PROCESS
MEASUREMENTS
REVIEW
                                       INDUSTRIAL
                                  ENVIRONMENTAL
                                        RESEARCH
                                     LABORATORY

                                 vvEPA
Volume 1, Number 4
Research Triangle Park, N.C. 27711
Spring Edition, 1979
DEVELOPMENT
OF A MASTER
ANALYTICAL SCHEME
FOR VOLATILE ORGANICS
          SYMPOSIUM ON ADVANCES
          IN THE SAMPLING
          AND MEASUREMENT OF
          PARTICULATE MATTER
   The development of a master scheme for the anal-
ysis of organics in water was discussed during a Jan-
uary 26,1979, workshop held in Atlanta, Georgia. Ap-
proximately 75 people attended the workshop, repre-
senting analytical personnel from government agen-
cies, private industry,  academic institutions, and re-
search organizations.
   The first generation of the analysis scheme is in-
tended to be applicable to volatile organics in indus-
trial, energy, or municipal effluents and in surface or
drinking waters. Volatile organics, for the purposes
of this scheme, include any that will elute from a gas
chromatographic column at 300° C in 1 hour or less or
any that may be derivatized to do so. Lower detec-
tion limits for the scheme have been set at 0.1 /tg/L
for drinking water, 1  /tg/L for surface water, and
10  /ig/L for  effluents.  Users of the scheme  will be
given guidance concerning sampling, addition of in-
ternal standards, handling, preservation, extraction,
concentration, and cleanup of the  sample. Detection
and quantification will be by gas chromatography-
mass  spectrometry.
   The project originated at EPA's Environmental
Research Laboratory in Athens, Georgia. Work on
|toe scheme is being carried out under EPA contract
P42-2704 with Research Triangle Institute (RTI).
A.  W. Garrison is EPA's Project Officer; Edo Pelliz-
?ari of RTI is the Principal Investigator. The project
,s scheduled for completion in the  spring of 1980.
             During the past few years, through the efforts of
           both industry and government, advancements have
           been made in the technology of sampling and sizing of
           particulate matter in various industrial and ambient
           environments. In order to gather together the ex-
           perts in these areas, EPA's Industrial Environmental
           Research Laboratory-RTP is sponsoring its second
           symposium on measurement of particulate  matter.
           Speakers will discuss the  status of current research
           and development in the areas of:
             •  Inertial, optical, diffusional, and electrical par-
                ticle sizing
                Control device evaluation
                Aerosol characterization
                Quality assurance
                Data reduction techniques
                Real-time monitoring of mass concentrations
                and size distribution
             •  Inhalable particulate matter.
           The number of speakers will be limited so that sym-
           posium attendees will have ample time to ask ques-
           tions and to discuss their own experiences in these
           fields. The symposium will be held October 7-10,
           1979, at the Daytona Hilton, Daytona Beach, Florida.
           Coordinator of the symposium is Wallace B. Smith,
           Southern Research Institute,  2000  Ninth Avenue,
           South, Birmingham, Alabama 35205.
  The views expressed in the Process Measurements Review do not necessarily reflect the views and policies of the Environmental Protec-
 tion Agency. Mention of trade names or commercial products does not constitute endorsement or recommendation for use by EPA.

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Process
                                                                            Volume 1, Number 4, Spring Edition, 1979
   SULFURIC ACID

   MEASUREMENT

   METHODOLOGY

      The present  interest in sulfur oxide emissions
   from flue gas desulfurization (FGD) units has stimu-
   lated increased sampling and analysis for  sulfuric
   acid (H2S04) and particulate sulfate. Though unsub-
   stantiated at this time, there is reason to believe that
   FGB units emit sulfate aerosols while removing S02.
   Part of the problem in confirming this theory is the
   lack of proven methodology to quantitatively sepa-
   rate and efficiently collect the various sulfur oxides
   emitted by stationary sources. EPA's Industrial En-
   vironmental Research Laboratory at Research Tri-
   angle Park (IERL-RTP) has established several pro-
   grams to define the present state of the art and to
   develop new methods for sulfate and  sulfuric acid
   sampling and analysis. This article summarizes some
   of the highlights of that research and provides back-
   ground information on the sampling problems asso-
   ciated with H2S04/sulfate aerosols.

