EPA-600/4-78-009
January 1978
Environmental Monitoring Series
  IEVELOPMENT OF A LARGE SAMPLE  COLLECTOR
             OF RESPIRABLE  PARTICULATE  MATTER
                               Environmental Monitoring and Support Laboratory
                                       Office of Research and Development
                                      U.S. Environmental Protection Agency
                                 Research Triangle Park, North Carolina 27711

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                RESEARCH REPORTING SERIES

Research reports of the Office of Research and Development, U.S. Environmental
Protection Agency, have been grouped into nine series. These nine broad cate-
gories were established to facilitate further development and application of en-
vironmental technology. Elimination  of traditional grouping was consciously
planned to foster technology transfer and a maximum interface in related fields.
The nine series are:

      1.   Environmental Health Effects Research
      2.   Environmental Protection Technology
      3.   Ecological Research
      4.   Environmental Monitoring
      5.   Socioeconomic Environmental Studies
      6.   Scientific and Technical Assessment Reports (STAR)
      7.   Interagency  Energy-Environment Research and Development
      8.   "Special"  Reports
      9.   Miscellaneous Reports

This report has been assigned  to the ENVIRONMENTAL MONITORING series.
This series describes research conducted to develop new or improved methods
and instrumentation for the identification and  quantification of environmental
pollutants at the lowest conceivably significant concentrations. It also includes
studies to determine the ambient concentrations of pollutants in the environment
and/or the variance of  pollutants as a function of time or meteorological factors.
 This document is available to the public through the National Technical Informa-
 tion Service, Springfield, Virginia 22161.

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DEVELOPMENT OF A LARGE SAMPLE COLLECTOR OF RESPIRABLE
                 PARTICULATE MATTER
                         by

            W.M. Henry and R.I. Mitchell
           Battelle, Columbus Laboratories
                Columbus, Ohio, 43201
                   No. 68-02-0752
                   Project Officer

                 Richard J. Thompson
             Analytical Chemistry Branch
   Environmental Monitoring and Support Laboratory
    Research Triangle Park, North Carolina 27711
   ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
         OFFICE OF RESEARCH AND DEVELOPMENT
        U.S. ENVIRONMENTAL PROTECTION AGENCY
    RESEARCH TRIANGLE PARK, NORTH CAROLINA 27711

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                                  DISCLAIMER

     This report has been reviewed by the Environmental Monitoring and Support
Laboratory, U.S. Environmental Protection Agency, and approved for publication.
Approval does not signify that the contents necessarily reflect the views and
policies of the U.S. Environmental Protection Agency, nor does mention of
trade names or commercial products constitute endorsement or recommendation
for use.
                                       ±±

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                                   ABSTRACT

     This report presents the final results of an experimental program to
develop a system of size-selective air particulate collection and analysis to
provide compositional particulate air pollutant data in support of health and
toxicity studies.

     A massive air volume sampler has been designed and constructed to collect
large masses of particulates in three particle size ranges:  >3.5 ym, 1.7 to
3.5 ym, and <1.7 ym.  The latter two smaller size ranges represent the partic-
ulates deemed by aerosol physiologists to be representative of the respirable
size particles.  The partition of the respirable fraction into two size ranges
is to provide more definitive data on aerosols which have been created by
secondary processes, such as photochemical reactions.

     Field tests of the sampler design and construction show that better than
gram masses of urban atmospheric particulate loadings can be collected in 24-
hour periods;  the samples can be recovered readily from the sampler collector
substrates;  and the mass fraction obtained correlates closely with cascade
impactor sampling results.

     Compositional and structural examinations of the collected particulates
clearly show that different size ranges have different chemical and physical
properties.  It is foreseen that the mass collection capability of the sampler
would provide respirable size particulate samples for certain types of health/
toxicity studies as well as providing samples for chemical analysis.

     Evaluations of the samplers in regard to sampling precision, collection
efficiency, and possible reaction of sulfur dioxide and nitrogen dioxide
during the collection process need completion.  These efforts were interrupted
                                      iii

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by a need to place the sampler immediately in the field at an Environmental
Protection Agency background catalyst study site.

     The field use of the  samplers on a continuous basis, rather than in the
intermittent mode as originally planned, revealed certain operational and
stability problems.  These problems were resolved under an expansion of the
program efforts to provide for better structural and field operational perform-
ance.

     This report is submitted in  fulfillment of Contract No. 68-02-0752 by
Battelle's  Columbus Laboratories  under the sponsorship of the U.S. Environ-
mental Protection Agency.  It covers a period from June 14, 1973 to April 13,
1975.
                                       iv

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                              CONTENTS
Abstract	*	iii
Figures	vi
Tables	vii
Acknowledgements	ix
     1. Conclusions 	  1
     2. Eecommendations 	  3
     3. Introduction 	 5
     k. Discussion	29

Appendices
     A. Operational and Procedural Description of Massive Air
        Volume Sampler	31
     B. List of Attendees of Aerosol Sampling Technology Meeting .  . ,h2

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                                   FIGURES

Number
    1  Generalized analytical scheme  	  8
    2  Los Alamos curve for first stage collection  	 10
    3  Collection efficiency of Aerotec 2 cyclones  	 11
    4  Prototype of High Volume air sampler	15
    5  Impaction efficiency curve for slot jet	16
    6  Particle size distribution of downwind pollutants at San Diego
          freeway site	.20
    7  Particle size distribution of upwind pollutants at San Diego
          freeway site	21
    8  X-Ray diffraction patterns of 4-day   (100-hr) collections 	 26
    A-l  Overall photograph of massive air sampler	32
    A-2  Lower part of massive air sampler showing  flow meter, electro-
         static power unit, and voltage meter	.33
    A-3  Impactor plate assembly module, partially  withdrawn 	 36
    A-4  Closeup of impactor plate assembly  (upper) and electrostatic
         precipitator  (lower) closed drawer compartments	37
    A-5  Electrostatic precipitator assembly, partially withdrawn  ....  39
                                      VI

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                                   TABLES
Number
     1 Particulate collection at L.A. site	18
     2 Semiquantitative optical emission analyses for metals 	 23
     3 Analyses of collected particulates from L.A. background catalyst
              study site — results in percent	2U
                                    vii

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                               ACKNOWLEDGEMENTS

     The encouragement, technical advice, and coordination of Dr. Richard J.
Thompson, Project Officer at the Environmental Protection Agency  (EPA), is
acknowledged with sincere appreciation.  Dr. Thompson has been particularly
helpful in developing the scope of work and overall sampling technology to
coordinate with the aims and objectives of the EPA health research groups.
The cooperation of the EPA Background Catalyst Site project team under the
overall direction of Mr. Franz Burmann and coordination of Mr. Charles Rodes
is appreciated.  Finally, the efforts of several Battelle Columbus Labs per-
sonnel are acknowledged, notably Norman Henderson for his efforts in fabrica-
tion and construction of the samplers, Peter Jones for his work on the organic
phase analyses, and R. Heffelfinger, D. Chase, C. Litsey, J. Lathouse, and P.
Schumacher for inorganic phase analyses.
                                     IX

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                               ACKNOWLEDGEMENTS

     The encouragement, technical advice, and coordination of Dr. Richard J.
Thompson, Project Officer at the Environmental Protection Agency  (EPA), is
acknowledged with sincere appreciation.  Dr. Thompson has been particularly
helpful in developing the scope of work and overall sampling technology to
coordinate with the aims and objectives of the EPA health research groups.
The cooperation of the EPA Background Catalyst Site project team under the
overall direction of Mr. Franz Burmann and coordination of Mr. Charles Rodes
is appreciated.  Finally, the efforts of several Battelle Columbus Labs per-
sonnel are acknowledged, notably Norman Henderson for his efforts in fabrica-
tion and construction of the samplers, Peter Jones for his work on the organic
phase analyses, and R. Heffelfinger, D. Chase, C. Litsey, J. Lathouse, and P.
Schumacher for inorganic phase analyses.
                                     IX

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                                   SECTION I

                                  CONCLUSIONS

     Considerations of the requisite sample loading and size separation
requirements of the program showed that a sampler design utilizing two impactor
stages and an electrostatic precipitator could provide for collection of gram
quantities of respirable range, urban air particulates in a 24-hour period.

