Measured Multimedia Emissions From The Wood Preserving Industry


March 1981
MEASURED MULTIMEDIA EMISSIONS
FROM THE WOOD PRESERVING INDUSTRY
by
Bruce DaRos, Dr. William Fitch, Richard Merrill, and Dr. Dean Wolbach
Acurex Corporation
Energy & Environmental Division
Mountain View, California 94042
Contract 68-03-2567
Task 4028
EPA Project Officer
Donald Wilson
Food and Wood Products Branch
Industrial Environmental Research Laboratory
Cincinnati, Ohio 45268
INDUSTRIAL ENVIRONMENTAL RESEARCH LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
N 0 f' 1 C £
M Wiriinary draft. UtaS
this document is a P-e;^.cd by EPA and
,0/Ihf''sta.=e be construed to rep-
iijouid not at this stag ^ ^ bL.;ng circulated
resent	accuracy and
for comment on its
poiicy implication oniy.

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ePQ o
March 1981
MEASURED MULTIMEDIA EMISSIONS FROM THE
WOOD PRESERVING INDUSTRY
by
Bruce DaRos, Dr. William Fitch, Richard Merrill, and Dr. Dean Wolbach
Acurex Corporation
Energy & Environmental Division
Mountain View, California 94042
Contract 68-03-2567
Task 4028
EPA Project Officer
Donald Wilson
Food and Wood Products Branch
Industrial Environmental Research Laboratory
Cincinnati, Ohio 45268
INDUSTRIAL ENVIRONMENTAL RESEARCH LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
J.S. EPA LIBRARY REGION 10 MATERIALS

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DISCLAIMER
This report has been reviewed by the Industrial Environmental Research
Laboratory, U.S. Environmental Protection Agency (EPA), and approved for
publication. Approval does not signify that the contents necessarily reflect
the view and policies of EPA, nor does mention of trade names or commercial
products constitute endorsement or recommendation for use.
11

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FOREWORD
When energy and material resources are extracted, processed, converted,
and used, the related pollutional impacts on our environment and even our
health often require that new and increasingly more efficient pollution
control methods be used. The Industrial Environmental Research
Laboratory-Cincinnati (IERL-Ci) assists in developing and demonstrating new
and improved methodologies that will meet these needs both efficiently and
economically.
This report documents a recently completed project. Its purpose was to
qualitatively and, when possible, quantitatively assess the organic emissions
resulting from the evaporation and thermal destruction of wastewater generated
by the wood preserving industry. The findings of this report can be used to
determine the driving forces governing the loss of organic constituents to the
atmosphere. The information contained in this report can also serve as a
basis for future work. For further Information, contact the Food and Wood
Products Branch, IERL, Cincinnati, Ohio.
David G. Stephan
Director
Industrial Environmental Research Laboratory
Cincinnati
iii

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ABSTRACT
Restriction of the discharge of wastewater generated during the
preservation of wood has resulted in the increased use of evaporation
techniqueis by the wood preserving industry. This report on the second phase
of work described in EPA report 68-03-2584 discusses emissions that may occur
to the atmosphere from thermal (pan) evaporation, spray pond evaporation, and
direct thermal destruction of organic components in the wastewater. The
information presented includes plant and evaporation device descriptions, test
plans, sampling and analytical results, and Conclusions and recommendations.
Also presented are qualitative descriptions of the fugitive emissions that can
occur during normal processing operations.
The primary conclusions are that organic compounds are emitted to the
atmosphere during thermal (pan) evaporation. Organic emissions from the spray
pond were below detectable levels. Fugitive organic emissions from the retort
and vacuum vents were significant in concentration but of short duration.
Thermal destruction of the compounds of interest may be a viable disposal
option if the boiler is properly designed.
iv

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CONTENTS
Foreword		iii
Abstract		iv
Figures		vii
Tables		viii
Abbreviations and Symbols			xi
Acknowledgment		xii
1.	Introduction		1-1
2.	Conclusions		2-1
3.	Recommendations			3-1
4.	Wastewater Treatment and Disposal by Evaporation or
Thermal Destruction 			4-1
4.1	Surface evaporation emissions		4-2
4.2	Droplet evaporation emissions . 		4-5
4.3	Emissions sumnary 				4-6
V Characterization of Multimedia Em1i»1on« From a Thermal
(Pan) Evaporation Device		 .	5-1
5.1	Program description and results		5-1
5.2	Models for thermal evaporation 		5-21
5.3	Conclusions 			5-31
6.	Characterization of Multimedia Emissions for Spray
Evaporation of Wood Preserving Wastewaters . 			6-1
6.1	Program description 				6-1
6.2	Discussion of results				6-3
7.	Characterization of Emissions from the Disposal of
Wood Preserving Wastes 1n an Industrial Boiler 		7-1
7.1	Program description and results		7-1
7.2	Material balance around incinerator 	 ; .	7-8
7.3	Chlorodibenzofurans and chlorodioxins ......	7-11
v

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CONTENTS (Concluded)
8. Evaluation of Fugitive Emission Sources
8-1
8.1	Treating cylinder spillage and drippage
8.2	Fugitive emission during unloading and
8-2
charging operations
8.3 Vacuum vent exhaust
8-2
8-4
Appendices
A.	Characterization of Multimedia Emissions From Thermal
(Pan) Evaporation of Wood Preserving Wastewaters .... A-l
B.	Characterization of Multimedia Emissions From Spray
Evaporation of Wood Preserving Wastewaters 	 B-l
C.	Characterization of Emissions From the Disposal of Wood
Preserving Wastes in an Industrial Boiler 	 C-l
vi

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FIGURES
Number	Page
5-1 Schematic of wood preserving plant wastewater/preservative
recovery system		5-3
5-2 Sampling locations for thermal (pan) evaporator tests
and fugitive emissions test		 5-17
5-3 Thermal evaporation system				5-23
5-4 Thermal evaporation cycle		 5-24
7-1 Schematic of plant wastewater/preservative recovery system . . 7-3
vii

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TABLES
Number	Page
2-1 Summary Table		 			2-2
5-1 Summary of Collected Samples 			5-5
5-2 Penta Pan Evaporator — Test 2 	 .....	5-6
5-3 Penta Pan Evaporator — Test 3			5-7
5-4 Penta Pan Evaporator — Test 4			5-8
5-5 Creosote Pan Evaporator — Test 2	¦....¦		5-9
5-6 Creosote Pan Evaporator -- Test 3 . 			5-10
5-7 Creosote Pan Evaporator — Test 4'				5-11
5-8 Penta Pan Evaporator — Average Values 		5-12
5-9 Cresote Pan Evaporator — Average Values 		5-13
5-10 Sampling Data				5-14
5-11 Creosote Pan Evaporator — Material Balance 		5-18
5-12 Penta Pan Evaporator — Material Balance 		5-19
5-13 Percent of Organic Specie Emitted in Vent . . . 			5-20
5-14 Penta Pan Evaporation -- Steam Distillation Model 		5-26
5-15 Creosote Pan Evaporation — Steam Distillation Model 	 5-27
5-16 Comparison of Pan Evaporator Models for Naphthalene 	 5-30
viii

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TABLES (Continued)
Number	Page
6-1 Summary of Samples Collected		6-3
6-2 Data for Pond Evaporation		6-4
6-3	Detection Limits — Pond Evaporation		6-7
7-1	Sample Collection Matrix 		7-5
7-2 Concentrations of Organic Components in Incinerator Samples . .	7-6
7-3 Inorganic Trace Element Compositions in Incinerator Samples . .	7-7
7-4 Rates of Discharge and Efficiency of Destruction for
Naphthalene and Phenol		 7-9
7-5 Calculation of Rates of Generation of Solids 	 7-11
7-6 Summary of Abbreviations for Chlorodibenzofurans and
Chlorodibenzodioxins .................... 7-12
7-7 Chlorodibenzofuran and Chlorodibenzodloxin Analytical Results
for Treatment Oil					7-13
7-8 Chlorodibenzofuran and Chlorodibenzodioxin Analytical Results
for Day 2 Composite Sludge Liquid	 7-14
7-9 Chlorodibenzofuran and Chlorodibenzodioxin Analytical Results
for Day 4 Composite Sludge Liquid			 7-15
7-10 Chlorodibenzofuran and Chlorodibenzodioxin Analytical Results
for Day 2 Composite Ash			 7-16
7-11 Chlorodibenzofuran and Chlorodibenzodioxin Analytical Results
for Day 3 Composite Ash			 7-17
7-12 Chlorodibenzofuran and Chlorodibenzodioxin Analytical Results
for Day 4 Composite Ash	 7-18
ix

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TABLES (Concluded)
Number	Page
8-1 Characterization of Penta and Creosote Treating Cylinder
Spillage and Drippage 		 8-3
8-2 Qualitative Organic Analysis Results for Fugitive
Emissions	 8-5
8-3 Summary of Total Hydrocarbon Determinations Performed at
a Common Vacuum Vent 	 8-6
8-4 Summary of Specific Low-Molecular-Weight Hydrocarbon
Determinations at a Common Vacuum Vent 		 8-7
8-5 Treating Cycle Sequence 	 8-8
x

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ABBREVIATIONS
LIST OF ABBREVIATIONS AND SYMBOLS
SYMBOLS
xi

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ACKNOWLEDGMENTS
Acurex gratefully recognizes the technical contributions of the
following staff members: Mr. Bruce DaRos for his supervision of the field
test program and sample collections; Dr. Bill Fitch for his contributions 1n
data analysis; Dr. Dean Wolbach for his contributions 1n data Interpretation
and report preparation. This document was compiled and drafted, in part, by
Mr. Richard Merrill, Program Manager.
Acurex is particularly indebted to Mr. Donald Wilson, Project Officer,
IERL, Cincinnati, for his continued support, guidance, and sustained interest
in the project. Finally, Acurex would like to thank the private sector
personnel for their interest and participation 1n this project.
x11

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SECTION 1
INTRODUCTION
The wood preserving industry consists of approximately 475 production
plants owned by approximately 300 companies. The primary products of this
industry are utility poles, railroad ties, and construction materials,
chemically treated to resist insect and fungi attack, improve weathering
characteristics, and promote insolubility in water and fire retardance. The
preservatives used to produce the desired product characteristics include
creosote, a coal tar derivative; pentachlorophenol, a crystalline compound
dissolved in light aromatic oil; and waterborne salts of arsenic, chromium,
copper, zinc, and fluoride.
The application of the preservatives requires certain processing
steps. The wood must first be debarked, formed (cut to size and shaped as
necessary), and conditioned. The conditioning step removes the water from the
wood, increasing its permeability and ability to accept the preservatives.
Drying the wood can be done by air seasoning, tunnel drying, or kiln drying,
all independent of the preserving step. The wood may also be conditioned in
combination with the preserving step as in steam conditioning, boultonizing,
or vapor drying. Each of these latter processes generates a wastewater stream
containing wood extracts'and preservatives which must be disposed of.
The toxic nature of the preservatives used by the wood industry has led
the Effluent Guidelines Division of the Environmental Protection Agency (EPA)
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to promulgate regulations governing the disposal of the generated wastewater.
The regulations presently in effect which do not allow the discharge of
wastewater outside plant boundaries have led plant operators to develop
treatment technologies other than direct discharge. The primary purpose of
this report is to discuss the results of test programs conducted to quantify
the uncontrolled transfer of toxic organic species contained in the wastewater
to other medias.
The wastewater treatment or disposal technologies developed by the
industry include plant modifications, improved oil/water separation,
wastewater treatment, and evaporation. Evaporation includes thermal (pan)
evaporation, cooling towers, spray ponds, and solar ponds. Under EPA contract
68-03-2584, an operating cooling tower was tested which showed virtually no
discharge of organics. In addition, the thermal (pan) evaporation technique
was evaluated in the laboratory; this work showed a significant fraction of
the organic compounds in the wastewater being discharged to the atmosphere.
To verify the release of organics from thermal (pan) evaporators, task 28 of
EPA contract 68-03-2567 was funded. Also Included 1n this task was the field
testing of a spray evaporation pond and examination of wastewater disposal in
an industrial steam boiler.
The scope of task 28 included plant identification, plant surveys, and
site selections. The program objectives were to qualitatively and
quantitatively evaluate multimedia emissions from a thermal (pan) evaporation
device (Including fugitive emissions from the treatment system), a spray pond
system, and an industrial boiler using the oil-laden wastewater as
supplemental fuel.
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Section 2 of this report presents the conclusions reached during the
execution of this task, followed by the recommendations in Section 3.
Section 4 discusses the wastewater evaporation options available to plant
operators, as well as thermal destruction of the wastewater. Sections 5
through 7 discuss the results of the thermal (pan) evaporation, the spray
evaporation, and the boiler disposal test programs, respectively. Finally,
Section 8 presents the fugitive emissions assessment.
Three appendices, one for each test program, presents all the details
of the field sampling programs. Included in each appendix is the data
collected in the field for that test program.
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SECTION 2
CONCLUSIONS


The results of this program confirmed the discharge of orgarii
compounds during wastewater evaporation in thermal (pan) evaporators and
showed that the emissions were greater than usual predictive methods woul
in<
Spray pond emissions were such that the cryogenic sampling systems
used did not yield enough sample material to reach the sensitivity needed to
detect the low volatility components of the wastewater. Therefore, of the
evaporation systems studied, thermal (pan) evaporation is the least
satisfactory and spray ponds the most satisfactory in terms of organic
emissions.
The destruction of the organic compounds in an industrial steam boiler
may be a viable disposal option if the boiler is designed properly. The L- ( 1
system tested did not reach a 99.99 percent destruction efficiency, and
certain dioxins and furans were present in the ash streams.
Industrywide, the air emissions from wastewater handling are on the
order of 50 to 100 metric tons/year. Major fugitive emissions, although of
high concentration, are of relatively short duration and low volume.
though localized problems may occur, the industry as a whole is not a
lificant emitter of organics to the atmosphere./ Table 2-1 presents a
l 11 vju yi
V^signv
summary of the organic emissions discharged from the evaporation devices.
2-1

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TABLE 2-1. SUMMARY TABLE
Emissions concentration
(ppm or ug/g)
Thermal evaporator
Spray pond evaporator
Retort emissions
Vacuum vent emissions
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SECTION 3
RECOMMENDATIONS
If evaporation technology is to be employed, thermal (pan) evaporation
is the greatest emitter of organic components to the atmosphere and its use
should be minimized. Regardless of the evaporator useq^ care should be taken
to develop oil/water separation techniques which minimize oil and sludge
carryover to the evaporator. Further, a program should be conducted to
establish the best available separation systems or to develop methods to
enhance the operation of existing systems.
The destruction of wood preserving wastes in boilers is a viable
disposal technology if the boiler is designed appropriately. It is
recommended that a program be conducted to determine the proper injection
(atomization) methods, and the residence times and temperatures necessary to
completely destroy the organics in the waste. This incineration study also
should be extended to the ash and sludge. Larger ash and sludge samples
should be taken to obtain a better speciation and quantitation of the
chlorinated dibenzo-p-dioxins and chlorinated dibenzofurans. In addition a
careful evaluation should be conducted of the partitioning of these organic
components between the bottom ash, mechanical hopper ash, and baghouse ash.
3-1