   HgSOj/SULFATES AS
   A HEALTH HAZARD
      The toxicity of H2S04 in gross quantities is well
   known, but until recently the effect of H2S04 aerosol
   had not been investigated. In recent tests, laboratory
   animals were exposed to various amounts of H2S04
   aerosol. Results were narrowed air passages and mu-
   cosal swelling or increased secretion. Consequently,
   people who already have trouble breathing (the aged,
   asthmatics, or heart patients) can be affected not only
   by the directly corrosive qualities of H2S04, but also
   by the respiratory strain that the aerosol places on
   them. As the particle size was decreased, an increase
   in the flow resistance to respiration was noted in the
   animals. Other sulfates produced similar results. A
   comparison of zinc ammonium sulfate, zinc sulfate,
   and ammonium sulfate showed zinc ammonium sul-
   fate to be the worst irritant. When zinc ammonium
   sulfate and HgSC^ aerosol of equal particle size were
   compared, H2S04 was the greater irritant.

   ftjSOj/SULFATE
   SAMPLING PROBLEMS
      Experience has shown that  the H2S04/sulfate
   content of typical combustion gas from oil- or coal-
fired sources ranges from 1 to 5 percent of the total
sulfur burned. The bulk of the sulfur ends up as S02.
Any  H2S04/ sulfate method must prevent small in-
terferences from S02 to avoid a large positive error
in the H2S04/sulfate quantification.
   A problem specific to H2S04 sampling is the diffi-
culty in separating H2S04 vapor (or aerosol) from al-
kaline particulate matter. TRW research results, re-
ported at the 70th annual APCA meeting, indicate
that  the current EPA Federal Reference Method 5
recommended filter temperature of 121° C is too low
to prevent collection of H2S04 on the  filter. When
this  happens, differentiation of H2S04 and particu-
late  sulfate is impossible. In fact, temperature con-
trol at all locations along the train is important. For-
mation of H2S04 aerosols from the vapor phase is
highly probable due to the nucleation sites provided
by the fine particles present in the flue gas. Surfaces
that these aerosols might contact must be hot enough
to revaporize the H2S04. TRW's investigation of this
problem  has shown  that gas  temperatures above
250° C are required to prevent H2S04 fallout in sam-
pling trains.


H2SO4 SAMPLING

METHODOLOGY
   The best approach to H2S04 sampling method-
ology would be to design a comprehensive sampling
system  so that S02, H2S04, and particulate sulfate
(SO^) are separated. Currently available method-
ology for sampling particulate  sulfate is adequate
provided it  is not  important if small amounts of
H2S04 are included in the final value. Numerous at-
tempts have been made to design systems capable of
separating H2S04 from sulfur dioxide. Almost all the
techniques fall into  one of two types of sampling
strategies — selective absorption or controlled con-
densation.
   Selective absorption uses 80 percent 2-propanol
(isopropyl alcohol) to collect the sulfur trioxide (S03)
and to pass the S02. The S02 is collected in 3 percent
hydrogen peroxide  (H202). This method has been
used extensively and is the basis of EPA's compli-
ance test (FederalRegulations, 41, 111, 1976) for acid
mist from sulfuric acid plants.  The major problem
with utilizing the EPA procedure for other types of
sources is the lack of a prefilter to effectively pre-
vent particulate matter from reaching the alcohol
impinger. The particulate  matter  in the  impinger
can act either as a direct interferent by contributing
S04 or as an indirect interferent by promoting the

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Process Measurements Review
                           Volume 1, Number 4, Spring Edition, 1979
    oxidation of 802 'n the liquid phase through action
    of trace elements such as iron, copper, or vanadium.
    The method also assumes that all S02 can be purged
    from  the  alcohol impinger.  Recently,  oxidizing
    agents have been found in reagent grade 2-propanol.
    This finding partially explains the high values nor-
    mally found when selective 2-propanol absorption
    methods  are used. Because of the particle  separa-
    tion and S02 purging problem, this procedure is not
    recommended for coal or oil combustion sources.
       The controlled condensation approach for H2S04
    was first proposed by B. P. Knol in a 1960 issue of
    Rivista dei Combustibili and was further developed
    by Goksoyr and Ross and reported in the Journal of
    the Institute of Fuel in 1962. The Goksoyr-Ross sys-
    tem is the basis of an American Society for Testing
    and Materials (ASTM) procedure for sulfur oxides
    (SOX) (Part 26, ASTM Method D3226-73T, 1974). In
    the controlled condensation approach, H2S04 is sep-
    arated from the gas stream by reducing the temper-
    ature of the flue gas below the  dewpoint for H2S04
    but above  the  dewpoint  for H20 (Figure  1). The
    resulting aerosol is collected either on the walls of
    the cooling coil or on a backup  frit. Controlled con-
    densation has been studied in  the laboratory and
    found to  have a precision and accuracy of ± 6 per-
                                                                      RELATIVE TEMPERATURES
 PARTICULATE MATTER
 REMOVED FROM
 H2SO4 VAPOR
 H2SO,
i SELECTIVELY
 REMOVED FROM
 GAS PHASE
 SO2 ENTRAINED WITH
 CONDENSING H?O
                    	H2S04 DEWPOINT (116 TO 143°C)
                          H20 DEWPOINT (50 TO 100°C)
  Figure 1. Principle of controlled condensation.
cent in synthetic gas streams. However, the labora-
tory systems  have neither adequate  temperature
control nor particle removal systems for field use.
   TRW, under EPA Contract 68-02-2165, adapted
the controlled condensation  procedure to particle-
laden streams and  developed the system shown in
Figure 2. This system uses an all quartz probe to col-
lect the gas from the stack and a quartz filter holder
                                   ADAPTER FOR
                                   CONNECTING HOSE