     Calibration and field test data demonstrated that the designed and
constructed sampler does provide the size range cutoff particulate sizes
deemed by aerosol physiologists as most representative for health effects
study.

     The collections can be readily removed from the Teflon-coated impactor
stages and from the very pure aluminum (Al) electrostatic plates without
introducing substrate contamination into the samples.

     The sampler provides for two cutoff sizes in the respirable size range,
1.7 to 3.5 urn and <1.7 urn, and for particles above the respirable range, >3.5
to 20 ym-  Thus, a total sample analysis can be obtained for comparison with
the more prevalent total suspended particulate (TSP) data.

     Collections of well over 1 gram (g)  can be made in a 24-hour period, so
detailed analytical methodology development can be carried out to provide
compound and species identification needed for toxicological testing and for
interrelating population health effects studies with particulate burdens.
Analytical examinations show definite composition versus size relationships
for many species.

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     In summary, the program efforts show the following benefits to health
study programs.
    (1)  Realistic,  "live", contaminant-free, air particulate burden samples
         can be collected  for the effective carrying out of dose/response
         health effects surveys and  studies.  Realistic and "live" samples
         refer to particulates collected  in large masses and segregated into
         respirable  and nonrespirable cuts.  These cuts show distinct differ-
         ences in appearance and odor emanations.  These physical attributes
         of particulate collections  are striking and usually are masked when
         samples are imbedded in filter or other substrate modes of collection.

     (2)  The samplers can  collect sized particulates in sufficient masses for
         in-vitro and in-vivo health studies.

     (3)  Samples can be collected in time periods which permit unusual atmos-
         pheric burden episodes, such as  inversions or unusual source emissions,
         to be sampled, analyzed, and the particulate species related to
         observed health consequences.   (Compare collection rates of about
         1000 cfm with the 40 cfm of high volume  [hi-vol] samplers.)

     (4)  Long-needed data  bases can  be obtained now on the presence and
         quantities  of pollutant species  contained in fine, respirable partic-
         ulates.  To date, overall species characterization efforts have been
         seriously hampered by lack  of adequate, contaminant-free samples,
         with a result that comparatively little is known on the presence of
         overall specific  and possible harmful  compound forms of pollutants.

     (5)  Continued investigations, as outlined  in the Recommendations, should
         permit completion of the original objective of the program:  to
         identify and quantitate species  implicated as causative agents for
         observed adverse  health effects  in man.

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                                  SECTION II

                                RECOMMENDATIONS

     The design and construction efforts on this program have provided a novel
system wherein airborne particulates can be collected in masses large enough
both to obtain detailed knowledge of size-related chemical and physical proper-
ties of pollutants and their associated health effects via in-vitro and in-
vivo studies.  The applications recommended for use of the system include:

     •   Obtain short-term "episodic" respirable particulate compositional
         analysis for correlation with health effects studies at Community
         Health and Environmental Surveillance System (CHESS) sites.
     •   Monitor point sources upstream and downstream to ascertain
         potentially hazardous compound species emissions.
     •   Collect specific particles—asbestos, silica, radionuclides, etc.—on
         a size basis either in short- or long-term periods.
     4   Collect sized samples solely for health burden studies
     •   Couple the Massive Air Volume Sampler with gaseous pollutant sampling
         collection to obtain total respirable range health burdens of pollut-
         ants by urban area, source emission, industrial operation (mining,
         refining, processing), residential (indoor-outdoor), and/or near
         heavy traffic areas.

     Analytical investigations on the program show that the capability to
collect relatively large masses of samples, free from troublesome substrate
interference, greatly facilitates obtaining complete compound identification
of inorganic and organic species.  It is recommended now that basic analytical
methodology developments be carried out to reduce compound identification
methods to routine practice in order that large numbers of samples can be
processed economically.  This would permit the obtaining of far more compre-
hensive and meaningful data bases than are available at this point for promul-
gating air quality standards, prescribing control process limitations, and
assessing health burdens of particulates.
                                      3

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     Prior to extensive field collection and analysis efforts, it is recom-
                                                            [i
mended that the precision, collection efficiency, and study of possible
sulfur dioxide  (SO2> and nitrogen dioxide  (NOj) reactions during sample
collection be studied in greater depth.  The possibility of ozone  (03)
formation in the electrostatic  section should be checked more thoroughly,
although no 03  odor  can be detected  and the overdesign feature permitting
operation at about 8000 volts appears to preclude this concern.  The collec-
tion efficiency for  very small  aerosols, estimated  50 percent for the 0.05-ym
range,  should be checked.

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                                  SECTION III

                                 INTRODUCTION

     Each year the evidence demonstrating health effects of pollutants has
become more impressive, and there now is little debate on whether pollutants
are harmful.  Rather the amount and types of pollutants which are safe and
tolerable have become the subject of debate.

     During recent years it has become apparent that the total mass concentra-
tion of particulates is not a definitive measure of the health hazard due to
airborne particles.  A major reason for this is that usually the aerosol
sampling has been performed using single stage collectors, with these collec-
tions analyzed to determine the mass concentrations and/or the constituents of
the overall samples.  Since most aerosols are polydisperse, the mass median
size approaches that of the larger particles in the sample.  Thus, the mass
concentration values of such samples are for practical purposes determined by
the concentration of the relatively fewer larger particles.  If these particles
are nonrespirable, the measured mass data will have little direct relationship
to the inhalation hazard of the pollutants, and attempts made to correlate
health effects with particulate burden can be ineffective.

     Size selective particulate sampling and analysis obviously would be more
meaningful, but thus far most sampling of this type has been directed toward
obtaining information primarily on particle size distribution.  The sample
mass obtained for each size range is quite small and is entirely inadequate
for complete chemical and physical characterization.  A further problem often
posed both by single and multistage samplers has been that of the substrate
collector stage or stages.  Frequently the collected sample cannot be separated

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totally from the collector substrate, and the resulting substrate contamination
severely impairs the accuracy of analysis of the collected particulates.

     The program, defined in concert with the EPA Project Officer and de-
scribed in the following sections of this report, was designed to develop a
system which would overcome the present day obstacles in obtaining size selec-
tive particulates on a  substrate interference-free basis in sufficient quan-
tities to provide the comprehensive analyses needed to realistically identify
pollutant characteristics with health effects studies.

                                  OBJECTIVES

     The overall objective of this program is to determine the chemical
composition of airborne particulate matter which constitutes the respirable
size in humans.  In order to achieve this objective, a sampler must be designed
capable of:
     •   Collecting large masses of particles in the respirable range and
         excluding particles above the respirable range, and
     •   Utilizing a collection system or medium which will not alter the
         particulate matter collected and which will yield a sample in a form
         and  size  (mass) amenable to a wide array of analytical methodology
         development effort.

     The primary objective of  the study  is to obtain elemental and compound
composition of those species which may have a deleterious effect on human
health with particular  attention to be focused  on the sulfate species  (both
organic and inorganic).

                                PROGRAM PLANNING

SAMPLER DESIGN

     The deposition  site of particulate  matter  in the lung is a function of
particle size, particle density, and breathing  rate.  Larger particulates
which manage  to penetrate beyond the nasal-pharnyx  region deposit on the

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ciliated epithelium of the upper trachael-"bronchial tree and effectively elim-
inated from the lung within a. few hours.   Smaller particles deposit in the
lower portions of the lung which are not  ciliated and may remain in intimate
contact with the thin alveolar membrane for weeks or months (depending upon
solubility).  Therefore, it is essential  to know what portion of an air pollut-
ant falls in the size fraction which will deposition the nonciliated portion
of the lung.
     When particle size data are missing on total particulate loading obtained
on an absolute filter, the NCRP-ICRP standards* have provided a built-in parti-
cle size correction which is based upon the assumption that only 12.5 percent
of the weight of the aerosol reaches the  nonciliated portion of the lung.
Therefore, it is necessary to develop samplers which will eliminate the need
for this arbitrary assumption that 12.5 percent is respirable.  Actually when
the primary source of the aerosol is from a combustion source, a major portion
of the aerosol is respirable.  Small differences in mass median diameter of an
aerosol can produce profound differences  in the region of prominent deposition.
     It was the concept of this part of the study to develop a hi-vol sampler
that has sampling characteristics which duplicates the "Respirable Dust Stand-
ard" defined by the Health and Safety Laboratory (HASL).
     The desired sample size of at least  1 g requires that the sample flow rate
be extremely large for most ambient conditions in order to collect this
sample within a reasonable period of time (l or 2 days).  The power limita-
tion — 15 amperes at 110 volts with a high efficiency blower which will pull
about 5 inches of water vacuum — limits  its size to about 30 cubic meters
per minute.
     The restriction that not more than 1 percent of the sample collected can
be larger than 8 urn while maintaining an  effective cutoff size of approximately
3.5 um appears to require the use of an impactor stage rather than a high-
volume cyclone.  (Subsequent to the initiation of the experimental program,
the requirements of the sampler design were changed to provide for a two-stage
*ICRP Standards: "Particulate Deposition and Retention Models for Internal
Dosimetry of the Human Respiratory Tract," Health,  Vol.  12, pp.  173-207,
1.966.  (Task Group on Lung Dynamics, International Commission on Radiological
Protection.)