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SECTION.4
WASTEWATER TREATMENT AND DISPOSAL BY EVAPORATION OR THERMAL DESTRUCTION
The treatment of wood with preservatives requires impregnation of the
wood with toxic materials designed to protect it from attack by insects,
fungi, weather, or fire. The processing steps include wood preparation
(debarking, shaping, drying) and preservative application. The preservative
can be applied using either pressure or nonpressure techniques. Nonpressure
techniques are used when only minimal treatment is necessary. Pressure
processes require the use of pressure or vacuum steps, either for preservative
application or for combinations of wood conditioning (to increase
permeability) and preservative application. Wood conditioning processes
generate steam (due to the water content of the wood and the
pressure/temperature/vacuum operations) which contains wood extractives and
organic constituents from the preservative formulation. The heat content of
the steam volatilizes low-molecular-weight organic compounds such as benzene
and toluene, or atomizes drops of emulsified preservative, carrier oil, and
water. When the resulting vapors are removed from the retort and condensed,
the condensate contains water, free oils (and preservatives), emulsified oils
(and preservatives), and wood extractives. Following removal of the free
oils, the wastewater stream is transported to a disposal facility.
Industry's technical response to requirements for process wastewater
control has included increased evaporation of water using thermal (pan)
4-1

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evaporators, spray and solar ponds, and cooling towers to decrease aqueous
discharges. The principle behind the evaporation of the wastewater is to
dispose of the water fraction while leaving the organic constituent for
subsequent recycling to the process or landfill disposal. Since volatile and
other low-molecular-weight organic constituents are present in the wastewater,
they may be released to the atmosphere. This section describes each
evaporation device and summarizes the emissions from it.
4.1 SURFACE EVAPORATION EMISSIONS
While evaporative processes allow plant operators to achieve zero
wastewater discharge, they are operated under the assumption that no organic
compounds are transferred to the air. Under EPA contract 68-03-2584, a
program was conducted to determine if organic compounds were emitted to the
atmosphere. The primary results of this program showed that organic
components of the wastewater were discharged during evaporation.
The mathematical expression for the evaporation rate of chlorinated
phenolic and other organic chemical pollutants from the surface of wastewater
evaporation systems (thermal ponds or pan evaporators) can be developed from
Fick's first law of diffusion. The following qualifying assumptions must be
made:
•	The system is at steady state (i.e., the liquid is at equilibrium
with the gas at the liquid surface)
•	The wastewater is an ideal solution
t There is a stagnant layer of air above the pond
•	The vaporized organic compound forms an ideal gas mixture with air
•	The solubility of air in the wastewater is negligible
•	There is constant temperature and pressure in the stagnant air layer
4-2

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With these assumptions, the minimum evaporation rate of each organic
pollutant in the wastewater can be estimated using equation 1. This equation
is expressed in terms of total and partial pressures:
N. = molar flux of species A into B in the z direction,
-2 -1
gmoles L t
Pj = total pressure, atm
°AB = binary diffusivity for system composed of species A and B,
lV1
P« = partial pressure of species A, atm
Z
R = gas constant, 82.05 cm"* atm gmole"^°K"^
T = ambient air temperature, °K
z2~z\ ~ l"1 thickness, cm
This expression shows the diffusivity and partial pressures impact on the rate
of organic emissions: as temperature increases, the diffusivity increases.
Therefore, higher-molecular-weight compounds can be driven out of solution.
In estimating the evaporation rate of organic vapors into air, it is
assumed that the diffusion layer (z2-z1) is finite, that the air is
stagnant and insoluble in the organic compound within that layer, and that the
contained wastewater surface is quiescent. Therefore, if the air above the
surface is turbulent, Z2~zi approaches zero, maximizing the transfer rate
of the organics to the atmosphere.
The diffusivity and vapor pressures calculated from these equations can
be used in estimating the evaporation rate of a pure organic liquid into air
if the organic constituents formed a layer over the wastewater. To estimate
(1)
where:
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the evaporation rate of an organic liquid from an aqueous solution (emulsion),
it is assumed that the organic compound forms an ideal solution with water and
that its vapor forms an ideal mixture in air. The evaporation rate of the
organic from the solution is given by the product of the pure liquid
evaporation rate and the mole fraction of organic in the wastewater.
It then was demonstrated in the laboratory that organic material is
stripped from water solutions. The transfer of chlorinated organics from
water solutions to the atmosphere is controlled by their rate of diffusion and
concentration in water and the thermal driving force.
This evaporation model is applicable to solar ponds and thermal (pan)
evaporators. A solar pond is a contained area where the wastewater is placed
and allowed to evaporate. The pond may be lined or unlined. An unlined pond
depends on soil attenuation to prevent organic materials from entering
underlying aquifers. A lined pond is designed so that the evaporation rate
exceeds the annual precipitation rate for a given geographical area. Solar
ponds require large land usage, and federal regulations now require that ponds
containing hazardous materials meet berm maintenance requirements and use
monitoring wells for leachate control. These regulations may cause plant
operators to install other evaporation technology.
The evaporation process can be accelerated by applying heat directly to
evaporate the water, as in a thermal (pan) evaporator. In this system, the
wastewater is contained in a vessel, such as a tank or lined pond, with an
external heat source, such as boiler steam or the condenser system, to
increase the solution temperature. The wastewater can be used as a cooling
fluid to condense the vapor from the retort then recycle back to the
4-4

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evaporation system. Again, as the temperature is increased, an increase in
organic emissions is predicted.
4.2 DROPLET EVAPORATION EMISSIONS
Another mechanism for enhancing evaporation is the formation of
droplets. This method creates large liquid surface areas, promoting greater
liquid/air contact and accelerated evaporation rates.
The evaporation rate of organic compounds from a droplet of wastewater
can be estimated using an equation for the evaporation rate of a free-falling
drop. Assuming that the evaporation rate is sufficiently small not to distort
the velocity and concentration profiles, and that the mass transfer
coefficient is independent of mass transfer rate, the resulting equation for
predicting the evaporation rate is shown in equation 2:
W
where:
„DC*Da xa. xa
n f a . o oo
a —r~ 1 - xa
ao
DV pf*1/2
2.0 + 0.60 ( -jjf0 T
(2)
Wa = evaporation rate, gmole/sec
D = droplet diameter, cm
Cf = molar concentration of air, 3.88 x 10"^ gmole/cc
Da a diffusivity, cm^/sec
Xa = vapor pressure of the liquid
V,,, = velocity of droplet (assume terminal velocity), cm/sec
pf = density of air, 1.12 x 10"3 g/cc
Mf = viscosity of air
This evaporation system again is impacted by diffusivity and partial pressure;
air resistance also affects the rate of evaporation.
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This evaporation model is applicable to spray pond systems and cooling
towers. A spray pond is a contained area (lined or unlined pond) which has a
pumping system connected to spray nozzles. This system decreases both the
land required by a solar pond and the effect of negative climatic impacts.
The use of a cooling tower is only applicable to Boulton conditioning
systems. As the water vapor from the retort is condensed, it gives up heat.
The condensed wastewater is accumulated, then sent to the oil/water
separator. The effluent wastewater from the oil/water separator is added to
the cooling water that recirculates through the condenser aid sent through the
cooling tower: the waste heat promotes evaporation. In steaming plants, there
is insufficient waste heat to evaporate the volume of wastewater generated.
A field test program was conducted at a site utilizing a cooling tower
to measure the presence of organic compounds in the air stream. It was found
that low-molecular-weight compounds were emitted to the atmosphere but that
nonvolatile organics remained in solution.
Other evaporation processes are used by the wood preserving industry
such as land irrigation. The wastewater is sprayed onto a field, during which
droplet evaporation occurs, after which solar evaporation takes place and
water percolates into the soil.
4.3 EMISSIONS SUMMARY
Each of the treatment processes discussed results in the formation of a
sludge. The amount of solid waste material generated depends on the
preservative used, and the effectiveness of the oil/water separator and the
treatment technologies employed. This material is typically disposed in
landfills (onsite, if land is available, or offsite). Incineration of solid
waste is not now widely practiced.
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Other sources of organic emissions, in addition to the evaporator
discharge, include fugitive emissions such as the dense vapor plumes emitted
as the pressure vessel is opened and wood charge removed, and emissions from
the treated wood as it cools and the vacuum exhaust. Quantifying data
describing the emissions were not identified in the literature. A primary
Purpose of this program was to collect additional field data to further
evaluate the multimedia emissions and disposal options available to the wood
Preserving industry.
4-7

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SECTION 5
CHARACTERIZATION OF MULTIMEDIA EMISSIONS FROM A THERMAL (PAN)
EVAPORATION DEVICE
A field test program was conducted at a wood preserving plant using
thermal (pan) evaporation to reduce its generated wastewater volume. The
program was designed to determine the organic emissions from two thermal (pan)
evaporators, one evaporating wastewater containing penta and other chlorinated
phenolic compounds, and one evaporating wastewater containing creosote
components (polynuclear aromatic hydrocarbons (PAH's)). Each stream was
qualitatively and semiquantitatively analyzed for organic compounds, including
chlorinated phenols, chlorinated dibenzo-p-dioxins, chlorinated dibenzofurans,
and PAH's.
5.1 PROGRAM DESCRIPTION AND RESULTS
This program focused on those primary multimedia effluents generated by
the plant that were expected to have the greatest environmental impact in
terms of gaseous and solid discharges. The sampling points of interest were
the ducted air emissions and solid wastes from wastewater treatment. Material
balance estimates were conducted around each evaporator. A primary objective
of this program was to quantitate the emission rate of organic compounds from
the evaporation devices.
5.1.1 Test Site
The wood treating facility selected for field testing employed two
treating cylinders using the Boulton conditioning process. One cylinder could
5-1

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treat wood with penta formulations, while the other cylinder could treat wood
with either penta or creosote.
Condensate generated from the individual treating processes was handled
by discrete subsurface oil/water separators on a batch basis. The recovered
oil fraction was returned to bulk storage tanks for reuse in the process.
Separated sludges and wastewater were routed to the appropriate thermal (pan)
evaporators — one penta and one creosote — for volume reduction. Figure 5-1
presents a schematic of the plant wastewater/preservative recovery system.
Each evaporator was operated on a semi batch basis. As the wastewaters
were transferred to their respective evaporators, steam from the boilers was
pumped through steam coils in the tanks to heat the wastewaters to boiling,
driving off the water. This process was continued until an oil/preservative
layer accumulated which was returned to the preservative work tanks.
Semiannually the evaporators were opened, and the nonpumpable sludge layer
removed and shipped offsite to a landfill.
5.1.2 Field Test Program
The sampling program conducted included each of these tests:
•	Source emission sampling at the penta and creosote thermal (pan)
evaporator outlets
•	Total hydrocarbon determinations at each air emission point
t Specific low-molecular-weight hydrocarbon determinations at each
emission point
•	Grab samples of:
—	Penta thermal (pan) evaporator contents
—	Creosote thermal (pan) evaporator contents
—	Bulk penta in treating oil
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Cooling pond
spray tower
Figure 5-1. Schematic of wood preserving plant wastewater/preservative
recovery system.
5-3

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—	Bulk creosote
—	Penta oil/water separator (both fractions)
—	Creosote oil/water separator (both fractions)
The sample collection matrix is shown in table 5-1. Source emissions sampling
was conducted using the EPA Method 5 sampling train with XAD-2 resins for
nonvolatile organic compounds. Volatile organic emissions were measured using
field gas chromatography (GC) techniques. Samples of the liquid fractions
were randomly collected by grab sampling during each test series. A complete
discussion of the field testing and the test data are contained in appendix A,
5.1.3 Data Presentation for Pan Evaporation
The concentration data for the pan evaporator tests are given in
tables 5-2 to 5-7. Average values for the penta pan evaporator tests and the
creosote pan evaporator tests are shown in tables 5-8 and 5-9, respectively.
Note that in test 4 on the penta evaporator, the units of emission are in
g/sm3, rather than mg/sm3 for all other tests.
Concentrations of evaporator gaseous emissions are calculated by
dividing the total milligrams of the component collected in the organic resins
by the water volume collected in the impinger train; the water volume data are
corrected to standard gas volume. For example, during test 4 on the penta
evaporator, 24,000 mg (24g) of penta was collected. The condensed water
volume collected was 598 ml. This translates to 1.76 m3 of water vapor at
23°C and 1 atm, as follows:
1 mole 22.414 liters v 296°K w 10"3m3
598g H?0£ x	x " —		 x	* T^
2 18g mole (0°C, 1 atm) 273°K 1iter
(1)
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TABLE 5-1. SUMMARY OF COLLECTED SAMPLES
Sample location number
1
2
3
4
Location
description
Collection method
Penta
oil/
water
retort
Creosote
oil /
water
separator
Penta
evaporator
Creosote
evaporator
Day 1 (Setup)
Day 2
XAD-2
Field GC
Liquid grab sample
Solid grab sample
X (2)
X (2)
X X X X
ro
CVJ
X X X X
Day 3
XAD-2
Field GC
Liquid grab sample
Solid grab sample
X (2)
X (2)
X X X X
ro
CM
X X X X
Day 4
XAD-2
Field GC
Liquid grab sample
Solid grab sample
X (2)
X (2)
X x x X
ro
X X X X
ro
Day 5 (Cleanup)
5-5

-------
TABLE 5-2. PENTA PAN EVAPORATOR — TEST 2
Stream
Working
solution
Oil/water
recycle
Waste-
water
Pan
water
Pan
sludge
Pan
vent
Date
9/23
9/24
9/24
9/24
9/23
9/24
Time
—
1300
1245
0900
—
1200
Concentration*






Penta
44,COO
40,000
14,000
140
6.2
1.8
Phenol
<200
<10
<10
0.5
1.2
<0.5
Fluoranthene
430
3,800
970
7.9
2.0
1.0
Naphthalene
3,800
3,700
1,500
0.4
1.1
2.0
Benzo(a)anthracene
<100
540
200
3.7
0.5
0.11
Benzo(a)pyrene
<100
110
40
0.1
0.05
<0.1
Benzofluoranthenes
<100
380
110
0.1
0.2
<0.1
Chrysene
<100
520
180
3.7
0.4
0.10
Acenaphthylene
170
140
310
0.1
0.05
<0.1
Anthracene
230
400
180
1.2
0.5
0.17
Benzo(g,h,i)perylene
<200
30
<10
<0.1
0.1
<0.1
Fluorene
1,100
2,700
850
1.4
1.0
<0.1
Phenanthrene
1,700
5,000
1,800
9.5
3.5
1.0
Dibenzo(a,h)
<200
4
<10
<0.1
0.1
<0.5
anthracene






Indeno(l,2,3-c,d)
<200
15
<10
<0.1
0.1
<0.5
pyrene






Pyrene
350
3,500
710
6.1
1.4
0.8
Benzene
<1
0.3
<10
<0.1
0.2
NA
Toluene
18
27
<10
<0.1
0.3
NA
Ethylbenzene
23
19
<10
<0.1
0.2
NA
~Concentration units are yg/g (ppm w/w) for solids, ug/ml (ppm w/w) for
liquids, and mg/sm3 (at 23°C, 1 atm) for gases
5-6

-------
TABLE 5-3. PENTA PAN EVAPORATOR — TEST 3

Working
Oil/water
Waste-
Pan
Pan
Pan
Stream
solution
recycle
water
water
sludge
vent
Date
9/23
9/25
9/25
9/25
9/23
9/25
Time
—
1500
1510
—
—
0800
Concentration*






Penta
44,000
45,000
980
70
6,2
3.4
Phenol
<200
<10
<10
0.4
1.2
0.65
Fluoranthene
430
2,800
2,000
2.7
2.0
5.2
Naphthalene
3,800
2,000
220
0.1
1.1
3.0
Benzo(a)anthracene
<100
430
290
1.4
0.5
0.29
Benzo(a)pyrene
<100
96
68
<0.1
0.05
<0.1
Benzofluoranthenes
<100
320
190
<0.1
0.2
<0.1
Chrysene
<100
400
420
1.0
0.4
0.26
Acenaphthylene
170
370
1,600
0.3
0.05
1.3
Anthracene
230
1,100
400
0.4
0.5
2.3
Benzo(g,h,i)perylene
<200
7
<20
<0.1
<0.1
<0.1
Fluorene
1,100
2,400
2,100
2.6
1.0
3.1
Phenanthrene
1,700
4,000
3,600
2.4
3.5
9.2
Dibenzo(a,h)anthracene
<200
<10
<20
<0.1
<0.1
<0.1
Indeno(1,2,3-c,d)pyrene
<200
28
<20
<0.1
<0.1
<0.1
Pyrene
350
1,900
1,300
2.0
1.4
3.2
Benzene
<1
1.2
0.2
<0.2
<0.2