                                  TCWELL
                GLASS-COL
                HEATING
                MANTLE
                  STACK
                           ASBESTOS CLOTH
                           INSULATION
                                                                                 VACUUM
                                                                                 GAUGE-
                                                                             PUMP

                                                                        SILICA GEL
                                                                                  THREE-WAY
                                                                                  VALVE
                                                                    8% Na2C03

                                                          RECIRCULATOR

                                                          THERMOMETER
                                            STYROFOAM
                                            ICE CHEST
                           Figure 2.  Controlled condensation system field setup.

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Process Measurements Renew
                                    Vblune 1, Number 4, Spring Edmon, 1979
    and filter to remove the participate matter. Prior to
    the controlled condensation coil, the gas temperature
    is maintained above 250° C to prevent H2S04 fallout
    and to ensure the separation of HgS04 from particu-
    late matter. Using this system during an intensive
    30-day test program at the TVA/EPA Shawnee FGD
    Test Facility, the average inlet HgSC^ concentration
    was 8.3  ppm  and  the  average outlet concentration
    was 3.1 ppm. Both values, based on daily morning and
    evening  tests, were found to be  highly variable. It
    became apparent that a continuous HgSC^ monitor
    was needed to record the fluctuations in process con-
    ditions. Such an instrument was designed using the
    controlled condensation approach and was built by
    TRW under the supervision of the Process Measure-
    ments Branch of EPA's IERL-RTP. This automated
    version of the controlled condensation system is de-
         signed to produce a H2S04 concentration value every
         15 minutes. It will operate continuously for 24 hours
         under  mass loading conditions  up to 13 ^g/m3.  A
         typical output from this monitor is shown in Figure 3.

         Summary

            Sampling for H2S04 requires the quantitative sep-
         aration  of  S02, particulate matter, and  H2S04.  To
         date, the best approach for this task is the controlled
         condensation  system. By automating this system,
         semicontinuous H2S04 measurements can be attained
         and a direct correlation with on-line process informa-
         tion is possible.

                                        Ray F. Maddalone
                                        TRW
       TO.O
        9.0
     i  8.0
     Q.
     O
     S  7.0
     
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Process Measurements Review
                          Volume 1, Number 4, Spring Edition, 1979
   COMPUTER-BASED CASCADE

   IMPACTOR DATA REDUCTION

   PROGRAM

       Cascade impactors have gained wide acceptance
   in  the measurement  of particle size  distribution.
   These devices are regularly used in a wide variety of
   environments ranging from ambient  conditions  to
   flue gas streams at 500° C (950° F). Specially  fabri-
   cated impactors can be used for more extreme condi-
   tions.
       Because of their usefulness, research has been
   funded under EPA Contract 68-02-2131 and performed
   by  Southern Research Institute to explore the theo-
   retical and practical aspects of impactor operation.
   As  part of this research, an effort has  been made to
   design a comprehensive data reduction system that
   will make full use of cascade impactor measurements.
       The cascade impactor data  reduction system is
   designed to automatically reduce data taken with any
   one of four commercially available round-jet cascade
   impactors: the Andersen Mark III Stack Sampler, the
   Brink Model BMS-11 (as supplied  and with  extra
   stages), the University  of Washington Mark III
   Source Test Cascade Impactor, and the Meteorology
   Research Inc. Model 1502 Inertial Cascade Impactor.
   With modification the computer programs can accom-
   modate any round-jet impactor with  an arbitrary
   number of stages. Provision is not presently made in
   the system for slotted jet impactors. However, with
   more extensive revision the system could also handle
   data from  these impactors.
       The original computer programs comprising this
   data reduction  system are written in FORTRAN IV
   language.  The plotting subroutines used were writ-
   ten specifically  for the Digital Equipment Corpora-
   tion PDP-15/76 computer and  are  not compatible
   with other plotting systems. However, these pro-
   grams are  in the process of being revised for use with
   other systems.
       The overall  system incorporates six programs:
   MPPROG, SPLIN1, GRAPH, STATIS, PENTRA, and
   PENLOG. Impactor design, particulate catch  infor-
   mation, and sampling conditions from single impactor
   runs are used to calculate particle size  distributions.
   MPPROG  and  SPLIN1 perform data  analyses and
   make curve fits. GRAPH is totally devoted to various
   forms of graphical  presentation of the calculated
   distributions. The particle size  distributions can be
   delivered in several forms. STATIS averages data
   from multiple impactor runs under a common condi-
tion, and PENTRA or PENLOG calculates the con-
trol device penetration and/or efficiency.
   Two reports describing this data reduction sys-
tem are available from NTIS. A brief overview of the
program, including several examples, is given in A
Data Reduction System for Cascade Impactors, EPA-
600/7-78-132a, July  1978. The detailed program de-
scription with program listings can be found in A
Computer-Based Cascade Impactor Data Reduction
System, EPA-600/7-78-042, March 1978.