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collection which would accommodate collection of secondary aerosols. (Details
of this provision  and design changes are given in the Experimental Work section
of this report.)

SAMPLE ANALYSIS

     Plans for complete chemical composition analyses usually divide samples
into two major classes:   organic and inorganic.   Within these major classes
there is a further subdivision:   elemental and species or compound identifi-
cation which must  be  considered  if appropriate data for health effects are to
be obtained.  In planning the analysis  of collected samples it is anticipated
that relatively large masses of  each particulate size fraction will be avail-
able so that, for  the most part,  separate sample portions can be used for each
analytical procedure  or method.   The general scheme planned for chemical and
physical characterization of samples is shown in Figure 1.  The organic soluble
fraction methods of analysis,  gas chromatography (GC),  mass spectrometry (MS),
GC-MS, and infrared (IR)  give compound  and/or species class indent!fication.
This is not true for  the inorganic compounds.   Generally,  complete elemental
analyses were planned using  such techniques as optical  emission spectrography
(OES); X-ray fluorescence (XRF);  spark  source mass  spectrometry (SSMS) ;  atomic
absorption spectrometry (AAS); gas mass spectrometry (GMS);  anion determina-
tion; ultimate analyses (CHN); total sulfur and carbon;  plus possible oxygen

                               SAMPLE CHARACTERIZATION

1 1
ELEMENTAL ANIONS
OES CHEMICAL
XRF AND ION-
SELECTIVE
SSMS ELECTRODE
AAS DETERMINA-
CHEMICAL T'ONS
TOTAL S
TOTAL C
C, H, N
1
| PARTICLE
COMPOUND SIZING SOLVENT E
XTRACTION
XRD OM 1
SEM EM ORGANIC FRACTION ANALYSES
ED
K-CELL

ESCA J | ||
EM GC MS GC-MS IR
                      Figure 1. Generalized analytical scheme.
                                       8

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determinations.  These should give a reasonable material balance on the samples.
Determination of inorganic species or compounds are much more difficult.
Available for these data are X-ray, diffraction (XRD); scanning electron micros-
copy (SEM); electron diffraction (ED); electron microscopy (EM); Khudsen cell
mass spectrometry (K-cell MS); and electron spectroscopy for chemical analysis
(ESCA).

     Originally, ten sets of duplicate samples from selected urban areas vere
planned in this program.  On revision of the planned sampler design, this was
reduced to two to three areas to accommodate the increased effort required to
redesign and construct a three-stage sampler system rather than the originally
proposed two-stage.   Finally, only single site sample collections were under-
taken in the program, since it appeared to be of most need to utilize the
samplers immediately to collect particulate at the EPA Background Catalyst
Study site.

                                EXPERIMENTAL

     Shortly after the inception of the program, discussions with the EPA
Project Officer revealed that there were some questions among the health study
group at EPA and elsewhere on the exact particle size fractions of particulates
which would represent the most realistic sample collections for health studies.
Pending resolution of this problem, initial efforts on the sampler design and
construction were carried out on a small prototype system.

INITIAL SAMPLER DESIGN CONSIDERATIONS FOR A TWO-STAGE SAMPLER

     Initial design considered a two-stage, hi-vol sampler which would provide
a collection efficiency of the first stage to duplicate the Health and Safety
Laboratory (HASL) or "Los Alamos" curve as shown in Figure 2.  Both an
impactor stage and a bank of miniature cyclones were considered to remove the
large  diameter aerosol particles.   An impactor stage should have a cutoff size
between 3-5 and U-ym.  The impactor jets would be extremely long slits and the
velocity through the slits would be minimized to reduce particle blowoff on
the impaction surface and to reduce the overall pressure drop.

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         C9
         2
         CO
         u
         <
         oc
           0.2
                        2          4          6          8        10
                    PARTICLE  SIZE OF UNIT DENSITY,microns
           Figure 2.  Los Alamos Curve  for  first  stage collection.
     If it were found that  the  cyclones  had the desired operating character-
istics, they would be used  since  they can be purchased commercially.   Dr.
              *
Morton Lippman  has shown that  the Aerotec  2 cyclone,  when operated at the
proper flow rate, closely reproduces  the HASI»  curve.   Figure 3  obtained from
Mr. Lippman1s final report  (December  15,  1972)  shows the composite collection
curve efficiency obtained for four Aerotec  2 cyclones  at several  flow rates.
The curve obtained at a  flow rate of  450 liters/min comes closest to  reproduc-
ing the HASL curve.  It  would be  expected the  the  larger Aerotec  3 cyclone
*Lippman, M., "Evaluation of  Tliree  Cyclones  for AEC-AGIN Size  Selective
Sampling.1*  Final Report on Contract  HSM099-17-48,  NIOSH.
                                       10

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 would have a  similar collection efficiency at about the same pressure drop.
 Although the  cyclones did appear to provide the desired characteristics,
 consideration of their use subsequently was abandoned since a large number of
 units would be required to obtain the flow rate needed for large mass collec-
 tion which in turn would make the sampler unwieldy from a bulk and weight
 aspect.
                                                       *

      A high-efficiency electrostatic precipitator appeared to be most suitable
 for collection of the very fine respirable-size particulates on the basis of
 collection efficiency, low pressure drop, and minimal substrate problems.
 Filters would have to be massive in size in order to avoid an excessively high
 pressure  drop and would create an undesirable substrate problem.  An impactor
 stage, even with extremely long slits, would not be efficient for particles
  100
   75
o
u
>-
>
z  50
   25
                                       S.S.AEROTEC2
                                       COMPOSITE NO. 1-4
                           S.S. AEROTEC 2 SANITARY CYCLONE
                           CARBON STEEL AEROTEC 2 CYCLONE
o 500 Ipm
D 450 Ipm
A 430 Ipm
O 400 Ipm
• 350 Ipm
'• 430 Ipm
A 430 Ipm
* ACGTH
                           UNIT DENSITY SPHERE, microns
            Figure 3.   Collection efficiency of Acrotec 2 cyclones.
                                        11

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less than 0.5 ym.  The electrostatic precipitator necessarily would require
special design to provide for high efficiency for particles less than about
0.5 um and to minimize the possibility of 03 formation which could cause
chemical reaction during the collection process.

TWO-STAGE PROTOTYPE SAMPLER

     A small-scale prototype sampler using two Aerotec-2 cyclones and a full-
scale electrostatic sytem was assembled to test the collection efficiency for
respirable range particulates*   This small unit has the capacity  (not fixed)
of providing the size distribution desired by EPA and can be scaled up to
provide the requisite sample mass.

     In addition to this assembly, a small-scale  (approximately 5 cfm) impactor
stage was constructed.  This stage has the same slit width as that needed for
a full-scale sampler.  Its slit length can be adjusted to give the sampling
capacity and cutoff size decided as most desirable by EPA respiratory physiol-
ogists.  The impaction characteristics of the large slit impaction stage with
a slit width of 1/4 inch was tested and calibrated using 3.5-vim particles
generated with a Berglund monodisperse aerosol generator.