Toluene
18
77
0.1
<0.2
0.3

Ethylbenzene
23
2.3
1.2
<0.2
<0.2

~Concentration units are ug/g (ppm w/w) for solids, ng/ml (ppm w/w) for
liquids, and mg/sm3 (at 23°C, 1 atm) for gases
5-7

-------
TABLE 5-4. PENTA PAN EVAPORATOR — TEST 4

Working
Oil/water
Waste-

Pan
Pan
Pan
Stream
solution
recycle
water

water
sludge
vent
Date
9/23
9/25
9/25

9/26
9/23
-•v.
9/26
Time
—
1500
1510

—
—
1135
Concentration*







Penta
44,000
45,000
980

41
6.2
30
Phenol
<200
<10
<10

0.3
1.2
0.52
Fluoranthene
430
2,800
2,000

1.2
2.0
1.7
Naphthalene
3,800
2,000
220

0.3
1.1
5.8
Benzo(a)anthracene
<100
430
290

0.9
0.5
0.20
Benzo(a)pyrene
<100
96
68

<0.1
0.05
<5x10-3
Benzofluoranthenes
<100
320
190

<0.1
0.2
0.043
Chrysene
<100
400
420

0.7
0.4
0.190
Acenaphthylene
170
370
1,600

0.1
0.05
1.370
Anthracene
230
1,100
400

0.2
0.5
0.740
Benzo(g,h,i)perylene
<200
7
<20

<0.1
<0.1
<5x10-3
Fluorene
1,100
2,400
2,100

1.7
1.0
1.7
Phenanthrene
1,700
4,000
3,600

1.5
3.5
1.5
D i benzo(a,h)an thr acene
<200
<10
<20

<0.1
<0.1
<5x10-3
Indeno(1,2,3-c,d)pyrene
<200
28
<20

<0.1
<0.1
<5x10-3
Pyrene
350
1,900
1,300

0.9
1.4
1.4
Benzene
<1
1.2
0.
2
<0.2
<0.2

Toluene
18
77
0.
1
0.2
0.3

Ethylbenzene
23
2.3
1.
2
0.2
<0.2

~Concentration units are ug/g (ppm w/w) for solids, ug/ml (ppm w/w) for
liquids, and mg/snw (at 23°C, 1 atm) for gases
5-8

-------
TABLE 5-5. CREOSOTE PAN EVAPORATOR — TEST 2

Working
Oil/water
Waste-
Pan
Pan
Pan
Stream
solution
recycle
water
water
sludge
vent
Date
9/23
9/24
9/24
9/24
9/23
9/24
Time
—
—
—
0830
—
1450
Concentration*






Penta
17,000
3,600
12
3.4
26.0
<0.15
Phenol
400
1,500
7
11
30
15
Fluoranthene
32,000
33,000
20
20
590
25
Naphthalene
24,000
33,000
42
13
680
200
Benzo(a)anthracene
20,000
23,000
10
14
390
0.4
Benzo(a)pyrene
600
610
2
24
91
<0.05
Benzofluoranthenes
650
530
4
5.7
190
0.05
Chrysene
15,000
19,000
10
8.9
240
0.3
Acenaphthylene
5,700
3,400
2
1.2
840
7
Anthracene
12,000
69,000
7
9.9
260
32
Benzo(g,h,i)perylene
<500
<500
0.2
0.6
10
<0.05
Fluorene
36,000
38,000
16
2.5
660
110
Phenanthrene
37,000
41,000
19
3.2
1100
98
Dibenzo(a,h)anthracene
<500
<500
0.2
0.9
<10
<0.05
Indeno(1,2,3-c,d)pyrene
<500
<500
0.3
0.7
16
<0.05
Pyrene
27,000
27,000
15
16
440
16
Benzene
26
<50
<0.1
<0.1
6.7

Toluene
2.7
<50
<0.1
<0.1
1.4

Ethylbenzene
<0.5
<50
<0.1
<0.1
0.3

~Concentration units are pg/g (ppm w/w) for solids, yg/ml (ppm w/w) for
liquids, and mg/sm3 (at 23°C, 1 atm) for gases

-------
TABLE 5-6. CREOSOTE PAN EVAPORATOR — TEST 3
Stream
Work ing
solution
Oil/water
recycle
Waste-
water
Pan
water
Pan
sludge
Pan
vent
Date
9/23
9/25
9/25
9/25
9/23
9/25
Time
—
—
—
—
—
1005
Concentration*






Penta
17,000
1,300
8.3
7.6
26.0
2.7
Phenol
400
800
5.2
31
30
58
Fluoranthene
32,000
13,000
140
9.3
590
2° „
Naphthalene
24,000
38,000
200
10
680
2.7x103
Benzo(a)anthracene
20,000
9,200
60
4.5
390
1.4
Benzo(a)pyrene
600
3,000
6.1
0.6
91
0.2
Benzofluoranthenes
650
500
15
1.4
190
0.7
Chrysene
15,000
5,400
50
3.7
240
1.2
Acenaphthylene
5,700
5,700
6
0.3
840
29
Anthracene
12,000
8,000
56
2.8
260
68
Benzo(g,h,i)perylene
<500
730
<10
<0.1
10
<0.05
Fluorene
36,000
35,000
110
8.9
660
550
Phenanthrene
37,000
22,000
190
15
1100
200
Di benzo(a,h) an thr acene
<500
1,500
<10
<0.1
<10
<0.05
Indeno(l,2,3-c,d)pyrene
<500
1,300
<10
0.1
16
<0.05
Pyrene
27,000
10,000
100
6.7
440
13
Benzene
26
27
<0.1
<0.1
6.7

Toluene
2.7
0.5
<0.1
<0.1
1.4

Ethylbenzene
<0.5
6.8
<0.1
<0.1
0.3

~Concentration units are yg/g (ppm w/w) for solids, wg/ml (ppm w/w) for
liquids, and mg/sm3 (at 23°C, 1 atm) for gases
5-10

-------
TABLE 5-7. CREOSOTE PAN EVAPORATOR — TEST 4

Working
Oil/water
Waste-
Pan
Pan
Pan
Stream
solution
recycle
water
water
sludge
vent
Date
9/23
9/25
9/25
9/25
9/23
9/25
Time
—
—
—
—
—
1300
Concentration*






Penta
17,000
1,300
8.3
0.5
26.0
1.6
Phenol
400
800
5.2
35
30
<0.05
Fluoranthene
32,000
13,000
140
6.0
590
21
Naphthalene
24,000
38,000
200
6 4
680
2.2x103
Benzo(a)anthracene
20,000
9,200
60
2.4
390
1.2
Benzo(a)pyrene
600
3,000
6.1
0.4
91
0.3
Benzofluoranthenes
650
500
15
0.8
190
1.3
Chrysene
15,000
5,400
50
1.9
240
0.9
Acenaphthylene
5,700
5,700
6
0.2
840
44
Anthracene
12,000
8,000
56
1.4
260
44
Benzo(g,h,i)perylene
<500
730
<10
<0.1
10
<0.05
Fluorene
36,000
35,000
110
6.0
660
580
Phenanthrene
37,000
22,000
190
12
1100
260
D i benzo (a, h) an thr acene
<500
1,500
<10
<0.1
<10
<0.05
Indeno(l,2,3-c,d)pyrene
<500
1,300
<10
<0.1
16
<0.05
Pyrene
27,000
10,000
100
4.2
440
16
Benzene
26
27
<0.1
3.4
6.7

Toluene
2.7
0.5
<0.1
<0.2
1.4

Ethylbenzene
<0.5
6.8
<0.1
0.3
0.3

~Concentration units are yg/g (ppm w/w) for solids, pg/ml (ppm w/w) for
liquids, and mg/sm3 (at 23°C, 1 atm) for gases
5-11

-------
TABLE 5-8. PENTA PAN EVAPORATOR — AVERAGE VALUES

Working
Oil/water
Waste-
Pan
Pan
Pan
Stream
solution
recycle
water
water
sludge
vent
Volume*


3,400
8xl04
109
6xl03
Concentration**





10*
Penta
44,000
42,000
7,000
80
6.2
Phenol
<200
<10
<10
0.6
1.2
200
Fluoranthene
430
3,300
1,500
4.3
2.0
600
Naphthalene
3,800
2,800
850
0.2
1.1
2xl03
Benzo(a)anthracene
<100
480
250
1.9
0.5
70
Benzo(a)pyrene
<100
100
60
<0.1
0.05
<5
Benzofluoranthenes
<100
350
150
<0.1
0.2
10
Chrysene
<100
460
300
1.7
0.4
60
Acenaphthylene
170
260
950
0.2
0.05
100
Anthracene
230
750
290
0.6
0.5
300
Benzo(g,h,i)perylene
<200
18
<10
<0.1
0.1
<5
Fluorene
1,100
2,600
1,500
1.5
1.0
600
Phenanthrene
1,700
4,500
2,700
4.0
3.5
500
D i benzo(a,h)an thr acene
<200
4
<10
<0.1
0.1
<5
Indeno(l,2,3-c,d)pyrene
<200
22
<10
<0.1
0.1
<5
Pyrene
350
2,700
1,000
3.2
1.4
500
Benzene
<1
6
<10
<0.2
<0.2
<5
Toluene
18
54
<10
<0.2
0.3
<5
Ethylbenzene
23
10
<10
<0.2
<0.2
<5
~Solid and liquid flowrates are averages based on monthly production figures
(kg/day or 1/day). Gas volumes are based on average daily decreases in tank
volume (sm3/day).
~~Concentration units are yg/g (ppm w/w) for solids, yg/ml (ppm w/w) for
liquids, and mg/sm3 (at 23°C, 1 atm) for gases
5-12

-------
TABLE 5-9. CREOSOTE PAN EVAPORATOR — AVERAGE VALUES

Working
Oil/water
Waste-
Pan
Pan
Pan
Stream
solution
recycle
water
water
sludge
vent
Volume*
_

5200
40000
114
7300



1/day
1
kg/day
sm3/day
Concentration**






Penta
17,000
2,500
10
6.2
26.0
2
Phenol
400
1,100
6
23
30
30
Fluoranthene
32,000
23,000
80
25
590
23
Naphthalene
24,000
36,000
120
12
680
2.5xl03
Benzo(a)anthracene
20,000
16,000
35
16
390
1
Benzo(a)pyrene
600
1,800
4
6.7
91
<0.2
Benzofluoranthenes
650
520
10
3
190
0.6
Chrysene
15,000
12,000
30
10
240
0.8
Acenaphthylene
5,700
4,600
4
1.4
840
30
Anthracene
12,000
39,000
30
10
260
50
Benzo(g,h,i)perylene
<500
600
<5
<0.1
10
<0.05
Fluorene
36,000
37,000
63
27
660
400
Phenanthrene
37,000
32,000
110
34
1100
190
D i benzo (a, h) an thr acene
<500
1,000
<5
0.2
<10
<0.05
Indeno(l,2,3-c,d)pyrene
<500
900
<5
<0.2
16
<0.05
Pyrene
27,000
18,000
55
19
440
15
Benzene
26
<40
<0.1
<0.1
6.7

Toluene
2.7
<25
<0.1
<0.1
1.4

Ethylbenzene
<0.5
<25
<0.1
<0.1
0.3

~Solid and liquid flowrates are averages based on monthly production figures
(kg/day or 1/day). Gas volumes are based on average daily decreases in tank
volume (sm3/day).
~~Concentration units are ug/g (ppm w/w) for solids, yg/ml (ppm w/w) for
liquids, and mg/sm3 (at 23°C, 1 atm) for gases
5-13

-------
Thus, the average concentration of penta leaving the evaporator during the
test was:
24 " 1()3 W - 3 x 104 mg/sm3	<2'
0.807 sni
System flowrates are based on plant operating information and field
measurements. Between November 19 and December 31, 1980, the test plant
generated 25,000 gal of wastewater from the creosote process and 16,000 gal
from the penta process. The plant was on a 3-day/week treatment schedule for
18 days. The generation rates are calculated at approximately 5,200 1/day
(1,400 gal/day) for the creosote process and 3,400 1/day (890 gal/day) for the
penta process.
Between September 10 and November 18, 1980, 41,000 gal of water were
evaporated in the penta pan evaporator, and 20 barrels (approximately 550 lb
each) of sludge were recovered for disposal. Thus, approximately 32g
sludge/liter of wastewater (0.27 lb/gal) were generated. For the creosote pan
evaporator, the corresponding numbers are 73,000 gal, 24 barrels, and 22 g/1
(0.15 lb/gal). From this, the rate of sludge generation is calculated to be
114 and 109 kg/day for the creosote and penta pan evaporators, respectively.
The driving force for vent emissions from the evaporator is boiling
water. Volume emission rates based on pure water vapor are calculated from
the rate volume change in the evaporators.
Given the diameter of the creosote evaporator (11 ft) and the average
rate of change in the liquid height (0.997 inch/hr), the volume of water
evaporated is estimated to be 5,370 1/day (1,420 gal/day), in agreement with
the input rate. The corresponding numbers for the penta evaporator are 12—ft
5-14

-------
diameter, 0.698 inch/hr, and 4,470 1/day (1,180 gal/day) with approximate
agreement. The liquid volumes are converted into the following gas volumes:
•	7.3 x 10 snr/day from the creosote evaporator
o q
•	6 x 10 snr/day from the penta evaporator
A summary of sampling times and volumes is given in table 5-10. A
schematic of the process, showing sample locations, is presented in figure 5-2.
5.1.4 Material Balances Around Evaporators
Material balance calculations made around each evaporator are shown in
tables 5-11 and 5-12. Volume flowrates are the average daily rates calculated
in the previous section. Values for the bulk streams are in kg/hr, including
water from the vents; values for individual components are in g/hr*
The air emissions rate is predicted for each component by subtracting
the output rate in the sludge from the input rate in the wastewater. The high
vent rate uses the highest concentration of the component observed during
testing, while the low value is from the lowest concentration observed. Both
cases use the average volume rate of water boiled off. The average emission
rate is the average of the high and low rates, not the rate calculated from
the average vent concentration.
The average emission rate cannot be used for estimating emissions. As
will be shown, a true average emission rate must be time weighted. Because
the amount of time during the evaporation cycle that each component is emitted
at a high concentration is not known, the time-weighted average is not
available. A study of the tables, however, shows that the predicted emission
rate falls between the high and low observed rates, making a fair estimate of
the average hourly emissions. Table 5-13 shows the percent of input emitted
to the atmosphere based on this average hourly rate: over 80 percent of
almost every component (and 100 percent of some) are transferred to the air.
5-15

-------
TABLE 5-10. SAMPLING DATA





Water
Water
Location/

Start
Stop
Sample
volume*
volume**
run number
Date
time
time
time
(ml)
(sm^)
Penta 2
9/24/80
1208
1238
30
1301.6
1.758
3
9/25/80
0806
0825.5
19.5
972.5
1.314
4
9/26/80
1135
1150
15
598.0
0.806
Creosote Z
9/24/80
1451
1547
56.
1130.4
1.524
3
5/25/80
1005
1050
45
762.3
1.028
4
9/25/80
1302
1313.5
11.5
945.6
1.275
~Liquid
**Gas at 23°C and 1 atm (73°F and 760 mm Hg)
5-16

-------
To atmosphere
To atmosphere
Figure 5-2. Sampling locations for thermal (pan) evaporator tests
and fugitive emissions tests.