                     Kenneth M. Gushing
                     Southern Research Institute
A MASSIVE VOLUME SOURCE
SAMPLER FOR HEALTH

EFFECTS STUDIES

   A critical need exists for information pertaining to
the health effects of the particulate pollution emitted
from emerging alternative energy sources. A portion
of this information can be obtained from bioassays
and animal inhalation studies conducted on samples
of these emissions. However, the extended time peri-
ods needed to perform these studies require large
quantities (1 kg or greater) of particulate sample. The
purpose of this task, sponsored under EPA Contract
68-02-2131, was to design, fabricate, and test a sam-
pling system that would collect sufficient quantities
of particulate samples for health studies in relatively
short time periods. A sampling rate of 340 normal cu-
bic meters per hour (Nm3/hr) was estimated to be ade-
quate. Other design considerations were the need to
separate the sample into two size fractions—coarse
and fine — and minimization of wall deposition within
the system. Because the  sampler would be used at
various  sites, it had to be readily transportable and
conveniently adaptable to different site conditions.
   The ultimate goal of this task was to ensure  that
the biological impact of the collected sample would be
an accurate representation of the emissions produced
by the energy source. Fulfilling the particle size dis-
tribution aspect necessitated the building of a tra-
versing  sampler capable of near-isokinetic sampling.
Accomplishing the biological impact goal required a
sampler that would prevent or minimize contamina-
tion of the sample. This was accomplished by using
special construction  materials to minimize contam-
ination by the walls of the sampler and by maintain-
ing source gas temperatures in the  sampler, thus

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Process MeastiBwiits Review
                                                                                     VWume 1, Nunter 4, Spring Edition, 1979
   eliminating condensation of organic and  inorganic
   vapors.
       The prototype system (see Figure 4) consists of a
   probe, a  cyclone dust collector,  a fabric filter, a
   flowmeter, a blower, and a. sampling/interconnecting
   line. The probe is 2.1 m  (7 ft) long and has an ad-
   justable opening at its inlet to establish  isokinetic
   sampling. The probe is capable of traversing and, al-
   though it is designed for a 9-cm (4-in.) port, it can be
   easily adapted to fit larger ports.
       A Fisher-Klosterman XQ-5 cyclone with a cali-
   brated 50 percent  efficiency cut point (D^) for a
   2.5-fim aerodynamic  diameter  at  340  Nm /hr
   (200 stdft3/min) is the initial particle collector. The
   cyclone, with its heated enclosure, is approximately
   2.1 m high x  0.6 m wide x 0.6 m long (6 x 2 x 2 ft)
   and weighs 91 kg {200 Ib). Immediately following the
   cyclone is a single chamber fabric filter approximate-
   ly 2.1 m high x OS m wide x 0.9 m long (7x3x3
   ft) and weighing 113 kg (250 Ib). The filter chamber
   can accommodate from 1 to 20 envelope bags. The fil-
   tration surface of the bags is composed of Gore-Tex
   porous Teflon laminate backed by Nomex. Each bag
   has 0.5 m2 (5.0 ft2) of collection surface. The fabric fil-
   ter is equipped with a manual shaker and can be eas-
   ily modified to a double-chambered, automatic shaker
   design.
      An orifice plate flowmeter is used to monitor the
                      PROBE
              STACK
340 Nm3/hr flow rate selected for the  sampler. The
flow rate must be stable to maintain the 2,5-/*m D^
cut point of the cyclone. A hand-operated damper at-
tached to the outlet of the blower is used to adjust
the flow rate. The  blower  is a centrifugal pressure
blower  powered  by a 3-phase, 7.5  HP  motor and
weighs  approximately 453 kg (1,000 Ib).  At the de-
signed flow rate, the sampler requires about 2.5 days
of continuous sampling to collect 1 kg of paniculate
matter from the outlet of an efficient control device
                                               o
with a particulate mass concentration of 0.05 g/Nm .
   The  entire sampler is heat traced from the probe
to the outlet of the fabric filter. All of the surfaces are
either 304  or  316 stainless steel, Teflon, or  glass.
Heating is controlled from three  heater  control
panels,  each panel handling a separate heater load.
The individual heaters can be connected in various
arrangements  to accommodate different sampling
site  voltages  and  heating  requirements.  Design
operating  temperature  of  the  sampler is  204° C
(400° F).
    Construction of the sampler has been completed
and a preliminary field test conducted. A  full field
test will be run in June 1979.