     A sample of Columbus air particulate matter was collected with the
prototype sampler utilizing two Aerotec-2 cyclones and a full-scale electro-
static precipitator.  The sampler was operated to produce a cyclone cutoff of
3.. 5  pm  (particulate size at which 50 percent detection efficiency is achieved).
Limited examination of the two  size fractions, generally characterized as
>5 um and <5 ym showed the following:
     (1)  Sulfur  (S) contents are size dependent and principally are of an
         inorganic nature—total S was determined to be about 2 percent in the
         >5-ym size range and about 6 percent in the <5-ym size sample.  Total
         S determinations made  after organic solvent extraction gave approxi-
         mately the same values indicating the organosulfur contents to be
         quite low.
                                       12

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     (2)  The electrostatic precipitator fraction was extremely difficult to
         recover.  This suggested a redesign wherein the plates can be individ-
         ually removed for cleaning and where a precipitator substrate material
         which will not materially contaminate the collected sample is used.
Resolution of Definition of Respirable Range Particulates

     In meetings with EPA aerosol physiologists and leading experts* in
aerosol sampling technology, it was decided that:
     (1)  The ACGIH curve provides the best knowledge to date as to what
         constitutes the respirable aerosol fraction and that the first stage
         of our sampler should try to duplicate this curve as much as possible
         and have a cutoff size of 3.5 ym.
     (2)  Secondary aerosols (principally photochemical) are less than 2 ym,
         and a special stage should be added to our sampler to collect a major
         portion of these aerosols.  It was decided that the cutoff size for
         this stage should be close to 1.5 ym.

Revised Sampler Design - Three Stage Collector

     The cutoff size of the second stage of the sampler was made at 1.7 ym.
The slight reduction to 1.5 ym would have reduced sampling rate considerably
compared to only about a 25 percent reduction for a 1.7-ym stage.

     In the design of the sampler, special consideration was given to the best
means of collecting the 'first two size fractions.  For the first stage either
cyclones or impaction techniques could have been used with reasonable power
requirements.  The problem with cyclones is that the collection efficiency
curves begin to deteriorate at the higher flow rates.   At least 30 cyclones
would have been required to maintain our sampling rate and still have a reason-;
able collection efficiency curve.  The size of the sampler would have been
increased quite dramatically using cyclones.

     The addition of the intermediate stage for the collection of the primary
respirable aerosols would almost necessitate using impaction techniques.
*A list of attendees at this meeting is given in Appendix B.
                                      13

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Cyclones to achieve the desired particle size classification would have
extremely low flow rates and excessive power requirements.  The size of the
sampler would have been increased significantly and the sampling rate decreased
drastically.

     Based on the above, it was decided to use impaction stages to obtain the
desired particle collection.   Impaction characteristics are much better
predicted than sampling characteristics of cyclones.  Also, impaction plates
are much easier to fabricate.

     The requirement  that  there should be minimum  contamination with the
collection substrate  almost dictated  that the submicron particles be collected
using  an electrostatic precipitator.  It would be  virtually impossible to
remove these particles from any filter media, and, at a rate of 1.3 million
cubic  feet per day, the quantity of filter media required would be unfeasible.
In the design of the  electrostatic precipitator it was decided to make two
compromises.

     (1)  The voltage  was to be maintained at less  than 8000 volts in order to
         minimize 03  formation.
     (2)  The precipitator  was  to be overdesigned in order to compensate for
         the low voltage,  yet  maintain a high collection efficiency.

     The precipitator was  designed so that the plates could be removed for
cleaning.  Also they  were  constructed of high purity Al in order to minimize
sample contamination. The impactor plates were Teflon coated to reduce any
possibility of sample contamination.

     Figure 4 is a schematic drawing  of this sampler.  The figure shows the
scalping stage to remove the extremely large particles, the two impactor
stages and  the high efficiency electrostatic collector.

     The sampler utilizes  inertial impaction to obtain the desired size
classification.  Both the  primary cutoff  size of  3.5 ym and the secondary size
of about 1.7 ym use multiple long slits  for the plate-type orifice.  The slits

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                                                       SCALPING STAGE,
                                                        CUT OFF ^20 M
                                                   3.5/Lt STAGE

                                                   = 1.7u STAGE
                                                   ELECTROSTATIC
                                                   PRECIPITATOR
Figure  4.  Prototype of high-volume air sampler.
                          15

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are 1/4 x 1 inch and 1/16 x  1  inch,  respectively.   Calibration tests show that
the impaction parameter ¥  for 50 percent collection efficiency is equal to
0.39 for both slits using the  desired cutoff size  of droplets of unit density.
(The symbol ¥  is a dimensionless parameter which  characterizes the impaction
process of particles impinging on a  surface after  being accelerated from a
jet.)  Gussman, et al., obtained the same impaction parameter for Stage 2 of a
slit width of 1/4 inch or 0.63 cm.   Figure 5 .shows an impaction efficiency
curve obtained in calibrating  the 1/4-inch (0.63-cm) wide slit and similar
data obtained by Gussman.  This curve shows that both experimentalists achieved
similar results.  These data,  presented as collection efficiency versus parti-
cle size, yield a curve very similar to the HASL curve for respirable aerosols.
      The  electrostatic precipitator assembly was redesigned to provide for
removable rather than fixed collector plates so that the collected sample can
             O GUSSMAN
             O BATTELLE
                                                       0.5    0.6   0.7   0.8  0.9  1.0
                                   p  )  Dp. IMPACTION PARAMETER
              Figure  5.   Impaction efficiency curve for slot jet.

                                       16

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be removed more readily.  Very pure Al (99-99 percent) was selected as the
optimum material for the precipitator collection plates.  The selection of
Al was based largely on the factors that Al can be obtained in pure form and
the possible small contamination incurred in removing particulate collections
from the Al substrate should not materially affect the analysis.  The possible
choices of noble and precious metal surfaces were rejected due to costs and
because of the EPA interest in monitoring catalytic converter exhaust emission
pollutant species.

     As designed, the full-scale samplers occupy a floor space of about 32 x
U8 inches with a power requirement of 110 volts and 20 amperes.

Construction of Samplers, Calibration and Laboratory  Trials

     With preliminary calibrations completed, detailed layouts and engineering
drawings were made for the samplers' construction.   Two were built.   Detailed
engineering drawings and a list of purchased items  are to be included in a
companion article to this publication.  This subsequent publication presents
revisions to the sampler and final commentary, suggestions and instructions for
its construction.  The samplers were assembled and tested.  The design
characteristics were for a total pressure drop of about 3 1/2 inches of water
through the impactor stages.  This, coupled with pressure drop through the
entrance and exit, should have produced a total pressure drop of 5 inches
at a flow of about 900 cfm using a 1-hp high efficiency blower.   On test it
was found that the total  Ap was 6 3/8 inches with  over half produced by the
exit plenum.  Flow straighteners were built in to eliminate this defect, and
the total   Ap was k 7/8 inches at cfm.

     The samplers were challenged using a fluorescent aerosol with a mass  mean
diameter, of 6.5  ym.  It was found that 90 percent  of this aerosol deposited
on the first stage and the penetration through the  electrostatic precipitator
stage was less than 0.01 percent.

     Initial laboratory tests of the samplers showed good mechanical and
electrical component reliability.  In later testing high voltage leaks occurred
                                     17

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in the electrostatic precipitator  section.   After checking,  this was attributed
to moisture pickup of the red  fiberboard insulating material used to hold the
electrostatic plates in place.   This material was replaced with Teflon,  and on
further testing no further  leakage problems occurred.

Field Site Application

     The initial  field site application of the sampler(s)  was carried out
during the period September 6  through  13, 1974,  at the Los Angeles Catalyst
Study  (LACS) site.  Two samplers were  taken as cargo on the  same commercial
air flight as carried the Battelle sampling and engineering  team.  Those were
set up the same day as departure at Sites A (upwind) and C (downwind).  They
were operated at  approximately road level.