-------
TABLE 5-11. CREOSOTE PAN EVAPORATOR — MATERIAL BALANCE
Stream name



Obs
Obs


Pred
high
low


pan
pan
pan

Sludge
vent
vent
vent
Wastewater
out
out
out
out
in (g/hr)
(g/hr)
(g/hr)
(g/hr)
(g/hr)
Obs avg
pan
vent
out
Stream (x 10"^)
Penta
Phenol
Fluoranthene
Naphthalene
Benzo(a)anthracene
Benzo(a)pyrene
Benzof1uor anthenes
Chrysene
Acenaphthylene
Anthracene
Benzo(g,h,i)perylene
Fluorene
Phenanthrene
Dibenzo(a,h)anthracene
Indeno(1,2,3-e,d)pyrene
Pyrene
Benzene
Toluene
Ethyl benzene
217
4.8
212
2.2
0.12
2.1
6.5
0.14
6.4
17.0
0.01
17
26.0
3.3
23
7.60
1.9
5.7
0.87
0.44
0.43
2.2
0.91
1.3
6.5
1.2
5.4
0.87
4.03
-3.2
6.5
1.3
5.3
1.09
0.05
1.04
13
3.2
10.5
24
5.3
19
1.09
0.002
1.09
1.09
0.002
1.09
12
2.1
9.8
<0.022
0.032
<0.02
<0.022
0.0067
<0.02
<0.022
0.0014
<0.02
—	__	223
0.812	0.045 0.43
17	0.015 8.7
7.5	6.0 6
810	60	430
0.35	0.12 0.27
0.09	0.015 0.053
0.39	0.05 0.20
0.36	0.090 0.23
13	2.2 7.7
17	9.6	15
0.015	0.015 0.015
150	33	104
65	29.5	50
<0.015	<0.015	<0.015
<0.015	<0.015	<0.015
4.8	3.9 4.4
5-18

-------
TABLE 5-12. PENTA PAN EVAPORATOR — MATERIAL BALANCE




Obs
Obs




Pred
high
low
Obs a>



pan
pan
pan
pan


Sludge
vent
vent
vent
vent

Wastewater
out
out
out
out
out
Stream name
in (g/hr)
(g/hr)
(g/hr)
(g/hr)
(g/hr)
(g/hr;
Stream (x 10~3)
142
4.5
138
	
	
186
Penta
994
0.03
994
7.5x103
0.42
3xl03
Phenol
1.4
0.0005
1.4
160
ND
80
Fluoranthene
2.3
0.01
207
420
0.25
210
Naphthalene
121
0.005
121
1.5x103
0.50
750
Benzo(a)anthracene
36
0.0023
36
50
0.07
25
Benzo(a)pyrene
8.5
0.0002
8.3
ND
ND
ND
Benzof1uor anthenes
21
0.0009
21
10
ND
5
Chrysene
43
0.0023
41
50
0.07
25
Acenaphthylene
135
0.0002
131
340
ND
170
Anthracene
41
0.0023
40
190
0.04
95
Benzo(g, h, i)pery1ene
<1.4
0.0005
<1.4
ND
ND
ND
Fluorene
213.0
0.0045
213.0
430
ND
220
Phenanthrene
383
0.0016
383
380
0.25
190
Dibenzo(a,h)anthracene
<1.4
0.00045
<1.4
ND
ND
ND
Indeno(l,2,3-e,d)pyrene
<1.4
0.00045
<1.4
ND
ND
ND
Pyrene
50
0.0063
50
350
0.2
180
Benzene
<1.4
0.0009
<1.4
ND
ND
ND
Toluene
<1.4
0.00004
<1.4
ND
ND
ND
Ethyl benzene
<1.4
0.0009
<1.4
ND
ND
ND
5-19

-------
TABLE 5-13. PERCENT OF ORGANIC SPECIE EMITTED IN VENT

Creosote
Penta
Specie
evaporator
evaporator
Penta
95
100
Phenol
98
100
Fluor Athene
100
97
Naphthalene
88
100
Benzo(a)anthracene
75
100
Benzo(a)pyrene
50
98
Benzofluoranthene
60
100
Chrysene
80
95
Acenaphthylene
—
97
Anthracene
80
98
Benzo(g,h,i)pery1ene
100
_
Fluorene
80
100
Phenanthrene
79
100
Di benzo(a,h)an thr acene
100
—
Indeno(l,2,3-e,d)pyrene
100
— .
Pyrene
80
100
Benzene
—

Toluene
—

Ethyl benzene

—.
5-20

-------
5.2 MODELS FOR THERMAL EVAPORATION
The original predictions for negligible organic emissions to the
atmosphere from thermal (pan) evaporation were based on ideal solution vapor
pressures (Raoult's law), and classical diffusion and mass transport theory.
Previous laboratory work indicated that these predictions might be wrong (1)
by postulating a hypothetical model applying regular solution theory and
activity coefficients. This model could increase the emission rates several
orders of magnitude, enough for measurement. The reported field tests
verified that organic emissions do occur at a significant level.
Although study of the field data reveals a wide variation in the
observed concentrations of organics in the emissions, these concentrations
were well above predicted levels. Because the sampling times varied with
respect to the evaporation cycle and the filling process was not continuous, a
closer inspection of the process produced a new model for predicting emissions.
5.2.1 Model Description
Thermal evaporation is similar to laboratory batch steam distillation:
wastewater is transferred to the evaporator, internal heating is applied by
steam coils, and after a given period of time, more wastewater is put into the
evaporator. As organics are driven out, their concentration in the system
decreases. When the concentration of a specie falls to zero in most of the
water, it falls to zero in the emission. Therefore, the concentration of the
emitted specie is cyclic: the average concentration measured during a given
test depends on when in the evaporation cycle the sample was taken.
Four physical regimes for evaporation have been identified:
•	Static evaporation (ideal or regular solution)
•	Steam distillation
5-21

-------
•	Controlled mass transfer evaporation from an infinite sink
•	Flash evaporation
A qualitative description of the model follows with a brief
mathematical description and sample calculations for each mechanism. Observed
values are then compared to predicted values for each mechanism involving one
compound.
Qualitative Description—
Thermal evaporation of organic components from a wastewater matrix can
be modeled as a series of physical processes. Each mechanism depends on the
phase distribution of the component under study. At the beginning of the
cycle, the component is distributed among sludge, water, and oil. Steam
distillation depletes the component in the (partially miscible) oil phase.
The infinite source mass transfer mechanism then operates until the component
can no longer be stripped significantly from the sludge. Finally, the static
evaporation mechanism operates until the component has been stripped from the
water or a new cycle begins. A diagram of the process is shown in
figure 5-3. An expected gas phase concentration plot is given in figure 5-4.
A summary of the model follows:
•	When water and component A exist as two partially immiscible
liquids, steam distillation of component A occurs
t When the sludge can act as an infinite source of component A, the
mass transfer rate from sludge to liquid to gas determines its
concentration in the gas phase
•	When component A is present solely in solution, static evaporation
determines its approximate concentration in the gas phase
5-22

-------
Figure 5-3. Thermal evaporation system.
5-23

-------
Charge
Figure 5-4. Thermal evaporation cycle.
5-24

-------
•	Flash evapoaration occurs only when the heat source is uncovered
and well above the boiling point of the wastewater
•	The duration of each mode differs for different components
Steam Distillation—
Immediately after charging, component A may exist as a partially
miscible oil. If it does, its concentration in the gas phase is approximated
by the pure steam distillation formula (2):
WA MA PA
AAA	(3)
WH20 MH20 PS20
where	WA = weight of component A in vapor phase
WH 0 » weight of water in vapor phase
= molecular weight of component A
q = molecular weight of water
= partial pressure of pure A at boiling temperature of mixture
Py = partial pressure of water at boiling temperature
Calculations for various components and tests in tables 5-14 and 5-15
show some compounds very near steam distillation concentrations and some very
far away. The lower the solubility and the higher the concentration (in the
incoming wastewater), the closer the component comes to steam distillation
concentration. The test time is also critical as shown by the differences
between the penta pan evaporator tests 3 and 4. Test 3 was conducted just
prior to the start of a new cycle, while test 4 was begun shortly after a new
wastewater charge was placed in the evaporator.
5-25

-------
TABLE 5-14. PENTA PAN EVAPORATION — STEAM DISTILLATION MODEL



Test
3

Test
4

WA

WA

OBS
,WA
OBS

WB
PRED
U
B OBS

PRED
u
B OBS
PRED
Penta
0.038

4.6 x 10"5
1
x 10"3
0.04
1
Phenol
0.25

10"6
4
x 10"6
7 x 10~4
3 x 10~4
Naphthalene
0.18

4 x 10"6
3
x 10"5
8 x 10"3
5 x 10"2
Anthracene
0.013

3 x 10-6
2
x 10~4
10"3
9 x 10~2
Fluorene
1.5 x
10"3
4 x 10"6
3
x 10"3
2 x 10"3
1.2
Phenanthrene
5.2 x
10"3
10"5
2
x 10"3
2 x 10~3
0.4
Pyrene
1.4 x
10"4
4 x 10"6
3
x 10~2
2 x 10"3
1.3
5-26

-------
TABLE 5-15. CREOSOTE PAN EVAPORATION — STEAM DISTILLATION MODEL
^A	OBS	WA	OBS
WB PRED WB OBS	PRED	^B OBS	PRED
Penta	0.041	9 x 10"5	2 x 10"3	3.7 x 10"6	9 x 10"5
Phenol	0.24	2 x 10"5	8 x 10"5	7.9 x 10~5	3.3 x 10"4
Naphthalene	0.16	2.7 x 10~4	1.7 x 10~3	3.7 x 10~3	0.023
Anthracene	0.013	4.3 x 10"^	3 x 10~3	9.2 x 10~5	0.007
Fluorene	1.6 x 10~3	1.5 x 10~4	0.096	7.4 x 10~4	0.46
Phenanthrene	2.3 x 10~3	1.3 x 10~4	0.056	2.6 x 10~4	0.11
Pyrene	1.2 x 10~4	2.1 x 10~5	0.18	1.7 x 10~5	0.16
5-27

-------
Mass Transfer Limited Emissions—
The concentration of component A in the gas phase falls as the
concentration in the solution falls; the emission rate also falls, assuming
the water evaporation rate remains constant. Given sludge with a high
concentration of component A (an infinite source), material dissolves from
this source into solution at an increasing rate as the concentration in
solution falls. At a certain concentration, transfer rate from source to
water is balanced by the rate of transfer from water to air.
Over an interval cf time, the average concentration of component A
emitted (assuming evaporation volume change is negligible) is given by:
V1(CAS-CA>
Vg " CAg	<4>
where	¦ volume of wastewater in evaporator (liters)
CAS = saturation concentration of A (mg/1)
CA = steady state concentration of A (mg/1)
Vg = volume of water evaporated (liter)
CAg = concentration of component A in emission (mg/1)
From the analytical data, only the creosote pan evaporator sludge
contains sufficient material to act as an infinite source.
Pure Static Liquid Evaporation—
Pure static liquid evaporation models are based on gas phase diffusion
calculations assuming that the source concentration is constant and the
driving force for transfer is pure vapor pressure. The classical approach for
determining vapor pressure (and therefore gas phase concentration) is to use
Raoult's law for ideal solution:
PA - p£
-------
where P^ = partial pressure of component A
P° = partial pressure of pure component A at the temperature of
the solution
X. = mole fraction of component A in solution
H
This approach assumes that the solution is ideal, that solute and
solvent do not interact, that the solute and solvent molecules are
approximately the same size, and that the concentration of the solute is well
below saturation. When such is not the case (as is obvious in the pan
evaporation system), a regular solution theory is invoked; an activity
coefficient of the solute-solvent system is incorporated into the formula:
"a ¦ paVa	(6)
The activity coefficient, y, is a measure of the departure from the
ideal (Raoult's law). For y > 1, there are positive deviations, and for
y > 1, negative deviations. Hydrocarbon/water systems almost universally have
positive deviations. Predicted deviations for the system studied here are
orders of magnitude greater than one (3).
Flash Evaporation—
When wastewater is flash-evaporated, the concentration of a given
component in the gas phase equals its concentration in the liquid phase. The
emission rate is equal to the evaporation rate of water times the component
concentration in the water.
5.2.2 Comparison to Predictions
The predicted emission concentrations for each mechanism during the six
tests is given in table 5-16. These values are for naphthalene, a major
component in both the creosote and the penta streams. The observed values are
5-29
-------
TABLE 5-16. COMPARISON OF PAN EVAPORATOR MODELS FOR NAPHTHALENE (g/sm3)
Test	Penta evaporator	Creosote evaporator
number
Mode
Pure steam	130	130	130	120	120	130
distillation
Limited mass	9	14	16	3.2	3.4	3.1
transfer (sludge
to water to gas)
Flash evaporation 3 x 10~4 7 x 10"^ 2 x 10~4 1 x 10"^ 7 x 10" 3 5 x 10~3
Pure static liquid 7.7 x 10"6 1.9 x 10~6 5.6 x 10~6 2.2 x 10~4 1.7 x 10~4 1.1 x 10"4
(ideal solution)
Pure static liquid 1.5	0.4	1.1	44	34	22
(regular solution)
Observed	2 x 10"3 3 x 10"3 6.0	0.2	2.8	2.2
-------
much higher than is predicted by classical evaporation theory, but lower than
the predicted steam distillation values.
5.3 CONCLUSIONS
The results of this study conclusively confirm that almost all organic
species analyzed in the wastewater stream are emitted to the atmosphere upon
pan evaporation. Furthermore, the bulk of the organics is emitted. Finally,
the emission rate of the organics in toto and of specific components is cyclic.
This cyclic nature is the result of the once-a-day charging of the
evaporators from the oil/water separators. The total amount of organics
emitted strongly depends on the effectiveness of the oil/water separator.
Sludge generation is approximately 2.5 metric tons/year/evaporator,
about half of which is returned to the process. The remainder is disposed of,
usually by landfill in 55—gal drums.
5-31
-------
SECTION 6
CHARACTERIZATION OF MULTIMEDIA EMISSIONS FROM
SPRAY EVAPORATION OF WOOD PRESERVING WASTEWATERS
This field test program was conducted at a wood treating plant
utilizing spray pond evaporation to reduce its wastewater volume. The program
was designed to determine the organic emissions from the spray pond and the
resulting sludge layer, as well as from the wastewater input. Each stream was
qualitatively and semi quantitatively analyzed for organic compounds, including
volatile organics, chlorinated dibenzo-p-dioxins, chlorinated dibenzofurans,
chlorinated phenolic compounds, and polynuclear aromatic hydrocarbons.
6.1 PROGRAM DESCRIPTION
This program focused on determining if organic emissions were
discharged to the air during evaporation and if the transport mechanism could
be established. Possible mechanisms were simple evaporation or aerosol
drift. In addition, the cryogenic sampling system and resin trapping methods
were compared.
6.1.1 Test Site
The wood treating facility selected for field sampling employed two
treating cylinders using a closed steaming process. Both cylinders could
treat wood using penta formulations; one cylinder also could use creosote.
Wood products treated at the plant consisted almost entirely of Southern
yellow pine in the form of utility poles and lumber.
6-1
-------
Wastewater and byproducts generated from the treating process were
discharged into discrete oil/water separators. Each separator held
10,000 gal. Primary separation was carried out as a batch process with an
average retention time of 18 hours. The tanks were operated manually, and the
recovered treating formulation was returned to the appropriate bulk storage
tank. Creosote wastewater was discharged directly into the spray pond.
Wastewater from the penta oil/water separator was further treated by a
three-zone gravity separator using a skimming device to recover any remaining
penta residue, after which the wastewater was discharged into the spray pond.
The spray pond consisted of an unlined pond with a pumping station and
seven spray nozzles. The sprays were operated 24 hrs/day unless local wind
conditions caused excessive drifting of the spray.
6.1.2 Field Test Program
The sampling program conducted included each of these tests:
•	Determination of atmospheric characteristics at the spray pond
•	Air emission sampling at the spray pond using:
-- Cryogenic U-tubes
— Tenax traps
~ XAD-2 cartridges
•	Liquid grab samples of spray pond wastewater
•	Solids samples of spray pond sludge and soil samples in areas near
the spray pond
Table 6-1 presents a summary of the field test matrix for the sampling period.
The air emission samples were collected using a sampling train
developed by the University of Arkansas. A complete description of this unit
is contained in appendix B. The train was used to collect cryogenics (water
6-2
-------
TABLE 6-1. SUMMARY OF SAMPLES COLLECTED
Sample
Air samples —
spray pond non-
isokinetic sampling
Liquid samples —
composited grab
sampling
Solid samples ~
composited sludge
sampling
1
4-XAD2, cryogenics
and field volatiles
using Tenax
1-composite
1-composite
2
4-XAD2, cryogenics
and field volatiles
using Tenax
1-composite
1-composite
3
4-XAD2, cryogenics
and field volatiles
using Tenax
1-composite
1-composite
and organics collected in a cold trap), nonvolatile organics in XAD-2 resin
traps, and volatile organics in Tenax traps. Temperature and wind vector
information also was collected.
6.1.3 Process Description
The data for the pond evaporation study is given in table 6-2.
6.2 DISCUSSION OF RESULTS
Emission rates could not be determined due to the detection limits of
the sampling and analytical methodology. While the University of Arkansas
(UA) methodology is currently the best approach to determining organic
emission rates from surface waters, the physical limits of spray pond
evaporation and the sampling system prevent the detection of low and medium
volatile compounds.
The best ambient air monitoring instrumentation available under optimum
laboratory conditions can obtain levels of sensitivity to about 10 ppb (v/v)
6-3
-------
TABLE 6-2. DATA FOR POND EVAPORATION
Waste-	Pond
Pond water	water
sludge input	recycle Test 4 All others
Component	(yg/g) (yg/g)	(yg/g) (total yg) (total yg)
Pentachlorophenol
15,000
1,100
15
41,
5.2, 4.0
ND*

