United States
                     Environmental Protection
                     Agency
                     Research and Development
Atmospheric Research and
Exposure Assessment Laboratory
Research Triangle Park NC 27711
EPA/600/S3-91/071 Jan. 1992
w EPA       Project Summary
                     Superfund  Innovative  Technology
                     Evaluation, The  Delaware  SITE
                     Study,  1989

                     W.A. McClenny, G.M. Russwurm, M.W. Holdren, A.J. Pollack, J.D. Pleil,
                     J.L. Yarns, J.D. Mulik, K.D. Oliver, R.E. Berkley, D.D. Williams
                     K.J. Krost, and W.T. McLeod
                       The Delaware SITE (Superfund Inno-
                    vative Technology Evaluation) Study
                    was carried out by personnel from the
                    Atmospheric Research and Exposure
                    Assessment Laboratory (AREAL), U.S.
                    EPA, and AREAL contractors, Battelle
                    Columbus Laboratory,  ManTech Envi-
                    ronmental Technology, Incorporated
                    (formerly NSI Environmental Sciences),
                    and Tecan Remote, Incorporated. Per-
                    sonnel of the Delaware Department of
                    Natural Resources and Environmental
                    Control (DNREC) hosted the operation
                    and obtained permission to use local
                    sites for monitoring. The objective of
                    the study was to field test several moni-
                    toring methods that have progressed
                    through a feasibility testing stage and
                    appear ready for predemonstration test-
                    ing at Superfund sites. Monitoring  oc-
                    curred near four Superfund sites in the
                    vicinity of New Castle, Delaware, and at
                    the Delaware Reclamation Plant located
                    just north of the  Delaware Memorial
                    Bridge. Several  different types of new
                    monitoring equipment were deployed
                    including: (1) automated gas chromato-
                    graphs, (2) canister-based sequential
                    samplers, (3) personal sampling de-
                    vices, (4) canister-based  sector sam-
                    plers, (5) long path infrared transmission
                    monitors, and (6) solid sorbent-based
                    phenolic compound samplers.
                       This Project Summary was devel-
                    oped by EPA's Atmospheric Research
                    and Exposure Assessment Laboratory,
                    Research Triangle Park, NC, to an-
                    nounce 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 Superfund Innovative Technology
 Evaluation (SITE) Program promotes the
 development, acceptance, and use of prom-
 ising innovative technologies capable of
 meeting the objectives of the overall Su-
 perfund program. One objective of the pro-
 gram is to provide the means for developers
 of technology to demonstrate innovative
 technologies at Superfund sites as alter-
 natives to the systems currently in  use. A
 second objective is to provide support to
 stimulate the development of promising
 concepts and technologies to the point
 that they are suitable for demonstration at
 Superfund sites. In the case of the Dela-
 ware SITE program, a proposal was made
 by AREAL to the SITE program coordina-
 tor to carry out predemonstration testing of
 new monitoring techniques. After accep-
 tance, a schedule was established for the
 testing in the summer  of 1989.       (
   The schedule of the SITE project con-
 sisted of the following  items:
    Selection of a field site
    Predemonstration plan preparation
     a. Planning/coordination meeting
       with participants, and
     b. Preparation   of  plans  for
       predemonstration testing.
       1.  Documentation of experimen-
          tal design, and
       2.  Preparation and clearance of
          a quality  assurance plan.
    Preliminary field screening study
    Preparation of a target compounds
    list for each test site
                                                                     Printed on Recycled Paper

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 •    Performance of the field testing
 •    Review of data and preparation of a
     highlight report
 •    Presentation of  preliminary data at
     the 1990 EPA/AWMA Symposium on
     Measurement of Toxic and Related
     Air Pollutants
     Development of information products
     for the SITE program
   The site proposed by J.J. Kliment of
the Delaware Department of Natural Re-
sources and Environmental  Control
(DNREC) was selected. The site was near
New Castle, Delaware, and included four
Superfund sites and one site near the Dela-
ware Reclamation Plant. A map of all the
sites is shown in Figure 1. Figure 1  shows
the Superfund sites:  Army Creek,  Dela-
ware Sand  and Gravel, Halby, and Stan-
dard Chlorine along with the Pigeon Point
site which is nearthe Delaware Solid Waste
Authority. The location of a monitoring site
in  the residential area  referred  to as
Llangollen Estates and the P4 monitoring
site maintained by the state of Delaware
are also shown. The Standard Chlorine
plant site was part of a large industrial
complex.