     After a preliminary 2-day run to  observe loadings obtained at these
sites, a 4-day sampling effort was performed.  During that period the particu-
lates were removed from the first  and  second impactor stages each day.  The
particulates on the electrostatic  plates were allowed to accumulate for  the
entire 4-day period and subsequently were removed at Battelle Columbus Labora-
tory  (BCL).  The  approximate masses obtained during this period are given in
Table  1.
SITE LOCATION
SITE A
(UPWIND)
SIZE FRACTION
3.5-20 Mm (1ST STAGE)
1.7-3.5 /urn (2ND STAGE)
< 1.7 /urn (ELECTROSTATIC PLATES)
TIME PERIOD
~4 DAYS (100 hr)
~4 DAYS (100 hr)
~4 DAYS (100 hr)
MASS.g
1.440
0.845
3.370
TOTAL 5.655
SITEC
(DOWNWIND)
3.5-20 jum (1ST STAGE)
1.7-3.5 fan (2ND STAGE)
<1.7 jum (ELECTROSTATIC PLATES)
~4 DAYS (100 hr)
~4DAYS(100hr)
~4 DAYS (100 hr)
1.245
0.945
4.495
TOTAL 6.685
PERCENT
25.5
14.9
59.6
100.0
18.6
14.2
67.2
100.0
                      Table 1.  Paniculate collection at L.A. site.
                                       18

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     The aerosol at both sampling sites of the massive volume sampler was
sampled with a special cascade impactor developed at BCL for sampling auto-
motive exhaust.  This impactor has a sampling rate of 1.0 cfm and extremely
sharp impactor stages of 0.25, 0.50, 1.0, 2.0, 4.0 and 8.0 ym.  The collections
were made on 2 consecutive days  (not concurrently) and covered approximately a
24-hour period for each run.  The particle size data for this impactor as well
as that obtained from the 100-hour sample collected in the massive volume
impactor are shown in Figures 6 and 7. These data show that the particle size
data obtained by the two impactors agree and that the downstream aerosol is
slightly smaller than the upstream aerosol.  It also shows that between 70 and
80 percent of the particulates are in the respirable size range.

     Vapor phase (chromosorb bed) samplings also were made at each site for
about a 24-hour period each—again, not concurrently.  Analyses of these would
be significant and enlightening for organic compounds which to a certain
extent could be "washed off" the particulates during samplings.  However,
investigation of these vapor phase collections were beyond the scope of this
program.

     The two samplers were operated continuously from the period September 6
through early November, 1974.  During this period, EPA technicians at the
Catalyst Site were instructed to remove the collected particulates each day
from each of the two impactor stages of each sampler.  This procedure should
require no more than a 15-minute period of shutdown for each sampler.  The
electrostatic precipitator should have the capacity to  contain particulates
from up to a month or longer collection time depending on the aerosol concen-
tration.  The removal of particulates from the electrostatic precipitator plates
requires 4 to 8 hours, although it appears that the process could be automated
by use of an ultrasonic bath.

     During the continuous 24-hour operation over a 2-month period,  several
problems, both of an operational and of a sample recovery nature, were observ-
ed.  These were resolved under a program modification effort described later
in this report.
                                      19

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UJ
99


98



95



90



80


70


GO


50


40


30


20
             O HIGH-VOLUME SAMPLER

             O SPECIAL AUTOMOBILE EXHAUST
              IMPACTOR
   10



    5
    2-


    iL
    0.2
               04      0.6   0.8   1            2             4

                         EQUIVALENT PARTICLE DIAMETER, microns
8   10
             Figure 6. Particle size distribution of downwind pollutants at San Diego
             freeway site.
                                         20

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   98


   95


   90
C9
UJ
UJ
   70

   60

   50
>  40

S
|  30


3  20
            D HIGH-VOLUME SAMPLER
            O SPECIAL AUTOMOBILE EXHAUST
              IMPACTOR
   10


    5
    0.2           0.4     0.6    0.8   1            2             46

                         EQUIVALENT PARTICLE DIAMETER, microns

          Figure 7.  Particle size distribution of upwind pollutants at San Diego
          freeway site.
                                                                             8   10
                                        21

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SAMPLE ANALYSIS

     The request to place the two samplers at the LACS Background Site and the
limited funds remaining after the design, construction, and test of the sam-
plers severely limited both the obtaining of multiple samples and the develop-
ment of analytical methodology, initially planned.  However, certain basic
analyses were made to indicate the type of data obtainable by the use of a
massive air volume size-selective collection mode.

Optical Emission Analyses

     Direct current  semiquantitative  analyses results are shown in Table 2.

Chemical Determinations

     Selected metallic elements were  determined by  AA analyses.  Anion, Am-
monium ion (NHij.), and benzene  soluble organic  (BSO) determinations were made
chemically.  Nitrogen  (N)  (ultimate)  and hydrocarbons  (HC) analyses were made
using a Perkin-Elmer Elemental Analyzer.  Total N determinations were made by
Kjeldahl.  These data are  given  in Table  3 on the basis of percent in the
fraction collected.  Quantitative recoveries of the collections were not made
so TSP values are not given.   Hi-vol  values taken frequently at the Catalyst
Site show  daily variations from  60 to 150 yg/m3.  From the tabular data, the
following  are indicated:
     (1)  Based on Lead  (Pb) determinations there  is a traffic effect seen in
         the downwind samples.
     (2)  The Iron  (Fe) contents  in the several sizes decrease with decreasing
         size.   Similar  decreases were found by optical emission spectrography
         for several other elements,  generally of crustal origin.
     (3)  S and BSO,  on the other hand, increase in  concentrations in the finer
         size fractions.
     (4)  Sulfate  (SO^) accounts  for most  of the total S in the two larger size
         fractions.  The SO^  to  S ratio plus the  total S versus S after
         benzene extraction indicate  the possibility of organo sulfur compounds
         accounting  for  up to 1  to 2  percent of the total S in the <1.7- urn
         fractions.
                                       22

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ro
U)

SAMPLE DESIGNATION
UPWIND
1ST STAGE
2ND STAGE
ELECTROSTATIC
DOWNWIND
1ST STAGE
2ND STAGE
ELECTROSTATIC
ELEMENTS DETERMINED, percent
Al

10
5
5

10
5
5
Ba

0.01
0.01
<0.01

0.01
0.01
<0.01
Ca

5
5
1

5
5
1
Cr

0.01
0.01
0.02

0.01
0.01
0.02
Co

<0.01
<0.01
<0.01

<0.01
<0.01
0.01
Cu

0.5
0.5
1.0

0.5
0.5
1.0
Fe

5
3
1

5
3
2
Pb

1
1
1

1
3
3
Mg

3
3
1

3
3
1
Mn

0.1
0.1
0.1

0.1
0.1
0.2
Ni

<0.01
<0.01
<0.01

<0.01
<0.01
0.01
K

3
3
3

3
3
4
Si

15
15
10

15
10
10
Na

2
2
2

2
2
2
Ti

0.5
0.5
0.5

0.5
0.5
0.5
V

0.02
0.02
0.03

0.02
0.02
0.05
Zn

0.05
0.05
0.1

0.05
0.1
0.1
                                     Table 2. Semiquantitative optical.emission analyses for metals.

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10

SAMPLE DESIGNATION
SITE A 1ST STAGE
UPWIND 2ND STAGE
ELECTRO-
STATIC
SITEC 1ST STAGE
DOWNWIND 2NDSTAGE
ELECTRO-
STATIC
DETERMINATION

Pb
0.86
1.13
0.93
2.43
3.16
3.74


TOTAL S
2.0
5.6
8.7
[8.9] (b)
2.0
4.7
5t5


Fe
3.6
2.9
1.0
3.8
3.1
1.9

BENZENE-
SOLUBLE
ORGANICS
8.0
9.0
16.6
4.3
8.8
16.0


S
2.4
6.5
9.4
1.9
5.2
6.1


S04=
6.45
16.8
21.3
6.3
14.6
17.4


C
7.3
7.9
6.5
8.6
10.6
9.4


H
1.5
2.4
4.3
1.7
2.3
3.4


N
2.2
2.5
3.1
1.9
2.3
2.5


N03'
7.75
2.85
6.5
7.4
5.5
3.0


NH4+
0.87
2.55
3.55
0.69
2.17
245

             RAFTER BENZENE EXTRACT.
             (b)RECHECK DETERMINATION.
               Table 3.  Analyses of collected particulates from LA. background catalyst study site - results in percent.

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     (5)  The nitrite  (NOa) form accounts  for ^70 percent of the total nitrogen
          (N) found in the large particle  size while NHt^ accounts  for ^75
         percent of the total N found in  the fine  fractions.