Phenol
50
48
0.1


ND
ND
Fluoranthene
5,800
23
3
1.4,
ND, ND
ND

Naphthalene
1,500
120
4


ND
ND
Benzo(a)anthracene
2,600
f®
0.4


ND
ND
Chrysene
2,000
ND
0.6


ND
ND
Anthracene
2,700
ND
0.7


ND
ND
Fluorene
5,600
58
1.7


ND
ND
Phenanthrene
9,000
67
6.4
1.7,
ND, ND
ND

Pyrene
4,400
15
1.6
1.1,
ND, ND
ND

Octachloro
dibenzodioxin
2.1
	**
	



—
Chloro
dibenzofurans
1.4
—
--


--
—
Oil and grease
—
--
160


	
—
*ND = Not detected
**— = Not analyzed
6-4
-------
or methane equivalents of about 10 pg per analytical injection: this is for
total organics, not individual components. Normal field monitoring
instruments are good to about 1 ppm (v/v) for total organics. The QA
procedure allows field samples to be analyzed at concentrations 10 times lower
than the most sensitive methods or 1,000 times lower than the usual methods.
For a compound such as phenol, this means a detection limit of about 1 to
5 ppb (v/v) in the gas phase of individual components.
The different molecular weights of the compounds under study make it
easier to work with concentration units of weight to sample volume. This
gives the following sensitivities for the three sampling methodologies:
•	Ambient monitoring — 10 ng/1 of methane equivalent for total
organics {no speciation)
•	Field monitoring — 1 yg/1 of methane equivalent for total organics
(no speciation)
•	UA methodology (FID) ~ 0.5 ng/1 of individual components
Use of gas chromatography/mass spectrometry (GC/MS) with the UA
sampling methodology decreases the sensitivity to about 50 ng/1. The sample
volumes for the two standard methods are fixed by the instrumentation, while
the sample volume of the UA system is limited by the moisture content of the
gas stream: water vapor frozen out in the collection device eventually stops
sample flow.
In this study we drew 5 to 10 times the recommended amount of sample,
increasing our sensitivity by approximately one order of magnitude.
Raoult's law of partial pressure predicts concentrations of penta in
the range of 3 x 10 pg/1. Pure penta exhibits concentrations of 3 ng/1
(300 ng/sm3). Although the normal sampling location for the UA system is at
6-5
-------
the water surface, this test required taking the samples on the berm, about 3
ft above water level. To offset the subsequent dilution, the samplers were
run as long as possible (until the traps froze up). The results were
detection limits only 2 to 3 times less than the maximum possible (see table
6-3), not nearly enough to make up for dilution. Dilution would be at least
10- to 20-fold over a distance of 2 ft.
In conclusion, the methodology was insufficient to determine emissions
off the ponds.
6-6
-------
TABLE 6-3. DETECTION LIMITS « POND EVAPORATION
Detection limit
Test
Flow
(ml /min)
Elapsed time
(min)
Temperature
(°C)
Volume
(sm3)
ppt (w/v)
GC/MS GC/FID
(ng/sm3) (ng/sm3)
Test type
1
66
23
8.5
1.6 x
0-3
640
6.4
Cryogenic blank
2
66
135
6.4
9.4 x
°i
110
1.1
Tenax + XAD blank
3
66
180
8
13.0 x
°i
80
0.8
Ten ax
4
66
90
12
6.1 x
°i
160
1.6
Cryogenic
5
66
42
12
2.9 x
0"3
350
3.5
Cryogenic
6
66
69
8
4.8 x
°i
210
2.1
Cryogenic
7
66
94
3
6.6 x
0-3
150
1.5
XAD
8
66
120
7
8.3 x
0-3
120
1.2
XAD
9
66
120
14
8.1 x
0-3
120
1.2
XAD
10
66
122
16
8.2 x
0-3
120
1.2
Tenax
11
66
120
8
8.3 x
0-3
120
1.2
Tenax
Maximum penta concentration = yg/sm3 (30 ppb v/v)
Analytical sensitivity
Field GC/TVOC = 1 ppm
GC/MS concentrate = 1 yg/sample (1 ng injected)
GC/FID concentrate = 10 ng/sample (10 pg injected)
-------
SECTION 7
CHARACTERIZATION OF EMISSIONS FROM THE DISPOSAL OF
WOOD PRESERVING WASTES IN AN INDUSTRIAL BOILER
The Resource Conservation and Recovery Act (RCRA) is expected to cause
some generators of hazardous wastes to dispose of their wastes within plant
boundaries. One disposal option is the thermal destruction of the waste in a
steam boiler. This field test program was conducted at a wood preserving
facility using a pile-burning watertube boiler cofiring a mixture of wood
waste and penta/creosote wastewater. The program was designed to determine
the destruction and removal efficiencies of the organic compounds in the
wastewater. Input materials (the wood waste and sludge) and output materials
(mechanical hopper ash, baghouse ash, and bottom ash) were analyzed, and
pertinent data for a material balance evaluation were collected. All samples
were qualitatively and semiquantitatively analyzed for organic compounds,
including chlorinated phenols, chlorinated dibenzo-p-dioxins, chlorinated
dibenzofurans, and polynuclear aromatic hydrocarbons.
7.1 PROGRAM DESCRIPTION AND RESULTS
This program focused on the gaseous emissions discharged from the stack
and the ash streams resulting from combustion and pollution control. Making
material balance estimates was difficult since ash and fuel flowrates were not
metered by the operator. However, estimates were made of each stream, and the
destruction and removal efficiencies were evaluated.
7-1
-------
7.1.1	Test Site
The wood treating facility selected for field sampling employs six
retorts using a steaming process to treat a variety of domestic and imported
wood products. The process can treat wood with penta, creosote, or waterborne
preservative formulations.
Wastewater and byproducts generated from the individual treating
processes are handled by discrete oil/water separators. The recovered
preservative fractions are returned to bulk storage tanks for reuse in the
process. Separated sludges and wastewater are routed to a storage tank; when
quantity is sufficient to ensure economic handling, the wastes go to the steam
boiler for disposal. Figure 7-1 presents a schematic of the plant
wastewater/preservative recovery system. An estimated 5,000 to 8,000 gal/day
of wastewater is generated during normal treating operations.
The boiler manufactured by WeiIons Company was designed to produce
40,000 lb/hr of steam for space heat, the treating cycle, and other plant
operations. The boiler unit, consisting of both a cell and a furnace, could
be fired using both or fired separately, depending on plant process demand.
The boiler fuel supply system consisted of transfer and metering
conveyors, wet and dry fuel silos, two metering bins for cell and furnace, and
a constantly running screw conveyor to charge the fuel to the cell and furnace
for burning. Both screw conveyors were modified to allow hog fuel to be mixed
with sludge and/or wastewater from the treating plant. The cell also was
equipped with a ram charging device for loading irregular-shaped and oversized
wood scrap into the boiler.
7.1.2	Field Test Program
The sampling program conducted included each of these tests:
7-2
-------
-10,000 gallon e«.
settling tanks
gallons
Figure 7-1. Schematic of plant wastewater/preservative recovery system.
7-3
-------
•	Determination of preliminary gas stream characteristics
•	Isokinetic source sampling of boiler flue gas
•	Total hydrocarbon determination of boiler flue gas
•	Specific low-molecular-weight hydrocarbon determination of flue gas
using gas chromatography (GC)
•	Composite sampling of:
—	Boiler bottom ash
—	Multicone hopper ash
—	Wood waste fuel
—	Sludge wastewater fuel
•	Grab sampling of:
—	Baghouse ash
—	Bulk penta in aromatic treating oil
—	Bulk creosote
The sample collection matrix is shown in table 7-1. The air samples were
collected using an EPA Method 5 sampling train with XAD-2 resins for
nonvolatile organic emissions. Volatile emissions were determined using field
GC methods.
7.1.3 Data Presentation — Organics and Inorganics
The concentrations of organic components in the various samples are
shown in table 7-2. The corresponding concentrations of trace elements are
given in table 7-3. Concentration units are in ug/g (ppm w/w) for the solids
and liquid (sludge), and in units of yg/sm^ (ppt w/v at 23°C and 1 atm).
Components not detected are listed as less than (<) values if the number is a
direct analytical measurement or as not detected (ND) if the value is
calculated (i.e., averaged or requiring independent test data). NA means the
7-4
-------
TABLE 7-1. SAMPLE COLLECTION MATRIX

Air samples

Solid samples

Sample
number
Outlet stock
Wood waste
and sludge
Boiler
bottom ash
Mech. hopper
ash
Baghouse
ash
1
1-XAD, GC
1-composite
1-grab
1-composite
1-grab
2
1-XAD, GC
1-composite
1-grab
1-composite
1-grab
3
1-XAD, GC
1-composite
1-grab
1-composite
1-grab
4
1-XAD, GC
1-composite
1-grab
1-composite
1-grab
7-5
-------
TABLE 7-2. CONCENTRATIONS OF ORGANIC COMPONENTS IN INCINERATOR SAMPLES
feed sludge	Button ash	Mechanical hopper	Baghouse dust	Stack gas
(119/9)	U9/9)	(»g/g)	(119/9)	(wg/sit3)
Saaple test	2 3 4 Ave 2 3 4 Ave 2 3 4 Ave 2 3 4 Ave 2 3 4 Ave
Pentachlorophenol
470
260
80
270
0.5
0.5
0.5
0.5
0.05
0.5
7.4
2.7
1.0
1.0
1.0
1.0
NO
ND
ND
NO
Phenol
1200
1000
1400
1200
0.1
0.8
0.6
0.8
0.1
0.1
0.1
0.1
0.5
0.2
0.3
0.3
4.1
2.7
2.3
3.0
Fluoranthene
2200
340
170
1355
92.0
15.0
1.4
36.1
0.5
0.6
1.7
0.9
0.7
0.2
6.2
2.4
NO
NO
NO
NO
Naphthalene
1300
1000
560
953
10.0
18.0
9.6
12.5
10.0
6.5
2.2
6.2
10.0
3.9
5.1
6.3
570.2
150.5
161.3
294. n
Benzo(a)anthrocene
160
120
27
102
7.6
0.6
0.1
2.8
<0.1
0.1
0.1
0.1
0.5
0.2
0.5
<0.4
NO
ND
NO
NO
Boizo(a)pyrene
<20
30
<10
20
1.4
0.1
0.1
0.5
<0.1
0.1
0.1
0.1
0.5
0.2
0.5
<0.4
NO
ND
NO
NO
Benzo fluoranthene
S2
64
14
43
9.3
0.9
0.1
3.4
<0.1
0.1
0.1
0.1
0.5
0.2
0.5
<0.4
NO
NO
NO

Cryrene
180
120
28
109
1.2
0.7
0.1
0.7
<0.1
0.1
0.3
0.2
0.5
0.2
0.5
<0.4
ND
NO
NO
NO
Acenaphthylene
130
68
24
74
4.4
3.0
0.1
2.5
<0.1
0.1
0.1
0.1
0.5
0.2
0.5
<0.4
NO
NO
NO
NO
Anthracene
760
250
92
367
4.5
1.0
0.2
1.9
<0.1
0.1
0.2
0.1
0.5
0.2
0.5
0.4
NO
ND
NO
NO
Fluorene
1200
420
180
600
0.6
0.8
0.1
0.5
<0.1
0.1
0.1
0.1
0.5
0.2
0.5
0.4
NO
NO
NO
NO
Phenanthrene
1800
590
330
813
24.0
31.0
3.0
19.3
0.6
0.5
0.4
0.5
6.9
3.0
7.3
5.7
NO
NO
NO
NO
Pyrene
1200
310
140
550
29.0
7.9
0.4
12.4
<0.1
0.1
0.4
0.2
0.5
0.2
0.5
0.4
ND
ND
NO
NO
Benzenes
1
<1
<1
1
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NO
NO
NO
NO
Toluene
12
3.7
9
8.2
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NA
NO
ND
NO
NO
Ethylbenzene
17
5.7
10
10.9
NA
NA
M
NA
NA
NA
NA
NA
NA
NA
NA
NA
ND
NO
NO
NO
-------
TABLE 7-3. INORGANIC TRACE ELEMENT COMPOSITIONS IN INCINERATOR SAMPLES
S«?le
Test
As
Be
Cd
Zn
Cr
Cu
Pb
N1
*9
Sb
Hg
Se
T1
Feed sludge
2
6.8
O.OOl „
<0.02
10.0
2.7
36
<1
<0.2
<0.06
<0.05
0.01
<0.05
<0.001
3
3.5
<9 * 10-*
<0.02
7.0
2.6
48
<1
<0.2
<0.06
0.2S
0.01
0.05
<0.001

4
8.1
<9 x 10-4
<0.02
3.0
2.0
19
<1
<0.2
<0.06
0.16
0.02
0.10
<0.001

Ave
6.1
NO
•0
6.6
2.5
34
NO
NO
NO
0.13
0.013
0.05
NO
Bottoa «sl)
2
0.35
1.0
<0.02
2.0
1.0
29
<1
0.6
<0.06
<5.0
1.0
<5.0
<0.11
3
40.5
0.7
<0.02
5.0
0.6
57
<1
0.5
<0.06
<5.0
2.0
10.0
<0.1

