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
Name.
. Position or Title.
Company.
Address _
ICilyl
ISUtel (Zip Codel
Return to: Ann Turner
Research Triangle Institute
P.O. Box 12194, Building 6
Research Triangle Park, N.C. 27709
{919)541-6893
Check if applicable:
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11
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