X-Ray Diffraction

     Diffraction patterns were obtained by the first stage  (>3.5  ym) and
electrostatic precipitator (<1.7 ym) fractions both upwind and downwind.  The
patterns are shown in Figures 8a, b, c, and d.  Detailed data interpretations
of the patterns were not made.  However, pattern differences can  be detected
visually.  Note the greater complexity of the fine versus the coarse particle
size fractions and the relatively more complex structure of the downwind
fractions.  Because of the complexity of air particulate compositions, full
exploitation of the XRD technique generally would require the use of frac-
tional separation techniques prior to taking of the patterns and  computer data
search.  Organic fraction removal, magnetic fraction separation,  water-soluble
fractionation and density separations are among the techniques which can be
used to obtain more definitive diffraction data.  The availability of large
sample amounts permits this type of exploration to be done while  still having
adequate sample for other compound identification efforts.

Organic Species Identification

     Each of the three fractions of Santa Monica Freeway particulate was
subjected to methylene chloride extraction, and a preliminary survey for an
appropriate GC column was carried out.  It was quickly evident that exceed-
ingly complex mixtures of organic compounds were present, and that it may not
be feasible to attempt a comprehensive analysis on one GC column alone.   A
polar high resolution column (25 ft, 3 percent Silar 5CP) was chosen as being
the most suitable for resolution of most aliphatic and smaller aromatic mate-
rials.  It is anticipated that PNA species can be analyzed without difficulty
using a Dexil 300 column preceded by isolation of the species of  interest by
the Rosen liquid chromatographic separation.

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                 A. UPWIND >3.5Atm FRACTION
                  B. UPWIND <1.7/im FRACTION
                C. DOWNWIND >3.5/jm FRACTION
                 D. DOWNWIND < 3.5 p.m FRACTION
FigureS.  X-ray diffraction patterns of 4-day (lOOhr) collections.


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     Preliminary analyses indicate that the great majority of organic materials
are found in the two smallest size fractions.  These latter  fractions exhibit
many similarities in organic composition, although there do  appear to be
several possible significant differences.  The largest size  fraction  (>3.5 ym)
is quite different from the smaller two, and shows none of the low molecular
weight polar species which they exhibit.  An envelope of unresolved high
molecular weight compounds is common to all these fractions, but is more
abundant in the small size fractions.  This unresolved envelope appears to
consist of a highly complex mixture of approximately Ci2 to  039 aliphatic HC
isomers.

     Gas chromatographic mass spectrometric analysis was carried out using
both electron ionization and chemical (methane) ionization spectra—the
chemical ionization spectra almost always give invaluable molecular weight
data, and the characteristic fragmentation is often sufficient to make a
reliable molecular assignment when coupled with GC data.  Electronization
could be additionally carried out in order to gain further structural data
from the more extensive fragmentation.

     Considerable spectra detail was obtained,  but an intensive spectral
matching computer search was not completed.   The spectra have been reserved
for interpretation under an anticipated extension of the present program.

                 SAMPLER AND COLLECTION PROCESS MODIFICATIONS

     The two Massive Air Volume Samplers proved suitable in their performances
during tests carried out in the laboratory and during the initial 2-day and 4-
day field tests at the LACS Site.   During these periods the samplers were
operated and the particulate collection was recovered by Battelle personnel.
As stated earlier, the program plans initially had called for relatively
short-term (days) sampling at various CHESS sites by Battelle personnel and
detailed analyses of the collected samples.

     The unplanned requests that the samplers be left at the Background
Catalyst Study Site for continuous (years) 24-hour operation by technicians
                                     27

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not familiar with the sampler construction, assembly detail, and sample recov-

ery process brought about needs to improve the structural stability of the

samplers and to modulize the collection assemblies.  These needs were discussed

with the EPA Project Officer and increased time and funds were approved for
the following changes.


    (1)  Detailed engineering changes were made to provide for additional
         structural stability to the Impactor Plate Assembly and Electrostatic
         Plate Assembly holders.  The changes accommodated for both materials
         of construction changes and machining and assembly tolerances.

    (2)  Four Impactor Plate Assembly holders were constructed using Al metal
         coated with Teflon.  These replaced the  two holders presently in
         place in the samplers  (one in each) made from red fiberboard
         construction.  The availability of two holders for each sampler would
         provide a simplified and contaminant-free mode of replacing the two
         impactor plates and two impactor slit stages  when they are loaded
         daily with collected particulates.  The  sampler operator  simply can
         remove the impactor plate holder module  which contains collected
         particulate and slide  in a fresh unit to provide for essentially
         continuous operation.

    (3)  Two additional electrostatic plate assembly holders were  constructed
         using strengthened design features.  The two  present holders in the
         samplers were similarly strenghthened in design.  Again,  the avail-
         ability of modulized replacement of particulate-laden plates with
         cleaned plates would ensure contamination-free handling and provide
         essentially continuous collection.
    (4)  Two freight shipping boxes for the electrostatic plate holder assembly
         and plates were constructed.  Since the  electrostatic plates  (47 in
         each sampler) can accumulate up to 1 month of urban aerosol sampling
         and since the particulate removal from the same 100 ft2 of collector
         surface is lengthy and tedious, it was deemed useful to be able to
         ship these to a clean, well-equipped laboratory for sample recovery,
         cleaning, and subsequent reuse in the sampler. With the  shipping
         boxes the plates  could be air freighted  to Research Triangle Park,
         North Carolina, Battelle, or elsewhere.
    (5)  Air volume flow and electrostatic precipitator meters were installed
         for ready check on the samplers performance.
                                      28

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                                  SECTION IV

                                  DISCUSSION

     Based on the results achieved at this stage, the program efforts show
that a long-needed sampling and analysis technology can be fulfilled.  Through
collection of a large mass of sample on a size basis, thorough characteriza-
tion of respirable range particulates can be made and thus good correlations
between particulate burden and health effects are attainable.  The applica-
tions of the system are many.  The samplers could be utilized at the several
CHESS sites where the health effects of populations are already under study.
Point source emissions could be monitored by taking upwind and downwind samples.
If the sampler developed under this program, together with a thorough ana-
lytical survey of the collected respirable size fraction, were coupled with
a gas phase sampling and analysis system it would be possible to obtain a
total knowledge of the airborne health threat posed to a given population
group.  Such knowledge is needed for useful and meaningful health/pollution
burden studies.

     The design and construction aspects of the program entailed greater
efforts than originally anticipated.  This coupled with an urgent need by
EPA for the samplers to be placed at the Background Catalyst Study Site
precluded the obtaining of more thorough data on collection efficiency and
precision as well as checking the possibility of chemical reaction due to 03
formation in the electrostatic precipitator section of the sampler.

     Additionally further isolation and identification of suspect compounds
are needed.  The identification and exploration of pathways to quantitative
assessment of the oxidized sulfur species which give rise to adverse health
                                      29

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effects have been correlated with sulfate ion concentrations found in the
water extract of particulate matter collected on glass-fiber filters.  These
identifications have been and remain a primary target for our investigations.
                                       30

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                                  APPENDIX A
                  OPERATIONAL AND PROCEDURAL DESCRIPTION  OF
                          MASSIVE AIR VOLUME SAMPLER
GENERAL DESCRIPTION OF MASSIVE AIR VOLUME SAMPLER

     The Massive Air Volume Sampler is designed to pull a very large volume
of air, M.OO ft /min, through the sampler system and to collect particulates
in three size ranges.  The first two size ranges of 3.5 to 20 ym and 1.7 to
3.5 ym are collected by a two-stage impactor system housed in an impactor
assembly module, and the third size range, <1.7 ym, is collected by a high-
efficiency electrostatic precipitator.  In use, for urban aerosol collection,
the particulates should be removed from the impactor plates daily and from
the electrostatic plates about monthly.  These time periods will vary depend-
ing on the particulate burden of the air being sampled.

     Viewing Figure A-l, the air inlet is through the 2-inch slot (covered
by a fine mesh screen to repel insects) seen near the top of the assembly.
The impactor assembly is in a drawer, closed by snaplocks on either side of
the sampler just below the air inlet.  (Only one upper snaplock can be seen
in the Figure.)  The electrostatic assembly is located just below the impactor
assembly.  Again, it is closed by snaplocks, only one of which can be viewed
in Figure A-l.  The motor and motor housing is in front of the sample col-
lector with the egress air outlet seen pointing left.   The intake to the
motor housing, of course, must be closely fitted to the sampler collector
so that no air loss occurs between the sampler and the motor housing.  A flow
meter and electrostatic voltage meter are provided as a check on the opera-
tional performance of the sampler (Figure A-2).
                                      31

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Figure A-1. Overall photograph of massive air sampler.
                       32

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Figure A-2.  Lower part of massive air sampler showing flow meter, electrostatic
power unit, and voltage meter.