Experimental Plan
   The experimental plan called for five
methods of monitoring to be tested in the
field.  An automated  gas chromatograph
(GC) using a solid sorbent to preconcen-
trate volatile organic compounds (VOCs)
from the ambient air was placed in the P4
station. The unit cycled through an auto-
mated sample and analysis sequence ev-
ery hour. The objective of this monitoring
method was to evaluate the use of a solid
sorbent as a  VOC preconcentrator and
further to demonstrate the use of auto-
mated GCs as a means to establish the
variability of VOC concentrations in time.
    The P4 site was  also used for place-
ment of sector samplers. These units were
placed at the P4 and S20 sites to charac-
terize the  industrial complex near Stan-
dard  Chlorine. Data was also taken near
the Army Creek and Delaware Sand and
Gravel site using the sector samplers.
    Personal sampling devices (PSDs) were
used as fenceline dosimeters at several of
the sites. These units sample by diffusion
and are small and convenient to use. Since
the units are less than two inches in diam-
eter, they can be attached to any conve-
nient  structure  and used  to obtain  a
time-integrated ambient air sample. To es-
tablish the validity of the fenceline moni-
tors for screening of  VOCs, they  were
used in side-by-side tests with canisters.
    Long path monitors based on selective
absorption of  infrared  radiation by target
gases were used at four of the sites. The
objective was to define the field capabili-
ties of FTIR-based long  path  monitors.
These monitors use source and receiver at
one end of a monitoring path and a retro-
reflector at the other end. The pathlength
is typically 300 m  long, giving a total
pathlength of 600 m.
   New solid sorbents specifically chosen
for retention of phenolic compounds were
also used at the  Superfund sites.  How-
ever, the field study was intended as a
scoping study in this case since only labo-
ratory studies  had been done  up to this
point.

Results and Discussion
   The  main field study was carried out
during the period 24 July through 9 August
1990 at the Superfund sites as planned.
Individual experiments and experimental
results are summarized below.
Automated Gas Chromatograph
     AREAL's new automated GC using a
     multisorbent bed for preconcentration
     operated  successfully when cycled
     on an hourly basis over two weeks.
     The automated  GC was calibrated
     daily for 12 consecutive days with a
     relative standard deviation (RSD) of
     response that was less than 10% for
     all but dichlorodifluoromethane.
     Use of the automated GC data in the
     Temporal Profile Analysis (TPA) ap-
     proach resulted in the identification
     of groups of compounds  originating
     from nearby sources.
 Fourier  Transform Infrared Long  Path
 System
     An independent calibration of the Fou-
     rier transform infrared (FTIR) sys-
     tem, in which  a mixture  of seven
     gases was presented to the system,
     demonstrated that  the results are
     compound-dependent and differ by 2
     to 35% from the nominal calibration
     standards.
  •  The precision of the FTIR was deter-
      mined by presenting the  same mix-
     ture of gases to the  FTIR on 16
     occasions. The results again show a
     compound dependency,  with  RSD
     values from 4 to 41%.
     The detection  limits of this instru-
      ment are compound-specific but can
      generally range from 20 to 100 ppb.
      The comparison of the  FTIR data
      with the results from the canister tech-
      nique was complicated by the rapidly
      changing concentrations  caused by
      the movement of a small plume of
      industrial emissions  that  touched
      down intermittently along the moni-
      toring path. The comparison for p-
    dichlorobenzene was good, the xe-
    sults of point sampling and long path
    monitoring  being statistically  the
    same. For chlorobenzene, the FTIR
    was operating very close to the theo-
    retical detection limit, and the aver-
    age difference between results was
    34%. The error bars on the FTIR
    data  for this compound  are large
    enough to conclude that  no statisti-
    cal difference really exists.
    Canister  samples taken simulta-
    neously but transported in opposite
    directions along the path show differ-
    ences of up to a factor of 2. Canister
    samples taken simultaneously  and
    side by side in the traversal of the
    path show variabilities of about 15%.
Sector Sampling
    .Sector sampling was used to identify
    the major compounds emitted from
    an industrial complex.
Sequential Sampler
    A  set of  25 compounds was  ana-
    lyzed  by  using the TPA  technique,
    and a subset of these compounds
     showed strong  correlation  (>0.85).
     The air mass  carrying these  com-
     pounds was seen to have  passed
     over the  industrial complex  prior to
     its arrival at the sampler.
Personal Sampling Devices
     Eleven sampling events were moni-
     tored  at three sites,  and data were
     analyzed for six volatile compounds.
     The analysis shows good agreement
     with the canister data. The PSDs can
     be used as fenceline  dosimeters
     around landfills.
Anion Exchange Resin
     This was the first field test of sorbent
     sampling with  anion exchange res-
     ins. The technique was the least de-
     veloped technique to be tested in the
     Delaware field study. Interpretation
     of results is limited and complicated
   ""by the lower-than-expected sample
     concentrations.
   One of  the most  interesting observa-
tions was that the  dominant  concentra-
tions  noted  in  monitoring   near  "old"
Superfund sites were due to local (within 5
km) industrial emissions.
   The Delaware SITE Study of 1989 has
shown the feasibility for field monitoring for
five of the  six monitoring  techniques that
were tested for organic compounds. Auto-
mated gas chromatographs, canister-based
sequential  samplers,  personal sampling
devices for VOCs, canister-based sector
samplers, and long path infrared transmis-
sion monitors  were successfully  used to
monitor target compounds at  ambient air
concentrations. Comparisons between per-