4
73.0
1.0
<0.02
8.0
1.1
29
<1
0.4
<0.06
<5.0
0.9
10.0
<0.1

Ave
38.0
0.9
NO
5.0
0.9
38
NO
0.5
NO
NO
1.3
10.0
NO
Nechanlcil hopper
2
0.02
2.0
0.1 .
90.0
1.9
85
100
0.3
<0.06
<5.0
3.0
<5.0
<0.1
*sh
3
6.5
0.9
<0.02
40.0
2.0
120
10
0.3
<0.06
<5.0
4.0
<5.0
<0.1
4
o.as
0.9
<0.02
30.0
1.8
70
10
0.2
<0.06
<5.0
2.0
<5.0
<0.1

Ave
0.5
1.3
0.03
53.0
1.9
92
40
0.3
NO
NO
3.0
NO
NO
B*gttouse dust
2
0.53
0.4
0.3
750.0
2.9
230
1500
0.4
0.1
2S.0
5.0
10.0
<0.1
3
11.4
0.4
0.4
750.0
4.4
305
1500
0.4
0.1
38.0
12.0
10.0
<0.1

4
49.0
0.2
0.3
500.0
3.4
22$
1200
<0.2
0.1
28.0
11.0
10.0
<0.1

Ave
20.0
0.3
0.3
700.0
3.S
253
1400
0.3
0.1
30.0
9.0
10.0
ND
Units — »9/9 (PP» */»)
-------
component was not analyzed for.
The air emission rates for naphthalene and phenol are summarized in
table 7-4. Other components are not listed because they were not detected
(detection limits are <10~^ g/sec). Stack sampling data are summarized in
appendix C.
7.2 MATERIAL BALANCE AROUND INCINERATOR
To determine the destruction efficiency of the hazardous waste
components, a material balance around the boiler facility was generated. The
particular components of interest could be used because an unknown fraction
was being destroyed. Therefore, an Indestructable material was used as a
tracer. The following steps were taken:
t Identification of Input and output streams
•	Determination of stream flowrates
•	Calculation of organic component mass flowrates
§ Calculation of destruction efficiency
The streams were Identified as the:
•	Feed sludge
•	Bottom ash
•	Mechanical hopper ash
•	Baghouse dust
•	Stack emissions
The working equation for the material balance 1s given as:
Rf CfJ - T Ri Cij	(7)
7-8
-------
TABLE 7-4. RATES OF DISCHARGE AND EFFICIENCY OF DESTRUCTION FOR NAPHTHALENE AND PHENOL
Feed Bottm ash Nech. hop. Baghouse Gas	Total out Efficiency
(g/sec) (g/sec) (g/sec)	(g/sec) (g/sec)	(g/sec) (percent)
Test 2
Naphthalene
Phenol
Solid rate
0.25
0.23
189
1 x 10-5
<1 x 10~7
1.01
7.6 x 10"6
<8 x 10"*
0.76
2 x 10"7
<8 x 10~9
0.017
3.9 x 10"3
2.9 x ir5
(6.85)a
3.9 x 10~3
2.9 x 10"5
98.4
99.99
Test 3
Naphthalene
Phenol
Solid rate
0.19
0.19
189
1.3 x 10-5
6 x 10-'
0.74
8.5 x 10"*
1.3 x 10~7
1.3
8.2 x 10-f
4.2 x 10~9
0.021
1 x 10-3 c
<1.9 x 10"5
(6.85)a
1 x 10-3
<2 x 10~5
99.5
>99.99
Test 4
Naphthalene
Phenol
Solid rate
0.11
0.27
189
2.9 x 10-$
1.8 x 10-7
0.30
1.8 x 10~®
<8 x 10-10
0.35
1.1 x 10-'
6.3 x lO-9
0.008
1.1 x 10"7
1.6 x 10"5
(6.99)*
1.1 x 10-3
1.6 x 10"5
99.0
99.99
Assumptions: " Feed rate, all cases - 189 g/sec sludge; sludge is source of wtals; all Zn, Cr, Cu coses out in
solids.
*Sa3/sec (23°C and 1 at*)
-------
where
Rf » feed rate of sludge
Cfj » concentration of jthcomponent 1n the feed
t h
Ri - rate of discharge of i stream
Cjj « concentration of jth component in 1th stream
Measured rates were available for the feed and the stack gas
emissions. The feed rate was 2.7 gal/min with a density of 1.1 g/ml or 189
g/sec. The gas volume ranged from 6.85 to 6.99 sm^/sec (23°C and 1 atm).
The grain loading was not detectable (<10-^ g/sm^ or <10~^ g/sec), so
solids in the gas stream were negligible.
Rates for the three ash streams were not directly measurable; these
were obtained using the trace element analyses and a corresponding set of
three simultaneous equations generated from (7). All the given element was
assumed to be introduced in the feed with none emitted out the stack. The
chosen elements, zinc, chromium, and copper, were relatively high in the feed
with relatively low volatility. An unmeasured portion possibly Introduced
with the wood chips is partially offset by the unmeasured air emissions.
The matrix of these equations is set up 1n table 7-5 with a solution
for the three unknown rates. The results for the three tests are consistent
and in good agreement. Using these calculated rates, the flowrates of
naphthalene and phenol (the only observed organic emissions) were derived and
presented in table 7-4. The destruction efficiency also 1s presented, as
calculated from the equation:
E - Rf CH;	°1"1 X 100	(8)
7-10
-------
TABLE 7-5. CALCULATION OF RATES OF GENERATION OF SOLIDS
Bottom ash Hopper ash Baghouse dust Feed
Ji.d , 
-------
TABLE 7-6. SUWARY OF ABBREVIATIONS FOR CHLORODIBENZOFURAN
AND CHLORODIBENZODIOXINS
Abbreviations
Name
Possible isomers
MCDF
Monoch 1 o rod i benzof uran
4
DCDF
Dichlorodibenzofuran
16
TrCDF
Trichlorodibenzofuran
28
TCDF
Tetrachlorodibenzofuran
53
PCDF
Pentachlorodibenzofuran
28
HxCDF
Hexachlorodibenzofuran
16
HpCDF
Heptachlorodibenzofuran
4
OCDF
Octachlorodibenzofuran
1
MCOO
Monoch1o rod i benzod i ox1n
2
DC DO
Dichlorodibenzodioxin
10
TrCOO
Trichlorod1benzodioxi n
14
TCDD
T etrachlor od1benzod1ox1n
22
PC DO
Pentachlorodibenzodioxin
14
HXCDO
Hexachlorodibenzod ioxi n
10
HPCDO
Heptach1orodibenzodioxin
2
OCOO
Octachlorodi benzod ioxi n
1
7-12
-------
TABLE 7-7. CHLORODIBENZOFURAN AND CHLORODIBENZODIOXIN ANALYTICAL RESULTS
FOR TREATMENT OIL (4.5 PERCENT PENTA IN OIL)
Minimum
detectable
Total no. of	Total detected*** concentration
COO/CDF* apparent Isomers** (ng/g)	(ng/g)
MCDF
4
2
0.4
DC OF
2
2
0.8
TrCDF
4
10
1.2
TCDF
5
18
0.1
PCDF
5
137
1
HxCDF
5
1813
1
HpCDF
2
114
1
OCDF
1
711
3
MCDD
2
1.5
0.4
DCDD
2
2
0.8
TrCDD
2
3.5
1.2
TCDD
-
1.1
0.5
PCDD
6
33
0.3
HxCDD
4
574
1
HpCDO
2
256
1
OCDD
1
3996
3
*See table 7-6 for sumnary of nomenclature
**See text
***Not corrected for recovery, these concentrations represent minimum values
7-13
-------
TABLE 7-8. CHLORODIBENZOFURAN AND CHLORIDIBENZOOIOXIN ANALYTICAL RESULTS
FOR DAY 2 COMPOSITE SLUDGE LIQUID
Minimum
detectable
Total no. of Total detected*** concentration
CDD/CDF* apparent Isomers**	(ng/g)	(ng/g)
MCDF
4
0.6
0.2
DCDF
0
0
0.3
TrCDF
0
0
0.7
TCDF
0
0
0.1
PCDF
1
0.3
0.2
HxCDF
2
0.8
0.5
MCDO
1
0.2
0.2
DC DO
0
0
0.3
TrCDD
0
0
0.7
TCDD
0
0
0.9
PCDD
3
0.6
0.3
HxCDD
4
2.5
0.5
*See table 7-6 for sumnary of nomenclature
**See text
***Not corrected for recovery, these concentrations represent minimum values
7-14
-------
TABLE 7-9. CHLORODIBENZOFURAN AND CHLORODIBENZODIOXIN ANALYTICAL RESULTS
FOR DAY 4 COMPOSITE SLUDGE LIQUID
CDD/CDF*
Total no. of
apparent Isomers**
Minimum
detectable
Total detected*** concentration
(ng/g) (ng/g)
MCDF
3
0.7
0.2
DCDF
0
0
0.4
TrCDF
0
0
0.9
TCDF
0
0
0.05
PCDF
1
0.5
0.2
HxCDF
3
8
2
HpCDF
2
7
1
OCDF
1
2
1
MCDD
1
0.6
0.2
DC DO
1
0.4
0.4
TrCDD
0
0
0.9
TCDO
0
0
0.9
PCDD
0
0
1
HxCDO
3
10
1
HpCDO
2
70
1
OCDO
1
225
1
*See table 7-6 for sumnary of nomenclature
**See text
~~~Results corrected for recovery
7-15
-------
TABLE 7-10. CHLORODIBENZOFURAN AND CHLORODIBENZODIOXIN ANALYTICAL RESULTS
FOR DAY 2 COMPOSITE ASH
CDD/CDF*
Total no. of
apparent Isomers**
Total detected***
(ng/g)
Minimum
detectable
concentration
(ng/g)
MCDF
3
75
0.1
DCDF
8
25
0.3
TrCDF
8
15
0.6
TCDF
7
7
0.5
PCDF
5
8
1
HxCDF
5
5
1
HpCDF
2
6
1
OCDF
1
2
1
MCDD
1
1
0.1
DCDD
4
5
0.3
TrCDD
5
2
0.6
TCDD
4
3.4
0.2
PCDD
5
32
1
HxCDD
5
81
1
HpCDD
2
117
1
OCOO
1
198
1
*See table 7-6 for sunmary of nomenclature
**See text
~~~Results corrected for recovery
7-16
-------
TABLE 7-11. CHLORODIBENZOFURAN AND CHLORODIBENZODIOXIN ANALYTICAL RESULTS
FOR DAY 3 COMPOSITE ASH
Minimum
detectable
Total no. of Total detected*** concentration
CDD/CDF* apparent Isomers** (ng/g)	(ng/g)
MCDF
3
90
0.1
DCDF
8
7.5
0.3
TrCDF
6
20
0.6
TCDF
8
1.2
0.05
PCDF
5
0.7
0.1
HxCDF
2
1
0.3
HpCDF
2
1.6
0.6
OCDF
1
1.2
1
MCDD
1
2
0.1
DC DO
5
1
0.3
TrCDD
5
5
0.6
TCDO
-
0.8
0.2
PCDD
5
2.6
0.1
HxCDD
1
8.7
0.3
HpCDO
2
42
1
OCDD
1
96
1
*See table 7-6 for summary of nomenclature
**See text
***Results corrected for recovery
7-17
-------
TABLE 7-12. CHLORODIBENZOFURAN AND CHLORODIBENZOOIOXIN ANALYTICAL RESULTS
FOR DAY 4 COMPOSITE ASH
CDD/CDF*
Total no. of
apparent Isomers**
Total detected***
(ng/g)
Minimum
detectable
concentration
(ng/g)
MCOF
3
5
0.1
DCDF
10
8
0.3
TrCOF
11
17
0.6
TCDF
8
3
0.1
PCDF
5
3
0.3
HxCDF
4
1.8
0.4
HpCDF
0
0
2
OCDF
0
0
1
MCDO
2
0.7
0.1
DC DO
4
0.5
0.3
TrCDD
4
6
0.6
TCDO
6
3.3
0.2
PCDO
4
6
0.3
HxCDO
3
10
0.4
HpCDD
2
4
2
OCDD
1
1
0.8
~See table 7-6 for sunmary of nomenclature
**See text
***Results corrected for recovery
7-18
-------
chromatographic peak does not necessarily correspond to a single isomer of a
given class; such peaks may represent more than one isomer. Hence, the
terminology "apparent isomers."
No CDF's or CDD's were detected in the air emissions. The detection
limits were <10 yg/sm^ (10 ppt w/v). CDF's were detected in the hopper and
baghouse dust, but not in the bottom ash; the converse was true for the CDD.
Although there was an apparent generation of TCDD's, data analysis placed this
in some doubt. Using OCDD as a tracer, the apparent dilution from the oil to
the sludge was about x200 or 5 x 10"^ ng/g total TCDD's in the sludge (well
below the detection limit of the analytical methodology). The mass flowrate
of TCDD's into the boiler (from previous material balance results) is about
1 ng/sec. The bottom ash generation rate 1s about 0.6 g/sec with a TCDD
concentration of about 2 ng/g or a TCDD output rate of 1.2 ng/sec. The
sampling, analytical, and data reduction error bounds are large enough to
preclude stating that TCDD 1s generated. It can be said that the apparent
destruction of TCDD is minimal.
What is of concern 1s that, while 2,3,7,8 TCDD does not appear to be
present 1n the sludge and oil, 1t does appear to be present 1n the ash. This
suggests formation by thermal 1somer1zat1ons, requiring a much deeper study of
these samples.
7-19
-------
SECTION 8
EVALUATION OF FUGITIVE EMISSION SOURCES
For the purposes of this program, fugitive emissions are defined as
emissions from:
•	Treating cylinder spillage and drippage
•	Vapors released from the treating cylinder during unloading and
charging operations
0 Vacuum vent exhaust during the treating cycle
•	Transfer of treating solution formulations from valves, fittings,
or open processing vessels
These emission sources are of concern because of the opportunities for
employees to contact directly the toxic compounds.
When the treating cylinder (retort) is opened, any treating solution
left in the vessel may spill onto the ground. If the retort is surrounded by
a spill beam, the treating solutions are recovered and recycled to the
system. However, if the treating solution is allowed to fall onto the ground,
housecleaning activities could accumulate hazardous waste material.
Low-molecular-weight organic compounds vaporize in the retort during
the high-temperature preservative application. During charge changes, these
organics are released as fugitive emissions through the open door of the
retort, forming a dense white plume. The wood removed from the retort also
emits material as a white plume that may exceed 40 percent opacity after
8-1
-------
20 min. Qualitative and semi-quantitative organic analyses for specific
pollutants in these emissions were expected to show the presence of benzene,
toluene, phenol, and similar volatile and low-molecular-weight compounds.
Emissions from the vacuum exhaust and other retort vents also are of
concern. Source tests at one mill measured 2.2 g/m^ (0.95 grain/scf) of
aerosol in 12.5 m3/min (440 scfm) of gas from a vacuum pump vent. Steam
3	3
conditioning released 44 g/m of aerosol in a 13 m /min stream.
Finally, while fugitive emissions from preservative handling,
transport, leaks, and valves can occur, no qualitative or quantitative data is
available to characterize such emissions.
This section presents the component speciation results from fugitive
emissions tests conducted at a wood preserving facility. Emissions from
preservative handling, transport, leaks, and valves were not tested.
8.1	TREATING CYLINDER SPILLAGE AND DRIPPAGE
The treating facility tested employed two treating cylinders, and used
penta and creosote preservatives. Samples of accumulated spillage and
drippage were collected from the area directly beneath the penta and creosote
treating cylinder access doors. Two samples were obtained at each location
before and after the field test period. Table 8-1 presents the qualitative
organic analysis for these samples.
8.2	FUGITIVE EMISSION DURING UNLOADING AND CHARGING OPERATIONS
Air samples were collected during unloading and charging operations
directly above the penta and creosote treating cylinder access doors.
Sampling was performed using the modified EPA Method 5 train and XAD-2
cartridges described in appendix A.
8-2
-------
TABLE 8-1. CHARACTERIZATION OF PENTA AND CREOSOTE TREATING
CYLINDER SPILLAGE AND DRIPPAGE