                      Paul R.  Cavanaugh
                      Southern Research Institute
                                               CYCLONE
                                               ENCLOSURE



r
CYC
	 1
L
\.


1
|
1
LONE
1
1
~ ™
../

                                                                        FABRIC
                                                                        FILTER
                                                                        HOPPER
                                                                                             ORIFICE
                                                                                             METER
                                                                                                    BLOWER
                              Figure 4. Schematic of high volume particle sampler.

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Process Measurements Review
                                                          VWume 1, Number 4, Spring Edition, 1979
                         THE USE OF SOEBENT RESINS
                        IN  ENVIRONMENTAL  SAMPLING
      Research in many laboratories over the past few
   years has shown that macroreticular (sorbent) resins
   have  desirable characteristics  for  environmental
   sampling. The resins tend to have good collection effi-
   ciency and also provide good recovery of the col-
   lected sample. While most of the reported work has
   focused on the sampling of organic species from air
   (source and ambient), these resins are also finding ap-
   plication in water sampling and in sampling of species
   such as organometallics.
      A research program is underway at Arthur  D.
   Little, Inc., to obtain a detailed quantitative under-
   standing of the behavior  of  sorbent resins in sam-
   pling systems. Most of the work to date has been ap-
   plicable to the sampling of air. This work is described
   in the documents Selection and Evaluation  of Sor-
   bent Resins for the Collection of Organic Compounds
   (EPA-600/7-77-044) and Characterization of Sorbent
   Resins  for Use in Environmental Sampling (EPA-
   600/7-78-054).
      In addition to chemical surface properties, impor-
   tant physical parameters in resin selection are parti-
   cle size, pore volume, and surface area.  Resins com-
   monly  considered for environmental  studies are
   Chromosorb 101,  Chromosorb 102,  XAD-2, XAD-4,
   Tenax-GC, and Poropak. Particle size of the resins
   has a practical impact on their use in sampling trains
   because the  size range utilized will affect the
   pressure drop across the  sorbent bed. The pressure
   drop of several resins tested in a 4.5-cm diam  x 9-cm
   holder at a velocity of 30 cm/sec (1 ft3/min flow rate) is
   shown in Table 1. Thermal stability of the resins is
   also  important. The decomposition  temperature of
   several resins, as  measured by differential scanning

         Table 1. Comparison of Pressure Drop
                 of  Various  Sorbents
       Sorbent
Mesh range     AP (cmHg)
    XAD-2



    Chromosorb 102

    Tenax-GC
  20-50
  30-40
  30-50

  48-60

  35-60
 6.4
 6.4
 8.9

15.2

 8.6
              calorimetry, is given in Table 2. Actual use tempera-
              ture should be maintained well below these values
              when the resins are being used for analysis of trace
              level compounds. XAD-2 has been found to be the
              preferred resin when  solvent extraction procedures
              are to be used in sample preparation. If thermal de-
              sorption is to be used, Tenax-GC is the sorbent of
              choice. Thermal desorption methods should generally
              be reserved for small-scale sampling apparatus.
                While XAD-2 and Tenax-GC have comparable col-
              lection characteristics at 20° C, XAD-2 generally has
              slightly better volumetric capacity and has substan-
              tially greater (10X) weight capacity than Tenax-GC.
              These two basic factors, weight capacity and the vol-
              umetric capacity (Vg) for each compound with its spe-
              cific volatility (boiling point) and polarity, control the
              quantitative behavior  of the resins in a sampling sys-
              tem. The capacity of the resin for a pollutant is a com-
              plex function of concentration, volatility, and polarity
              in  streams  with  high  pollutant  levels.  Generally
              speaking, XAD-2 will have an upper weight sorption
              capacity of 1 to  10  percent of the resin weight.
              Tenax-GC weight capacity is generally about 10 per-
              cent of that of XAD-2, or 0.1 to 1 percent of the resin
              weight.
                The collection of vapors in most environmental as-
              sessment studies occurs when the pollutant concen-
              tration is quite  low (e.g., 1 to 100 mg/m3). In these
              cases, the principal characteristic influencing resin
              quantity and sampling conditions is the  volumetric
              capacity (VJ for the specific pollutant. The volumetric
              capacity describes the breakthrough capacity of the
              resin (in  units of milliliters per gram) and is the max-
              imum volume of sample stream that can be pulled
              through  the resin while still quantitatively retaining
              the pollutant.