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sonal sampling devices and canisters, and
between long path infrared transmission
monitors, were effective in providing for a
strong quality assurance program.  Based
on  results  of the study, four articles for
submission to peer-reviewed journals have
been prepared. Information from the Dela-
ware study is already being used in EPA
Region I (sector samplers), in EPA Region
VII  (long path infrared transmission moni-
tors), and in  EPA Region IV (automated
gas chromatographs).
Conclusions and
Recommendations
Automated Gas Chromatograph
     This system should be redesigned
     so that liquid nitrogen  is no longer
     required.
     A  single supplier of an integrated
     system including both  the GC and
     the preconcentrator should be identi-
     fied.
 •   Different  sorbents  such  as the
     Supelco triple bed sorbent should be
     evaluated  as a preconcentrator of
     VOCs.
Figure 1.     Monitoring sites for the 1989 Delaware SITE study.
Fourier Transform Infrared Long Path Sys-
tem
    Several changes to the instrument de-
sign need to be addressed to improve the
detection capability of this technique. These
include
      Recoat the retro-reflector with a coat-
      ing that is  nonabsorbing across the
      spectral region of interest.
      Direct the  beam through the  inter-
      ferometer before it traverses the path
      in order to eliminate the background
      emission.
      Identify and install a  smaller light
      source.
      Develop a procedure for determining
      the precision  and accuracy of the
      FTIR data.
Sector Sampling
      The design of this instrument should
      be altered to include  sector  limits
      that can be reset rather than being
      fixed at 90°.
      The instrument should be provided
      with a threshold for wind speed.
      Technology transfer to the regional
      offices should  be initiated.
Sequential Sampler
      The difficulty with the accumulation
      of water vapor  in the instrument's
      valve system must be solved.
      A portable, battery-operated  wind
      speed/wind direction sensor must be
      identified for use with the sampler at
      monitoring sites.
      Technology transfer of this technique
      to the EPA regional offices should be
      initiated.
Personal Sampling Devices
 •    The use of sorbents other than Tenax
      GC should  be evaluated. This re-
      quires both laboratory and field test-
      ing.
      An investigation should be made into
      the use of supercritical fluid extrac-
     tion of VOCs from solid sorbents.
      The use of these devices as a screen-
      ing technique  for a wider range of
      volatile compounds at Superfund sites
      should be investigated.
Anion Exchange Resin
     A sealable field  sampling cartridge
     should be developed that is capable
     of sustaining sample flow rates up to
      1 L/min.
     The sampling  technique  should be
      retested at a site with known  high
     concentrations  of phenolic com-
     pounds.
     A series of  both laboratory and field
     tests should be conducted in which
     the impinger method (EPA Method
     TO-8), given in the Compendium of
     Methods for the Determination  of
                                                                   •&U.S. GOVERNMENT PRINTING OFFICE: 1992 - 648-080/40143

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     Toxic Organic Compounds in Ambi-
     ent Air, is used as a comparison.

   The information in this document has
been funded in part by the U.S. Environ-
mental Protection Agency. It has been sub-
jected to Agency review and approved for
publication. Mention of trade names and
commercial products does not constitute
endorsement or recommendation for use.
   The EPA authors, W.A. McClenny (also the Project Officer; see below), J.D. Pleil, J.L.
     Vams, J.D. Mullk, RE. Berkley, K.J. Krost, arid W.T. McLeod, are with the Atmo-
     spheric Research and Exposure Assessment Laboratory, Research Triangle Park, NC
     27711. G.M. Russwurm, K.D. Oliver, andD.D. Williams are with ManTech Environ-
     mental Technology, Inc., Research Triangle Park, NC27709. M.W. Holdren andAJ.
     Pollack are with Battelle Columbus Laboratories, Columbus, OH 43201.
   The complete report, entitled "Superfund Innovative Technology Evaluation, The
     Delaware SITE Study, 1989," (Order No. PB92-125749/AS; Cost: $26.00, subject to
     change)  will be available only from:
          National Technical Information Service
          5285 Port Royal Road
          Springfield, VA 22161
          Telephone: 703-487-4650
   The EPA Project Officer can be contacted at:
          Atmospheric Research and Exposure Assessment Laboratory
          U.S. Environmental Protection Agency
          Research Triangle Park, NC 27711

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