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     The particulate collections of course should be kept separate when

recovered.  They should be placed in large opaque containers  (Teflon is
preferred) according to stages:

         First Stage, Impactor - Size 3.5-10 ym

         Second Stage, Impactor - Size 1.7-3.5 ym

         Third Stage, Electrostatic Precipitator - Size <1.7  ym.


Refrigeration is recommended to minimize possible chemical interaction.  Two

impactor assembly modules and two electrostatic precipitator  assemblies are
provided with each sampler.


     In operation the sequence of sample collection is as follows:


      (1) Shut off power to the motor blower and to the electrostatic
         precipitator—generally every 24-hour period.
      (2) Remove the impactor plate assembly from the sampler  and take
         to a clean area or place in the impactor assembly shipping box.

      (3) Install a second impactor plate assembly having cleaned  (parti-
         culate removed—not washed) plates.

      (4) start up the sampler again.

      (5) in a clean area, remove the collected particulates from the
         impactor plates and replace the plates in the assembly for
         reinstallation and collection in the sampler.  The objective
         of this operation  (which is repeated daily) is to prevent
         excessive particulate buildup on the impaction plates which
         could be blown off resulting in improper size fractionation.
         Do not wash or excessively scrub the particulates from the
         plates.  Repeated collection and removal will result in
         nearly total recovery over a time period.
      (6) The electrostatic assembly sample recovery should follow the
         same general procedure as above, except the assembly will be
         changed only about once a month.  The recovery of particulates
         from the 47 plates or about 100 ft2 of surface will  require up
         to an 8-hour period.  It is recommended that at least each month
         the electrostatic assembly containing the loaded plates be placed
         in the shipping box provided and be sent to a well-equipped clean
         laboratory for particulate recovery, reinstallation  of the 47
         plates, and reshipment to the field collection site.

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OPERATIONAL GUIDE
Setup of Sampler System


     It is assumed in this description that no electrical connections have

been made and that the impactor plate assembly and electrostatic precipitator

assembly are not in place in the sampler.


     (1) Select a location to provide intake air at the desired vertical
         level.  Keep in mind that the egress air flow is of very high
         volume and may resuspend particulates which could get into the
         ingress air stream.  A large sheet of plastic spread below the
         sampler base can minimize this problem.  In Figure A-l, the
         sampler and blower are seen fastened to a large sheet of ply-
         wood.

     (2) The base on which the sampler and blower motor are placed should
         be approximately level.  The weight of the sampler and blower motor
         is about 500 pounds.

     (3) Secure the sampler and blower motor independently to the base to
         minimize movement during operation.  There are bolt holes pro-
         vided for this as seen in Figure A-2.  Prior to fastening, be
         certain that the blower motor housing inlet is in alignment and
         snugly fitted to the bottom sampler air fitting.  The sampler
         should also be positioned so that the high velocity blower ex-
         haust is not deflected back into the sampler inlet.

     (4) Install impactor plate assembly (Figures A-3 and A-4).   Open the
         two snapfasteners located near the top of the sampler and raise
         the door opening.  Remove the impactor assembly from shipping box
         and carefully slide the impactor assembly (Figure A-3)  into the
         opening.  NOTE:  The impactor assembly may be already in place in
         the sampler.  In that event it may be useful to check that the four
         plates are correctly oriented as follows:

         (a) The impactor assembly consists of a unit Teflon "box" containing
             four sets of machined grooves into which are fitted four Teflon-
             coated (green)  stainless steel plates.   It is important that
             these plates be in the right sequence and proper alignment,
             both in the initial setup and in subsequent collections.  The
             proper impaction plate sequence is as follows:
                         (a)
         Plate   Position      Slit Width, in.            Purpose

           1        Top            1/4         Stage 1 Jets

           2        2nd            3/8         Stage 1 Impaction Plates

           3        3rd            1/16        Stage 2 Jets

           4        Bottom         1/8         Stage 2 Impaction Plates


                                      35

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Figure A-3. Impactor plate assembly module, partially withdrawn.
                             36

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Figure A-4. Closeup of impactor plate assembly (upper) and electrostatic precipitator
(lower) closed drawer compartments.

-------
        It is also necessary that the slits for all four plates run in
        the same direction (preferably perpendicular to the axis of the
        electrostatic precipitator plates).

(5)  Install the electrostatic assembly (see Figures A-3 and A-5) by
    (a)  similarly opening the two snaplocks located on either side near
    the bottom of the sampler, (b) opening the precipitator door, and
    (c)  carefully sliding the electrostatic assembly into place.  Again,
    the assembly may already be in place.   Do not lift using the handle
    seen on the front.  It will not support the weight of the precipi-
    tator plate assembly.  The purpose of the handle is to be able to
    pull the precipitator plate assembly out of the sampler far enough
    so that it can be lifted from underneath.  After the precipitator
    plate assembly is placed completely within the sampler, it will
    then be possible to close the precipitator door and lock it with the
    two snap connectors.

(6)  The electrostatic precipitator plate assembly has a male banana plug
    which extends through the precipitator door.  High voltage is sup-
    plied to the precipitator plates by means of an insulated female
    portion of the plug which is connected to the power supply.  Connect
    the male and female plug together.

(7)  After completion of the above steps the sampler is ready to be con-
    nected to an electrical outlet.  It is recommended that both the
    blower and precipitator be connected to a 100 volt duplex plug from
    a single outlet with a capacity of at least 15 amps.  It is also
    recommended that an electric clock be plugged into the same circuit
    in order to check on electrical outage.

(8)  After both the blower and precipitator power supply have been con-
    nected, check to ensure that both are functioning properly.  The
    switch on the precipitator power supply should be turned on and the
    voltmeter should read approximately 800.  (Actual voltage to the
    precipitator plates is about 7800 as the voltmeter has a voltage
    divider with a factor of 10 located in its input.)  If the volt-
    meter reads substantially below 800, there is a short in the system—
    either the precipitator plate assembly or the ionizer section.  These
    can be isolated by disconnecting the banana plug at the precipitator
    door.  The problem should be readily discernable as the high voltage
    will arc at the trouble point.  The high volume blower will essen-
    tially provide a constant volume flow through the sampler unless
    there is an extremely low voltage input.  A magnehelic pressure
    gauge is attached to the blower to indicate total flow and should
    read at least 5 inches of water.
(9)  Daily Change of Impactor Assembly and Recovery of Impactor Collec-
    tions .*  Remove the entire Impactor Assembly unit by opening the
    snaplocks at the top of the sampler and opening the door.  Using
    the knurled screws, partially withdraw the unit until it can be
    grasped at the bottom with two hands for final withdrawal.  Take
    to a clean area for sample recovery.   (NOTE:  The second impactor
    assembly can be put in place and the Sampler system restarted.)
                                 38

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Figure A-4. Closeup of impactor plate assembly (upper) and electrostatic precipitator
(lower) closed drawer compartments.

                                  37

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        It is also necessary that the slits for all four plates run in
        the same direction (preferably perpendicular to the axis of the
        electrostatic precipitator plates).

(5)  Install the electrostatic assembly (see Figures A-3 and A-5) by
    (a)  similarly opening the two snaplocks located on either side near
    the bottom of the sampler, (b) opening the precipitator door, and
    (c)  carefully sliding the electrostatic assembly into place.  Again,
    the assembly may already be in place.  Do not lift using the handle
    seen on the front,  it will not support the weight of the precipi-
    tator plate assembly.  The purpose of the handle is to be able to
    pull the precipitator plate assembly out of the sampler far enough
    so that it can be lifted from underneath.  After the precipitator
    plate assembly is placed completely within the sampler, it will
    then be possible to close the precipitator door and lock it with the
    two snap connectors.

(6)  The electrostatic precipitator plate assembly has a male banana plug
    which extends through the precipitator door.  High voltage is sup-
    plied to the precipitator plates by means of an insulated female
    portion of the plug which is connected to the power supply.  Connect
    the male and female plug together.

(7)  After completion of the above steps the sampler is ready to be con-
    nected to an electrical outlet.  It is recommended that both the
    blower and precipitator be connected to a 100 volt duplex plug from
    a single outlet with a capacity of at least 15 amps.  It is also
    recommended that an electric clock be plugged into the same circuit
    in order to check on electrical outage.