                   Table 2. Sorbent Thermal Decomposition
                           Characteristics
   Sorbent
Onset of Decomposition
XAD-2
Chromosorb 102
Tenax-GC
         210° C
         200° C
         400° C

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Process Measurements Review
                                                                                     Vbkme 1; Number 4, Spring Edition, 1979
        The general behavior of the resin/pollutant in-
    teraction can be conveniently summarized in terms of
    an empirical correlation observed  between elution
    volume (actually log Vg) and boiling point, as shown in
    Figure 5. As is indicated in  Figure 5, good correla-
    tions were observed between log Vg and the boiling
    point for each compound category studied. There are
    some  significant differences in Vg values for com-
    pounds that have the same boiling point but  are in
    dissimilar compound categories.
        These data can be used in two basically different
    ways starting  with either the resin quantity  or the
    volume to be sampled as the fixed quantity. The fol-
    lowing examples describe the procedures used in de-
    signing the sampling approach. Suppose a  source
    were to be sampled for chlorobenzene and a typical
    set of Method 5 conditions were  to be used, i.e.,
    28 L/min for 1 hr. The Vg for chlorobenzene on XAD-2
    is 2.4  x 105 mL/g. Because 1,680 L are to be sampled,
    a minimum of 7  g of XAD-2 would be required for
    complete collection.
                     A different type of question would be whether the
                 SASS train, with its predetermined resin bed  vol-
                 ume, will quantitatively collect benzyl amine, for ex-
                 ample. The sorbent cartridge in the SASS train con-
                 tains about 130 g of XAD-2 and a 30-m3 sample is nor-
                 mally collected. These values can be used to calculate
                 a cutoff Vg value for the SASS train of 2.3 x 105mL/g
                 or log Vg = 5.4; this value is indicated by the dashed
                 line in Figure 5. In order for  a  compound to be col-
                 lected completely by the sorbent module, its Vg would
                 have to be greater than 2.3 x 105. The Vg for benzyla-
                 mine is 7.9 x 106; thus, benzylamine would be com-
                 pletely collected. A comparison of several sampling
                 trains relative to vapor collection is given in Table 3.
                     The compound categories studied, as represented
                 in Figure 5, cover each of the different types to be en-
                 countered well enough so that one can estimate a Vg
                 (log Vg) value for new compounds by careful interpola-
                 tion and extrapolation.
                                               Philip L. Levins
                                               Arthur D. Little, Inc.
                 8.0
                 7.0
                6.0
                5.0
                   0               50               100               150               200
                                                       Boiling Point ("Cl
                      Figure 5. Log Vg vs. boiling point for individual adsorbate groups on XAD-2.
       Table 3. Relationship of SASS and Modified Method 5 Trains to Specific Retention Volume (Vg) Data
                                                                                     XAD-2
                           Sampling
                           time (hr)
  Sampling
volume (m^)
                           Breakthrough
Sorbent trap    Resin     _
volume (mL)   cap (g)      Vg (mL/g)    Iog10 Vg
     SASS                      4
     141 L/min (5 ft3/min)        1

     Modified Method 5          4
     28.3 L/min (1 ft3/min)       1
      34
      8.5

      6.8
      1.7
                                                              445
100
                                  130
                  29
260,000
 65,000

234,000
 59,000
5.42
4.81

5.37
4.77
                                                       8

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Process Measurements Review
                                                                Volume 1, Number 4, Spring Edition, 1979
                REVISIONS TO IERL-RTP PROCEDURES MANUAL: LEVEL 1
                ENVIRONMENTAL ASSESSMENT BIOLOGICAL TESTS FOR
                PILOT STUDIES, EPA-600/7-77-043
   Change 1:
"Marine Algal Bioassay"
Chapter 3, beginning on page 65
      The old procedure, while effective, required revi-
   sions in order to simplify the assay and provide for
   both stimulation and inhibition of growth caused by
   Level 1 samples. The new, simplified procedure pro-
   vides a combination of nutrients and minerals neces-
   sary to allow both growth inhibition and stimulation
   to be evaluated for Level 1 samples.


   Change 2:  "Daphnia Bioassay"
              Chapter 3, page 50

      On page 52 of the current manual, Daphnia pulex
   is  recommended. Daphnia magna should replace
   Daphnia pulex as the test animal throughout the pro-
   cedure because it is much larger, is easier to work
   with, and has a much stronger toxicity data base.
Change 3:   "Chinese Hamster Ovarian Clonal
           Growth Use for Cytotoxicity Testing"
           Chapter 3, pages 35-36

   The existing procedure  recommends the use of
the cell line WI-38 for cytotoxicity testing of liquid
samples (i.e., aqueous and organic liquids). The cost of
this test has increased markedly since its inclusion in
the protocol and alternate  cytotoxicity tests exist
that provide comparable results at much less expense.
The Chinese Hamster Ovarian (CHO) clonal  assay
(Chapter 3, page 36) should be used as the cytotoxic-
ity test in the Level 1 biological procedures for liquid
samples.