Penta treating cylinder
Creosote treating cylinder
Sample location:
spillage and
drippage
spillage and drippage
Date collected:
9/23/80
9/25/80
9/23/80
9/25/80
Compound

Concentrations in vg/g

Pentachlorophenol
1,500
2,100
390
1,800
Phenol
<10
<10
<20
<10
Fluoranthene
29
180
420
200
Naphthalene
50
200
1,300
1,400
Benzo(a)anthracene
60
80
870
1,000
Benzo(a)pyrene
50
5.6
240
200
Benzofluoranthenes
54
26
700
500
Chrysene
50
85
710
850
Acenaphthylene
16
11
72
180
Anthracene
47
55
1,200
1,500
Benzo(ghi)perylene
<10
<5
<50
40
Fluorene
110
140
1,100
2,600
Phenanthrene
150
320
2,300
2,200
Dibenzo(a,h)anthracene
<10
<5
<50
20
In deno(1,2,3-cd)pyrene
<10
<5
<50
52
Pyrene
24
140
370
1,700
Benzene
<0.5
0.1
0.3
15
Toluene
<0.5
0.5
<0.2
<1
Ethylbenzene
<0.5
0.5
<0.2
<1
8-3
-------
Fugitive emissions released through the open cylinder door during
charge changes appeared as a dense white plume which persisted throughout the
sampling. Table 8-2 presents the qualitative organic analysis for these
samples in concentration per volume of air sampled. It was not feasible to
quantify a mass emission rate due to large fluctuations in ambient air
dilution caused by changing wind speed and direction.
8.3 VACUUM VENT EXHAUST
Certain wood treating processes require the application of pressure and
vacuum at various steps of the treating cycle. The pressure release and
vacuum exhaust are sources of fugitive emissions, both aerosols and vapors.
Emissions from a vacuum vent common to the penta and creosote treating
cylinders were characterized. Grab samples were analyzed onsite for total
hydrocarbons (THC) using the procedures described in appendix A. Table 8-3
presents a summary of the results of the THC analysis during both penta and
creosote treating cycles.
Grab samples of emissions from the vacuum vent also were analyzed for
specific low-molecular-weight hydrocarbons: benzene, toluene, and
ethylbenzene. These components were measured onsite using the methods and
procedures described in appendix A. Table 8-4 presents a summary of the
analyses for specific low-molecular-weight emissions during penta and creosote
treating cycles.
These data tables show that significant concentrations of organic
compounds are emitted to the atmosphere. During the course of a single
treating cycle at this facility, the chronological sequence in table 8-5 was
observed.
8-4
-------
TABLE 8-2. QUALITATIVE ORGANIC ANALYSIS RESULTS FOR FUGITIVE EMISSIONS




Creosote




treating
Sample location:
Penta treating cylinder
cylinder
Run number:
1
2
3
1
Compound

Concentration*

Pentachlorophenol
<0.02
8.12
2.63
0.63
Phenol
<0.02
1.62
<0.02
0.11
Fluoranthene
0.026
<0.16
0.019
0.94
Naphthalene
0.057
5.85
1.86
2.81
Benzo(a)anthracene
<0.02
<0.16
<0.02
0.01
Benzo(a)pyrene
<0.02
<0.16
<0.02
<0.01
Benzof1uor anthenes
<0.02
<0.16
<0.02
<0.01
Chrysene
<0.02
<0.16
<0.02
0.01
Acenaphthylene
0.135
0.29
0.11
0.086
Anthracene
0.026
0.05
0.03
0.46
Benzo(ghi)perylene
<0.02
<0.81
<0.02
<0.01
Fluorene
<0.02
0.32
0.46
0.08
Phenanthrene
0.31
0.49
0.28
2.81
Dibenzo(a,h)anthracene
<0.02
<0.81
<0.12
<0.01
In deno(1,2,3-cd)pyrene
<0.02
<0.16
<0.02
<0.67
~Concentration units are mg/sm^
8-5
-------
TABLE 8-3. SUMMARY OF TOTAL HYDROCARBON DETERMINATIONS
PERFORMED AT A COMMON VACUUM VENT



Emission point



Penta pan
evaporation
device
Creosote pan
evaporation
device
Penta
treating
cylinder
fugitive
emissions
Creosote
treating
cylinder
fugitive
emissions
Vacuum vent
penta cycle
Vacuum vent
creosote cycle
Date

ppm* total hydrocarbons as methane (time)**

9/23/80
evaporation
444 (1326)
evaporation
emissions
emissions
penta cycle
creosote cycle
9/24/80

892 (1730)
36 (1747)
3,660 (1326)
984 (1351)
1,787 (1425)
646 (1519)
——
——
9/25/80
165 (1250)
185 (1305)
1,456 (1450)
1,442 (1514)
—
221 (0828)
365 (0914)
42,066 (1034)
52,294 (1052)
22,117 (1332)
41,475 (1349)
*ppm = parts per million
**(time) » time sample was collected, 24-hr clock
-------
TABLE 8-4. SUMMARY OF SPECIFIC L0W-M0LECULAR-WEI6HT HYDROCARBON
DETERMINATIONS AT A COMMON VACUUM VENT
Total
hydrocarbon
Time	Benzene Toluene Ethylbenzene as methane
Date (24-hr clock) (ppm) (ppm) (ppm)	(ppm)
Emission point: penta thermal evaporation device
9/23/80 1650
1.6 ND ND
4.6
9/25/80 1250
ND ND ND
—
1305
ND ND 1.8
6.9
Emission point:
creosote thermal evaporation device

9/24/80 1730
ND ND ND

1747
ND ND 1.5
5.8
9/25/80 1450
ND ND 13
53
1514
ND ND 13
53
Emission point:
penta treating cylinder fugitive emissions

9/24/80 1326
ND ND ND

1351
ND ND 27
110
1425
ND ND 11
43
Emission point:
creosote treating cylinder fugitive emissions

9/24/80 1519
ND ND ND

2/25/80 828
ND ND 3.3
13
914
ND ND 2.1
8.6
Emission point:
vacuum vent during penta cycle

9/25/80 1034
ND 1,567 1,607
11,571
1052
104 1,482 1,722
12,010
Emission point:
vacuum vent during creosote cycle

9/25/80 1332
1,356 42 1,618
10406
1349
1,304 64 1,598
9,960
ND * not detectable
8-7
-------
TABLE 8-5. TREATING CYCLE SEQUENCE
Pressure
or Tem.
Treating Cycle	vacuum °F Time started Time completed Lapse time (hours)
CONDITIONING
1.	Steaming
2.	Vacuum	23 in. 8:15 am	10:15 am	2:00
3.	Preservative In.	5:45 am	6:15 am	0:50
4.	Heating in Oil	210 6:15 am	10:15 am	4:00
5.	Preservative Back	10:15 am	10:45 am	0:50 5:00
TREATING
6.	Initial Vacuum
7.	Initial Air	70 psi	10:45 am	11:00 am	0:25
8.	Preservative In.	11:00 am	11:20 am	0:33
9.	Pressure Commenced 90 psi 200 11:20 am	1:30 pm	2:17
10.	Preservative Back	210	1:30 pm	2:00 pm	0:50
11.	Final Vacuum	23 in.	2:00 pm	4:00 pm	2:00
12.	Recovering Drippings	4:00 pm	4:15 pm	0:25
13.	Secondary Steam
14.	Secondary Vacuum
15.	Changing Time	0:50
TOTAL TIME	11:00
-------
From this table, it can be seen that a vacuum was drawn for a total of
4 hrs, and the retort was open for a total of 50 min. Based on these emission
times and the data contained in table 8-3, the vacuum vent represents the
3
greatest emission source. A vacuum vent exhaust of 12.5 sm /min with an
organic concentration of 50,000 mg/1 (50 mg/nr*) results in an emission rate
of 625 mg/min. For a plant with two retorts, the annual emission rate would
be less than one metric ton/year. A medium refinery may emit as much as
1,000 metric ton/year. Therefore, though these concentrations of organics may
cause localized problems, the total emission burden is not significant.
8-9
-------
APPENDIX A
CHARACTERIZATION OF MULTIMEDIA EMISSIONS FROM THERMAL (PAN)
EVAPORATION OF WOOD PRESERVING WASTEWATERS
CONTENTS
A-l Program Description and Results
A-2 Raw Data: Source Emission Sampling for High-Molecular-Weight
Emissions
A-3 Raw Data: Total Hydrocarbon and Specific Low-Molecular-Weight
Determinations
A-l
-------
SECTION A-l
PROGRAM DESCRIPTION AND RESULTS
This field test program was conducted at a wood preserving plant using
pan evaporation to reduce its generated wastewater volume. The program was
designed to determine the organic emissions from two thermal (pan)
evaporators, two retorts, and a vacuum vent, as well as from organic input
liquids and remaining sludges. Each stream was qualitatively and
semiquantitatively analyzed for organic compounds, including chlorinated
phenols, chlorinated dibenzo-p-dioxins, chlorinated dibenzofurans, and
polynuclear aromatic hydrocarbons (PAH's).
This program focused on the primary multimedia effluents generated by
the plant which were expected to have the greatest environmental impacts in
terms of gaseous and solid discharges. No wastewater discharge from plant
boundaries is permitted by law. The sampling points of interest were the
ducted and fugitive air emissions, and solid wastes from housecleaning and
wastewater treatment. Because of the batch nature of the preserving process
and the variability of the input materials (wood), the cost of a program
extensive enough to generate a meaningful plantwide material balance was
determined to be prohibitive. Besides, the primary focus was on multimedia
environmental emissions. Material balance estimates were conducted around
each evaporator since they represented the only totally quantifiable
A-3
-------
processes, and the evaporators were expected to generate a majority of the
gaseous and solid emissons.
A.l TEST SITE
The wood treating facility selected for field testing employs two
treating cylinders using the Boulton conditioning process. One cylinder can
treat wood with pentachlorophenol (penta) formulations, while the other
cylinder can treat wood with either penta or creosote. Table A-l presents a
summary of the total production during the field test period.
Wastewater and byproducts generated from the individual treating
processes are handled by discrete subsurface oil/water separators on a batch
basis. The recovered oil fraction is returned to bulk preservative storage
tanks for reuse in the process. Separated sludges and wastewater are routed
to the appropriate thermal (pan) evaporator — one penta and one creosote —
for volume reduction. Figure A-l presents a schematic of the plant
wastewater/preservative recovery system.
Product Treated
5a Percent penta
(light oil)
(ft3)
Creosote
Utility poles
Posts
4,012
1,509
Lumber
4,180
6,318
Pilings
1,306
Total
9,701
7,624
A-4
-------
Figure A-l. Schematic of wood preserving plant wastewater/preservative
recovery system.
A-5
-------
A.2 FIELD TEST PROGRAM
The sampling program conducted included the following tests:
•	Source emission sampling at the penta and creosote thermal (pan)
evaporator outlets
•	Source emission sampling at the penta and creosote treating
cylinder during unloading and charging operations
•	Source emission sampling at the common vacuum vent
•	Total hydrocarbon determinations at each air emission point
•	Specific low-molecular-weight hydrocarbon determinations at each
emission point
•	Grab samples of:
—	Penta thermal (pan) evaporator contents
—	Creosote thermal (pan) evaporator contents
—	Bulk penta in treating oil
—	Bulk creosote
—	Penta treating cylinder spillage
-- Creosote treating cylinder spillage
—	Penta oil/water separator (both fractions)
—	Creosote oil/water separator (both fractions)
The sample collection matrix is shown In table A-2. The following subsections
describe the equipment and techniques employed during sampling.
A.2.1 Source Emission Sampling of Pan Evaporators
Sampling of high-molecular-weight organic emissions from the pan
evaporator outlet was conducted using the EPA Method 5 sampling train
nonisokinetically as shown in figure A-2. The train consisted of a heated
A-6
-------
TABLE A-2. SUMARY OF SAMPLES COLLECTED
Saaple location ntmber
1
2
3
4
5
6
7
Collection aethod Location
Penta
retort
Creosote
retort
Vacuus
vent
Penta
oil/water
separator
Creosote
oil/Mater
separator
Penta
evaporator
Creosote
evaporator
Day X
(Setup)
Day 2
XA0-2
Field gas chromatography
Liquid grab saaple
Solid grrft saaple
X
X
X*
(drips)
X
X
X*
(drips)
X
X (2)
X (2)
X
X
x (2)
X
X
X
X (2)
X
Day 3
XAD-2
Field gas chroaatograpfiy
Liquid grab saaple
Solid gr* saaple
X
X
X*
(drips)
X
X
X*
(drips)
X
X (2)
X (2)
X
X
x (2)
X
X
X
X (2)
X
Day 4
XAD-2
Field gas chroaatography
Liquid grd> saaple
Solid gr* saaple
X
X
X*
(drips)
X
X
X*
(drips)
X
X (2)
X (2)
X
X
X (2)
X
X
X
X (2)
X
0*y S
(Cleanup)
«tlill be conpos 1 ted to yield on* staple per retort
-------
Heated Teflon sampling line
(r
XA0-2 trap
QQQ
Dry gas meter control module
Empty
Gas meter thermocouple?*"'"^
-« i—«
Ice/water
batn
Impinger
thermocouple
SiOg trap
100ml D.I. |
Vacuum line
Vacuum gage
I
Coarse adjustment valve
Figure A-2. Schematic of modified EPA Method 5 sampling train.
-------
1/2-inch O.D. Teflon sample line connected to an empty Greenberg-Smith
impinger (without an impaction plate), followed by the XAD-2 resin cartridge.
The resin was followed by a second Greenberg-Smith impinger containing 100 ml
of deionized water. The third impinger, an empty Greenberg-Smith without an
impaction plate, was followed by a silica gel desiccant (Si02) trap to
protect the vacuum pump and sampling control module from moisture.
Four complete source tests were conducted at the penta thermal (pan)
evaporator and at the creosote thermal (pan) evaporator. The evaporators and
sampling locations are shown in figures A-3 and A-4. For each source test,
the sampling equipment was placed on the roof of the thermal (pan) evaporator,
the Teflon sampling line was allowed to preheat to approximately 250°F, and
the impinger train was prepared. Sampling was started by turning on the
vacuum pump and opening the coarse adjusting valve to its midpoint. This
valve position was maintained during the entire sampling period.
The volume of condensate determined the possiblesampling times . As
the first impinger filled with water, the sampling rate became
uncontrollable. The sampling run was terminated by shutting off the vacuum
pump, disconnecting and sealing the inlet and outlet of the Teflon sample
line, and moving the train to the field laboratory. Table A-2 presents a
summary of the pertinent source sampling parameters at each test location.
The raw field data is presented at the end of this appendix.
Samples were transferred from the sample trains to specially cleaned
and labeled storage containers. The probe nozzle, probe, and connecting lines
were rinsed with methylene chloride, and the recovered samples transferred to
the appropriate storage containers. Immediately following sample recovery in
the field, all samples were iced and maintained under those conditions for
their transport to the analytical laboratory.
A-9
-------
Figure A-3. Photograph of penta thermal (pan) evaporator and sample location.
A-ll
-------
Figure A-4. Photograph of creosote thermal (pan) evaportor.
-------
TABLE A-3. SUW4ARY OF SOURCE EMISSION SAMPLING PARAMETERS FOR
TEST CONDUCTED AT THE PENTA AND CREOSOTE THERMAL (PAN)
EVAPORATION DEVICES
Barowtric	Actual	Molecular*	Molecular	Saapled	Total
pressure	sMple	Meter	Condensate	Stack	might	weight gas	stapling
Location/ (inches	voluae	temperature	voluae	teaperature	dry	net	voluae	Percent tlae
rwi nuaber Date Hg)	(acfa)	(°F)	(al)	(°F)	(tb/lb-aole)	(lb/lb-aole)	(scfa)	HjO (ain)
Penta
evap 1
9-24-80
29.20
18.863
59.0
679.1
209.0
29.84
22.43
19.083
62.6
50.0

