the series train was designed to have
a Dso value  of 2.5 ±0.5/um aerodynamic
at the flowrate required for the 1 5 /um
cut in the first cyclone.
  To measure the paniculate formed by
condensation of volatile material as the
hot stack gases mix with ambient air, a
Stack Dilution Sampling System (SDSS)
was designed. The system was designed
to be used with the in-stack IP  dual-
cyclone sampler. Figure 7 shows major
components of the apparatus. In opera-
tion, gas from the stream being sampled
is drawn through the IP cyclone sampler,
in which particles larger than 15/um and
those 2.5-15 um are removed in two
stages. The  gas containing the fine
particle fraction (less than 2.5 /urn) and
the condensable vapors passes through
the dilution  chamber, and through

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    100
  u
 Uj
 §
 ti
 •SJ
 §
                                      Q = 1.0ACFM
                                      7 = 22°C
                                        m  Cyclone V
                                           Cyclone IV
                                           Cyclone III
                                           Cyclone II
                                           Cyclone I
                                          \\        \
              0.2
0.3 0.4  0.60.81.0     2.0      4   6
  Aerodynamic Particle Diameter, Mm
                  8 10.0   20.0 30.0
 Figure 5.    Calibration curves for  the five-stage cyclone system.  Flowrate  1.0
             ft3/min. temperature 22°C.

                Sampling Nozzle

                            Probe
 Cyclone SRI-X
 Dso=15±
Cyclone SRI III
050 = 2.5 ±0.6/urn
 Figure 6.     Sketch  of two-cyclone
              system.

 heated probe and sample line and is
 introduced axially into the bottom of the
 cylindrical  dilution chamber. Here  the
 gas is mixed with dilution air to form a
 simulated plume which flows up through
the dilution chamber, and through a
standard hi-vol filter, which collects the
fine particles and any new particles
formed by condensation. The design of
the dilution chamber simulates the flow
patterns and mixing times observed in
actual plumes.
  A field version of the dilution  system
was  constructed  to  the  following
specifications:
  Active length of dilution tube, 1.22 m
  (4ft)
  Total height of sampler, 1.8-2.1 m (6-
  7ft)
  I.D. of dilution tube, 21.3 cm (8.4 in.)
  I.D. of sample inlet tube,  4.27  cm
  (1.68 in.)
  Active dilution volume, 43.6 I (1.54
  ft3)
  Sample  flowrate,  17  1/min  (0.6
  ftVmin), determined by cyclone cut
  point
  Dilution  flowrate,  425  1/min  (15
  ftVmin)
  Dilution factor, 25
  Residence  time,  6.2  sec Sample
  velocity, 25 cm/sec at 150°C Dilution
  air velocity, 19.8 cm/sec at 21 °C

  The system was tested on flue  gas
from a domestic furnace burning fuel oil
under controlled combustion conditions.
The  results  indicated  that  organic
chemical vapors  condensed to solid
particles within the dilution chamber as
expected, at dilution ratios of 10 to 40.
Higher dilution ratios favored a larger
number of small particles.

Selected Bibliography
Gushing, K. M., J. D. McCain, and W. B.
Smith. Experimental Determination of
Sizing Parameters and Wall Losses of
Five Source-Test  Cascade Impactors.
Environ. Sci. Technol. 13:726, 1979.

Johnson, J. W., G. I. Clinard, L G. Felix,
and J.  D. McCain. A Computer-Based
Cascade Impactor Data  Reduction
System. Report EPA-600/7-78-042
(NTIS PB 285433), Southern  Research
Institute, Birmingham, AL, March 1978.
601 pp.
                                        McCain, J. D., G. I. Clinard, L G. Felix,
                                        and J. W. Johnson. A Data Reduction
                                        System for Cascade Impactors. Report
                                        EPA-600/7-78-132a (NTIS PB 283173),
                                        Southern Research Institute, Birming-
                                        ham, AL, July 1978. 44 pp.

                                        Smith, W. B., P. R. Cavanaugh, and R. R.
                                        Wilson, Jr. Technical Manual: A Survey
                                        of Equipment and Methods for Paniculate
                                        Sampling in Industrial Process Streams.
                                        Report EPA-600/7-78-043  (NTIS PB
                                        282501), Southern Research Institute,
                                        Birmingham, AL, March 1978. 280 pp.

                                        Smith, W. B., R. R. Wilson, Jr., and D.
                                        B. Harris. A Five-Stage Cyclone System
                                        for  In-Situ  Sampling. Environ. Sci.
                                        Technol.  13(11): 1387-1392, 1979.

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                 Hi- Vol Impactor
                 Filter Assembly
   Process Stream
Dilution
Chamber
  Exhaust Blower
                                                 To Ultrafine
                                            jl   Particle Sizing
                                                System (Optional)
                                                   Dilution Air
                                                  'Heater
                                                         Condenser
                 -To Heaters, Blowers
                  Temperature Sensors
                                     To Orifice      Ice Bath
                                     Pressure Taps
                                                                 Dilution Air
                                                                 Blower
                                    Flow, Pressure
                                    Monitors
                    1 Main Control'
Figure 7.     Diagram of stack dilution sampling system (SDSS).
   'Wallace  B.  Smith, Kenneth  M. Gushing, Jean W.  Johnson, Christine  T.
    Parsons, Ashley D. Williamson, and Rufus R. Wilson, Jr., are with Southern
    Research Institute, Birmingham, AL 35255.
   D. Bruce Harris is the EPA Project Officer (see below).
   The complete report, entitled "Sampling and Data  Handling Methods for
    Inhalable Paniculate Sampling," (Order No. PB 82-249 897; Cost: $22.50,
    subject to change} will be available only from:
          National Technical Information Service
          5285 Port Royal Road
          Springfield, v'A 22161
          Telephone: 703-487-4650
   The EPA  Project Officer can be contacted at:
          Industrial Environmental Research Laboratory
          U.S. Environmental Protection Agency
          Research Triangle Park, NC 27711
    . S. GOVERNMENT PRINTING OFFICE: 198^559 -092/0505

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