NOTE: Revisions appear in condensed form. For com-
plete  change  notices, contact Ray  Merrill,  PMB,
IERL-RTP (919-541-2557).
                        DEVELOPMENTS IN SAMPLING TECHNIQUES
                           FOR EVHALABLE PARTICULATE MATTER
      In support of a reassessment of the total sus-
   pended particulate standard now underway by EPA's
   Office of Air Quality Planning and Standards, three
   laboratories in EPA's Office of Research and Develop-
   ment—the  Health  Effects  Research  Laboratory
   (HERL-RTP), the Environmental Sciences Research
   Laboratory (ESRL), and the Industrial Environmen-
   tal Research Laboratory (IERL-RTP)—are examin-
   ing potential sampling  requirements. The  HERL-
   RTP has recommended a 15-^m upper cut size for in-
   halable particulate matter and a second division at
   2.5  /tm for fine  particulate matter.  Current par-
   ticulate matter sampling techniques do not provide
   data at these cut sizes for either ambient or source
   samples. At a workshop of leading aerosol scientists
   sponsored  by the Process Measurements Branch of
   IERL-RTP, a measurement development program
   was  recommended. The program considers short-
   term modifications  for  existing  techniques and a
   longer term  effort to fully investigate the  require-
                                       ments for more information, including data on stack
                                       condensable matter.
                                          A number of developments have been made in
                                       this  program.  Extrapolation techniques  have  been
                                       developed to estimate the 15-/*m particulate loading
                                       using existing data on loadings up to 10 /tm. A 15-/tm
                                       cyclone has been designed and is being tested for use
                                       with a Method 5 train.  Horizontal elutriators are
                                       being investigated and have shown good laboratory
                                       agreement with theory. A prototype elutriator is be-
                                       ing built for use  with the Fugitive Air Sampling
                                       Train (FAST)  system  for fugitive  emission  meas-
                                       urements. ESRL is investigating particle losses in
                                       nozzles; preliminary data indicate significant collec-
                                       tion  (up to 90 percent) for many particle sizes below
                                       15 /tm.

                                                                       D. B. Harris
                                                                       EPA/IERL-RTP

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        ntste
                          Volume 1, Number 4, Spring Edmon, 1979
      ENVIRONMENTAL ASSESSMENT  MEASUREMENT SYMPOSIUM
   The  second symposium on "Process Measure-
ments for Environmental Assessment" is scheduled
for February 25-27, 1980, in Atlanta, Georgia. The
symposium will consist of sessions on sampling tech-
niques, chemical  analysis, and  biological assays  of
samples from energy and industrial processes. Major
emphasis will be placed on measurement method de-
velopment and application to complex samples. Pro-
cedures  for  both  initial  screening  and  detailed
analysis will  be included in the presentations.  Au-
thors wishing to propose papers for the symposium
should submit titles and brief abstracts to Philip L.
Levins, Arthur D. Little, Inc., Acorn Park, Cam-
bridge, Massachusetts 02140.
                   RECENT EPA PUBLICATIONS OF INTEREST
R. R. Wilson, Jr., P. R. Cavanaugh, K. M. Gushing,
W. E. Farthing, and W. B. Smith
Guidelines for Particulate Sampling in Gaseous Ef-
fluents from Industrial Processes, EPA-600/7-79-028,
PB 290 899 (1/79).
   This report lists and briefly describes many in-
struments and techniques used to measure the con-
centration or size distribution of particles suspended
in process streams. Standard (well-established) meth-
ods are described, as well as some experimental meth-
ods and prototype instruments. Instruments and pro-
cedures are described for measuring mass concentra-
tion, opacity, and particle size distribution. Proce-
dures for planning and implementing tests for control
device evaluation are also included.

D. E. Lentzen, D. E. Wagoner, E. D. Estes, and W. F.
Gutknecht
IERL-RTP Procedures Manual: Level 1 Environmen-
tal Assessment (Second Edition), EPA-600/7-78-201,
PB 293 795 (10/78).
   This manual presents revised Level 1 environmen-
tal assessment procedures  for personnel collecting
and  analyzing samples from industrial and energy-
producing processes. The strategy of the environmen-
tal assessment program provides a framework for de-
termining industrial process and stream priorities on
the basis of a staged sampling and analysis techni-
que.  Level 1 is a screening phase that characterizes
the pollutant potential of process influent and ef-
fluent streams. The manual is divided into two major
sections. Chapters 3-7 discuss sampling procedures
for gases, fugitive emissions, liquids (including slur-
riesA and solids.  The  remainder of the manual is
divided into three chapters on procedures for in-
organic, organic, and particle analyses.  Chapter 11
briefly discusses bioassay  procedures.  Biological
assessment techniques are detailed in a companion
procedures manual (EPA-600/7-77-043).
E. D. Estes, F. Smith, and D. E. Wagoner
Level  1  Environmental Assessment Performance
Evaluation, EPA-600,7-79-032, PB 292 931 (2/79).
   This report discusses a two-phased evaluation of
Level 1 environmental assessment procedures. Re-
sults from Phase I, a field evaluation of the Source
Assessment Sampling System (SASS), showed that
the SASS train performed well within the desired
Level 1 accuracy limit. A Method-5 train was used to
estimate the "true"paniculate loading. Phase  II of
the evaluation consisted of  three types  of control
samples to challenge the spectrum of Level 1 analyti-
cal procedures: an artificial sample  in  methylene
chloride, an artificial sample on a flyask matrix, and a
real sample composed of the combined XAD-2  resin
extracts from  all Phase I runs. Phase  II  results
showed that when the Level I analytical procedures
are carefully applied, data of acceptable accuracy are
obtained. Estimates  of intralaboratory and inter-
laboratory precision were made.