(8)  After both the blower and precipitator power supply have been con-
    nected, check to ensure that both are functioning properly.  The
    switch on the precipitator power supply should be turned on and the
    voltmeter should read approximately 800.  (Actual voltage to the
    precipitator plates is about 7800 as the voltmeter has a voltage
    divider with a factor of 10 located in its input.)  If the volt-
    meter reads substantially below 800, there is a short in the system—
    either the precipitator plate assembly or the ionizer section.  These
    can be isolated by disconnecting the banana plug at the precipitator
    door.  The problem should be readily discernable as the high voltage
    will arc at the trouble point.  The high volume blower will essen-
    tially provide a constant volume flow through the sampler unless
    there is an extremely low voltage input.  A magnehelic pressure
    gauge is attached to the blower to indicate total flow and should
    read at least 5 inches of water.
(9)  Daily Change of Impactor Assembly and Recovery of Impactor Collec-
    tions .*  Remove the entire Impactor Assembly unit by opening the
    snaplocks at the top of the sampler and opening the door.  Using
    the knurled screws, partially withdraw the unit until it can be
    grasped at the bottom with two hands for final withdrawal.  Take
    to a clean area for sample recovery.   (NOTE:  The second impactor
    assembly can be put in place and the Sampler system restarted.)
                                 38

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Figure A-5.  Electrostatic precipitator assembly, partially withdrawn.
                              39

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    Using  a large  Allen wrench remove the four Allen-head screws seen
    at  the four corners of the assembly—Figure A-4.   Disassemble and
    clean  the plates in the following sequence:

     (a)  Top Plate.   Using plastic throw-away gloves,, withdraw the top
         slot guide plate and place on a clean sheet of aluminum foil.
         There should be little if any collection on this guide plate.
         Brush any  particulate onto a small square or tray of aluminum
         foil and then place the collection, if any, into a sample col-
         lection bottle labeled "1st Stage."  Set the cleaned plate aside
         for subsequent reinstallation (in the same position and slot
         orientation) in the Assembly unit.

     (b)  Second  Plate (1st Stage Collector).  Repeat as described above.
         This plate should contain a fairly even load of particulates.
         Brush and/or loosen lightly using a Teflon coated knife or tool.
         There is no need to excessively scrape or abrade to obtain a
         total 100  percent recovery since the operation will be repeated
         approximately daily.  Recover the particulates and place them
         in the  sample bottle marked "1st Stage."  Place the plate aside
         for reinstallation.

     (c)  Third Plate.  This is the slot plate for the second impactor
         stage assembly.  It should contain very little collection.
         Treat as with (a) above but place any collections in a sample
         bottle  marked "2nd Stage."

     (d)  Fourth  Plate.  This plate contains the second stage impactor
         collections.  Treat as with (b) above but add the collections
         to the  sample bottle marked "2nd Stage."  Reinstall the four
         plates  in  the order and orientation they were removed.  (See
         Instruction 4 above.)

(10) Bimonthly or Monthly Change of Electrostatic Assembly.

     (a)  Turn off power supply switch and disconnect electrical connec-
         tion (banana plug) to electrostatic precipitator.  (See Figure
         A-3.)  Open the two snaplocks and raise the metal drawer door.
         Using the  pull handle on the front of the assembly (Figure A-5)
         partially  pull the assembly out to the point where the assembly
         can be  lifted.  Do not lift using the pull handle.
     (b)  Place the  Electrostatic assembly with the particulate-laden
         plates  in  the shipping boxes provided.

     (c)  Install the second Electrostatic assembly; connect the electro-
         static  electrical power connection (banana plug) and turn on
         power supply switch.
(11) Recovery of Sample Collection from Electrostatic Plates.   Open the
    shipping box and remove the electrostatic assembly in a clean area.
    Remove the  plates individually, place on a clean subsurface such
    as  aluminum wrap and remove the collected particulates by scraping
    both sides  of  each plate with a sharp-edged Teflon spatula.  Using
    a clean lab brush, brush the particulates into a sample bottle
    labeled electrostatic precipitator catch.

                                  ko

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After recovery of the sample, scrub the plates clean using a
detergent and fine abrasive powder, rinse with deionized water,
dry, and reinstall the plates back into the electrostatic assembly
according to the following procedure.

The precipitator plate assembly is designed so that every other
plate is either at ground potential or connected to the high voltage
potential.  Thus, in order that the individual plates can be inter-
changeable they are notched at the bottom corner, so that there will
not be a direct short across the two buss bars.  The first plate
should be installed so that the unnotched corner slides into a small
clip attached to the buss bar and the notched corner does not touch
the buss bar on the opposite side.  Each additional plate is placed
in the same manner and the notches will be opposite each other.

After all the plates have been installed, place the assembly into
the shipping box and ship back to the sampling site.
                             Ul

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                                  APPENDIX B


           LIST OF ATTENDEES OF AEROSOL SAMPLING TECHNOLOGY MEETING


     A meeting was held December 11, 1973, at Research Triangle Park to dis-

cuss, review, and obtain a consensus of opinion from EPA personnel and lead-
ing experts in the field on the proposed sampler designed to duplicate the

HASL or ACGIH collection efficiency for respirable particulates recommended

by the ACGIH Threshhold Limits Committee.  The curve has been well defined
by respiratory physiologists and has a cutoff size  (50 percent collection of
3.5 ym).  The design was considered within the parameters of collection of

gram quantities of ambient air particulates in a 24-hour period with minimal

substrate interference, low power requirements, and portability.  The meeting

was attended by the following:


              Name                          Affiliation

         Morton Lippman                New York University
         Harry Ettinger                Los Alamos Science Laboratory
         T. T. Mercer                  University of Rochester
         R. J. Thompson                EPA
         Elbert Tabor                  EPA
         J. H. Knelson                 EPA
         A. V. Colucci                 EPA
         S. Simione                    EPA
         Bob Burton                    EPA
         Walter Crider                 EPA
         W. Wilson                     EPA
         W. Gary Eaton                 EPA
         R. I. Mitchell                Battelle Columbus Laboratories
         W. M. Henry                   Battelle Columbus Laboratories

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                                    TECHNICAL REPORT DATA
                             (Please read Instructions on the reverse before completing)
1. REPORT NO.         ^
       EPA  -600/4-7K-009
                              2.
                                                            3. RECIPIENT'S ACCESSION-NO.
4. TITLE AND SUBTITLE
      Development of a  Large Sample Collector of
      Respirable Particulate Matter
             5. REPORT DATE
                 November 1977
             6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
       W.  M. Henry and  R.  I.  Mitchell
       (Battelle Laboratories)
                                                            8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS

       BatteHe Laboratories
       Columbus, Ohio   43201
              10. PROGRAM ELEMENT NO.

               1A1005  and   1A1001
              11. CONTRACT/GRANT NO.
               68-02-0752
12. SPONSORING AGENCY NAME AND ADDRESS

       Environmental  Protection Agency
       Research Triangle Park, NC   27711
              13-TYPE OF REPORT AND PERIOD COVERED
                          6/14/73 to 4/13/75
                          AGENCY CODE
                                                              EPA-ORD
15. SUPPLEMENTARY NOTES
16. ABSTRACT
       A prototype  sampler designed  to  collect particulate matter from  air in sized
       fractions has  been designed and  tested.  The  sampler excludes  particles above
       20 ym in diameter and collects fractions centered at 3.5 pm and  1.7 ym on
       impaction plates and smaller  particles by electrostatic precipitation.  The
       report includes test data, engineering drawings  and materials  list.
17.
                                KEY WORDS AND DOCUMENT ANALYSIS
                  DESCRIPTORS
                                               b.lDENTIFIERS/OPEN ENDED TERMS
                           c.  COSATI Field/Group
       Sized  Fractionation of  Particulate
       Matter,  Respirable, Photochemical,
       Fine Particulate, Massive Volume
       Sampler
                             13B

                             14G
18. DISTRIBUTION STATEMENT
       RELEASE TO PUBLIC
19. SECURITY CLASS (ThisReport)
  UNCLASSIFIED
                                                                          21. NO. OF PAGES
                                               20. SECURITY CLASS (Thispage)

                                                 UNCLASSIFIED
                           22. PRICE
EPA Form 2220-1 (9-73)

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