J. C. Harris, J. J. Hayes, P. L. Levins, and  D. B.  Lind
say
EPA/IERL-RTP Procedures for  Level 2 Sampling
and Analysis of Organic Materials, EPA-600/7-79-033,
PB 293 800 (2/79).
   This manual presents  Level 2 procedures for
sampling and chemical analysis of organic materials.
It represents a step in the development of a general
methodology for chemical and biological assessment
of environmental effects of  industrial effluents. It
presents concepts and general guidelines,  together
with a number of more fully developed,  tested, and
validated Level 2 procedures. The accumulation of ex-
perience in sampling and chemical analysis of  envi-
ronmental pollutants is by no means complete,  how-
ever. Users of the manual will find a number of areas
in which additional research and testing is needed,
and in which present knowledge is insufficient to per-
mit hard and fast procedures to be established.
                                               10

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Process Measurements Review
                                                     Volume 1, Number 4, Spring Etfition, 1979
    E. M. Smith and P. L. Levins
    Sensitized Fluorescence for the Detection of Polycy-
    clic Aromatic Hydrocarbons,
    EPA-600/7-78-182, PB 287 181 (9/78).
      This report describes  a fluorescent  spot test,
    devised for poly cyclic aromatic hydrocarbons (PAH),
    based  on the sensitization of the  inherent fluores-
    cence of such compounds. On filter paper, 10 pico-
    grams  (1 pg = 10~12 grams) of PAH in  a spot of
    0.25 cm diameter can  generally be detected when
    treated with naphthalene. In the case of benzo(a)py-
    rene, 1 pg has  been detected. This method has been
    shown to be specific for PAH with minimum interfer-
    ence from other compounds. The method may be used
    to estimate the general level (factors of 10) of PAH in
    samples to aid in decisions for more specific analyses.

    P. L. Levins, C. E. Rechsteiner, and J. L.  Stauffer
    Measurement  of PCB  Emissions from Combustion
    Sources, EPA-600/7-79-047, PB 293 360 (2/79).
       Use of gas chromatographic procedures for the de-
    termination of polychlorinated biphenyls (PCBs) in
    solids  and water to measure  PCBs in combustion
    source  emission has encountered certain difficulties.
    This report describes a gas chromatographic/mass
    spectrometric procedure that overcomes these diffi-
    culties. The procedure  relies on selected mass scan-
    ning in restricted regions of the chromatograms. It
    was developed because the distribution pattern of the
    individual PCBs changes in the combustion process.
    This renders invalid the pattern-matching approach
    used with the gas chromatographic/electron capture
    detector method.
                         W. B. Smith, Compiler
                         Proceedings: Advances  in  Particle  Sampling  and
                         Measurement (Asheville, NC, May 1978), EPA-600/
                         7-79-065, PB 293 363 (2/79).

                         J. L. Rudolph, J. C. Harris, Z. A. Grosser, and P. L.
                         Levins.
                         Ferroalloy Process Emissions Measurement, EPA-
                         600/2-79-045, PB 293 171 (2/79).

                         L. E. Sparks
                         Cascade Impactor Data  Reduction with SR-52  and
                         TI-59 Programmable Calculators, EPA-600/7-78-226,
                         PB 290 710 (11/78).

                         R. G. Patterson, P. Riersgard, and S. Calvert
                         Effects of Charged  Particles on Cascade Impactor
                         Calibrations, EPA-600/7-78-195, PB 288 270 (10/78).

                         N. H. Gaskins and F. W. Sexton
                         Compilation of Level 1 Environmental  Assessment
                         Data, EPA-600/2-78-211, PB 286 924 (10/78).

                         E. A. Burns, Compiler
                         Symposium Proceedings: Process Measurements for
                         Environmental Assessment (Atlanta, February 1978),
                         EPA-600/7-78-168, PB 290 331 (8/78).

                                 Copies of these publications are available at cost from:

                                     National Technical Information Service
                                     U.S. Department of Commerce
                                     5285 Port Royal Road
                                     Springfield, Virginia 22151.
                                  Request for the Process Measurements Review
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