9-24-80
29.20
0.69S
63.5
1,301.6
215.0
29.84
18.13
0.6971
98.9
29.0

9-24-80
29.40
19.500
48.5
972.5
209.0
29.84
20.036
6.499
82.8
19.5

9-24-80
29.48
8.67
54.8
598.0
206.0
29.84
20.82
8.802
76.2
15.0
Creosote
9-24-80
29.40
16.064
59.3
622.7
191.0
29.84
22.38
17,156
63.1
30.0
9-24-80
29.2S
27.291
59.0
1,130.4
193.0
29.84
22.1
29.02
64.7
56.0
9-25-80
29.40
22.005
49.7
762.3
190.5
29.84
22.72
23.87
60.1
45.0
9-25-80
29.50
19.413
55.5
945.6
195.2
29.84
27.78
20.89
68.1
43.5
*Assuaed W of air.
-------
a.2.2 Source Emission Sampling of Penta and Creosote Treating Cylinders
Sampling of high-molecular-weight emissions during the unloading and
charging of the penta and creosote treating cylinders was conducted using the
same procedures and methods described in section A.2.1. The sampling
locations are shown in figures A-6 and A-7. Sampling was initiated a few
minutes prior to opening the cylinder door and terminated a few minutes after
the door was closed. Sampling times varied from 11 to 21 min, depending on
the size of the charge being unloaded or loaded and the ease with which the
operation proceeded. Table A-4 presents a summary of the pertinent source
sampling parameters for each test.
A.2.3 Total Hydrocarbon Determinations
Total hydrocarbon sampling was conducted at the outlet of the penta and
creosote themal (pan) evaporators, the penta and creosote treating cylinders
during unloading and loading, and at the outlet of the vacuum vent discharge
to the barometric condenser. Sampling was conducted using the system shown in
figure A-8. The gas sample was extracted from the stack via a 7p sintered,
stainless steel Model No. SS-4 FE-7 filter, manufactured by Nupro Valve
Company, Willoughby, Ohio. The filter removed fine particulates which could,
if allowed to pass into the THC analyzer, occlude the FID sample inlet
capillary. A 0.006m 0.0. stainless steel probe connected the filter unit to
the heated sampling line via a three-way stainless steel solenoid valve. This
valve introduced sample gas or calibration gas depending on the desired mode
of operation. A 100-ft, heat-traced, 3/8-inch O.D. Teflon sample line
manufactured by Unitherm Company was used to transport the sample to the
vacuum pump. The sample line temperature was maintained at 394°K by
internal temperature controllers already installed. A Teflon-coated diaphragm
vacuum pump manufactured by Thomas Industries, Sheboygan, Wisconsin, was used
A—16
-------
Figure A-6. Photograph of penta treating cylinder being charged with
poles and the fugitive emission vent.
-------
Figure A-7. Photograph of creosote treating cylinder building and
fugitive emissions vent.
A-19
-------
TABLE A-4. SWWARY OF SOURCE EMISSION SAMPLING PARAMETERS FOR TESTS
Barantric	Actual	Molecular*	Molecular	Stapled	Total
pressure	saaple	Meter	Condensate	Stack	weight	weight	gas	saaplfng
Location/ (inches	voluae	temperature	roluae	teaperature	dry	net	roluae	Percent tiae
rim mmber Oate Hg)	(acfa)	<°F)	(¦!)	(°F)	(lb/lb-aole)	(Ib/lb-anle)	(scfa)	HjO (aln)
Pent* retort
1	9-23-00	29.45	16.494	73.0	55.5	S2.0	29.84	28.19	16.17	13.9	11.0
2	9-24-80	29.24	21.8S1	61.5	29.7	90.0	29.84	29.12	21.73	6.04	14.0
3	9-25-80	29.40	22.395	52.0 S.I	69.0	29.84	29.72	22.81	1.0	1S.0
Creosote
retort 1	9-26-80	29.40	24.448	43.0 —	70.0	29.84	29.84	25.17	0.0	21.0
-------
7um sintered stainless steel filter
-0.006cc stainless steel orobe
• — — — To stack
'Three-way stainless steel solenoid valve
Heat traced Teflon sample line (3C.48m)
Heat traced Teflon connecting line
Teflon diaphragm vacuum pump
Unburned
hydrocarbon
^nal^zer
Strip
chart
recorder

Calibration
gases
2ml injection
loop and
backflush valve
Gas
chromatoqraph
(FID)
Strip
chart
recorder
(H li—I
«sl
8
a

Figure A-8. Schematic of unburned hydrocarbon and gas chromatograph
sampling system.
A-22
-------
to pull the sample through the heated line. From the vacuum pump exit, the
sample was split and routed to the analyzers via short lengths of heated
Teflon line.
Prior to operation and calibration, the completed sampling system was
operated at normal line sampling conditions and purged for several hours with
zero nitrogen to remove any traces of residual hydrocarbon contamination in
the lines. During this "bake-out" procedure, stainless steel tube unions,
filters, and probes were heated using a propane torch. Before and after each
test, a leak test was performed on the sampling system followed by calibration
of the THC analyzer using zero nitrogen gas and a mixture of 801 ppm methane
in nitrogen. During calibration, the three-way valve was positioned to block
the sample probe and filter, allowing the calibration gas to pass into the
heat-traced sample line. Introducing the calibration gases at this location,
ensured the sample gases and calibration gases were treated in the same
manner, mulUfylng possible undesirable effects due to absorption in the
sampling line and system.
A Model 400 total hydrocarbon (THC) analyzer manufactured by Beckman
Instruments, Fullerton, California, was used to continuously monitor total
hydrocarbon emissions from the vacuum vent discharge. This analyzer uses the
flame Ionization detection (FID) method. The analyzer output was recorded
using a Model 585 strip chart recorder manufactured by Linear Instruments
Corporation, Irvine, California.
The FID was operated using zero grade 1.0 hydrogen fuel and zero air
supplied by Airco Industrial Gases, Santa Clara, California. Hydrogen fuel
and zero air pressure were set at 207 KPa (30 ps1) and 103 KPa (15 psl),
respectively, using Internal differential pressure regulators in the analyzer.
A-23
-------
After approximately 1 hr of sampling at the vacuum vent, the heated
sampling line was contaminated heavily with hydrocarbons. Attempts to
recalibrate and rezero the THC analyzer were impossible. At this point, the
heated bulb method was substituted for the continuous method.
A grab sample from each appropriate source was collected by evacuating
and purging a 250-ml pyrex sampling bulb heated to 121°C (250°F).
Aliquotes of the collected sample then were withdrawn from the heated bulb
using a 5-ml gas-tight syringe inserted through a septum port in the bulb.
The syringe contents were injected via a 2-cm^ injection loop and backflush
valve into a Varian Model 3700 gas chromatograph (GC). GC operating
conditions for THC analysis are presented in table A-4.
Table A-5 presents a summary of the results of THC determinations at
the various emission points based on the total area chromatograph and
backflush. The results are reported as ppm methane (CH^).
The accuracy of the data presented using the heated bulb method of
sampling varies substantially. The greatest error associated with this method
is sample integrity. It was apparent that samples collected at the penta and
creosote thermal (pan) evaporators were mostly water vapor. When these
samples were transferred via syringe to the GC for analysis, condensation
within the syringe most likely co-condensed hydrocarbons, thus causing lower
values than would be expected. The error is estimated to be +50 percent
maximum.
THC values for samples collected from the treating cylinders are also
very uncertain due to the nature of the sampling site. The fugitive emissions
were prone to large fluctuations in ambient air dilution caused by changing
wind speed and direction. The possible error associated with these sites,
A-24
-------
TABLE A-4. GAS CHROMATOSRAPH OPERATING CONDITIONS FOR
THE DETERMINATION OF TOTAL HYDROCARBONS
Column:
Injector temperature:
Temperature program:
Special note:
6-ft x 1/8-inch O.D. stainless steel tubing packed
with 1 percent SP 1000 on carbopack (80/100 mesh)
1200C
Isothermal at 120°C
Injected 2-cm3 sample for approximately 5 min or
until ethyl benzene component was eluted, then
backflushed until baseline returned to zero
A-25
-------
TABLE A-5. SUMMARY OF TOTAL HYDROCARBON DETERMINATION PERFORMED AT
VARIOUS EMISSION POINTS
Emission point



Penta treating
Creosote treating



Penta
Creosote
cylinder
cylinder

Vacuum vent

thermal (pan)
thermal (pan)
fugitive
fugitive
Vacuum vent
creosote
Date
evaporation
evaporator
emissions
emissions
penta cycle
cycle
ppa* total hydrocarbons as methane (time)*
9-23-80
9-24-80
9-25-80
444 (1326)
165 (1250)
185 (1305)
892 (1230)
36 (1747)
1456 (1450)
1442 (1514)
3660 (1326)
984 (1351)
1787 (1425)
646 (1519)
221 (0828)
365 (0914)
42,066 (1034)
52,294 (1052)
22,117 (1332)
41,475 (1349)
*ppm m parts per ail lion
*(time) - Time sample was collected, 24-hr clock
-------
based on total gas volumes, 1s estimated to be +100 to 50 percent. The error
based on water vapor volume will be much lower.
THC values for samples collected from the vacuum vent have less
uncertainty about them since those emissions were relatively low in moisture
content. It 1s estimated that the error associated with these values is
+20 percent.
A.2.4 Specific Low-Molecular-Weiqht Hydrocarbon Determinations
Periodically, benzene, toluene, and ethylbenzene concentrations were
determined for each emission point. The Varlan Model 3700 gas chromatograph
separated the hydrocarbon sample Into Its components. GC operating conditions
for the analysis were the same as presented in table A-4.
Calibration standards for the compounds of interest were prepared
onsite using 501 Teflon bags and the methods outlined in "Evaluation of
Emission Test Methods for Halogenated Hydrocarbons," Vol. I, EPA-600/4-79-025,
March 1979. The calibration mixture then was used to calibrate the GC and to
give retention indices for the appropriate components. Table A-7 presents a
summary of the resultant field test analysis. The data are reported by ppm
(specific specie) and as ppm methane.
A.2.5 Liquid Grab Sampling
Grab samples of the following were collected during the 3-day sampling
period:
•	Penta thermal (pan) evaporator contents
•	Creosote thermal (pan) evaporator contents
•	Bulk penta 1n treating oil
•	Bulk creosote
•	Penta treating cylinder spillage
A-27
-------
TABLE A-7. SUMMARY OF SPECIFIC LOW-MOLECULAR-WEIGHT HYDROCARBON
DETERMINATIONS AT VARIOUS EMISSION POINTS
Date
Total hydro-
Time Benzene Toluene Ethylbenzene carbon (ppm*
(24-hr clock) (ppm)* (ppm)* (ppm)* methane)
Emission point: penta thermal (pan) evaporator
9-23-80
1650 1.6 ND+ NO
4.6
9-25-80
1250 NO ND NO
1305 NO NO 1.8
6.9
Emission point: creosote thermal (pan) evaporator
9-24-80
1730 NO NO NO
1747 ND NO 1.5
5.8
9-25
1450 ND ND 13
1514 ND ND 13
53
53
Emission point: penta treating cylinder fugitive emissions
9-24-80
1326 ND ND NO
1351 ND ND 27
1425 NO ND 11
110
43
Emission point: creosote treating cylinder fugitive emissions
9-24-80
1519 ND NO NO
	
2-25-80
0828 ND ND 3.3
0914 ND ND 2.1
13
8.6
Emission point: vacuum vent during penta cycle
9-25-80
1034 ND 1567 1607
1052 104 1482 1722
11,571
12,010
Emission point: vacuum vent during creosote cycle
9-25-80
1332 1356 42 1618
1349 1304 64 1598
10,106
9,960
*PPM > parts per Million
NO - not detectable
A-28
-------
•	Creosote treating cylinder spillage
•	Penta oil/water separator (both fractions)
•	Creosote oil/water separator (both fractions)
Liquid samples of the penta and creosote evaporator contents were collected in
the morning and afternoon of each sampling dey. Samples were collected by
lowering a precleaned sample container into the evaporator tank and retrieving
the liquid near the surface.
Samples of liquid fractions contained in the penta and creosote primary
oil/water separators were obtained on a dally basis. Samples were obtained by
immerslnf an Inverted sample container into the appropriate layer then tipping
it to collect the sample. Some contamination was observed during retrieval of
the lower fraction; however, this was minimal with respect to the initial
sample volume. This will bias the creosote wastewater values to the high
side, and the penta recycle oil to the low side.
The remaining samples of bulk penta and creosote, and of penta and
creosote treating cylinder spillage were collected on a one-time basis. After
collection, all samples were immediately 1ced and maintained on ice for
transport to the analytical laboratory.
A.3 ANALYTICAL METHODS AND RESULTS
Samples from the thermal (pan) evaporation system were received on
October 21, 1980. The samples were assigned consecutive laboratory
identification numbers and stored at 4°C until analyzed.
A.3.1 Analytical Methods
Analyses were conducted for voltalle organics, semi volatile organlcs,
and dloxlns. Volatile organic analyses were based on variations to EPA
Method 624. Semlvolatlle organic (phenols and polynuclear aromatics) analyses
A-29
-------
were based on sample preparation variations to EPA Method 625 in conjunction
with fused silica capillary column gas chromatography/mass spectrometery
(X/MS).
Analysis of Volatile Organlcs—
The analytes of interest were benzene, toluene, and ethylbenzene. The
sludge and wastewater samples were analyzed for these components.
A l.Og aliquot of the mixed sludge or wastewater was weighed Into a
15-ml crimp top vial. Pentane (9 ml) and l-bromo-2-chloropropane (10pg) were
added as Internal standards. A 1-ul aliquot of this diluted sample was
injected in a 0.2-percent Carbowax 1500 on a Carbopack C packed GC column in a
Finnegan 1020 GC/MS instrument. Analysis and quantitation were conducted per
EPA Method 624 using the internal standard method.
Quality control for the volatlles analysis entailed the analysis of
method blanks and method standards spiked at 10vg/g of sludge. In addition,
the control requirements of Method 624, including instrument tuning to meet
specifications, were met.
Analysis of Semi volatile Organlcs—
Semlvolatlle organics analyzed are listed 1n table A-8. These analyses
were conducted by variations to EPA Method 625. The variations were 1n the
sample preparation and in the use of fused silica capillary column GC/MS to
determine these compounds.
Sample Preparation-
Sludge samples were prepared as follows:
1. Place 10.Og of the sludge 1n a clean 250-ml brown bottle. Add
10.Og of anhydrous sodium sulfate and 100 ml of pesticide grade
dlchloromethane. Shake occasionally and allow to sit overnight at
room temperature.
A-30
-------
TABLE A-8. SEMIVOLATILE ORGANICS ANALYZED IN WOOD PRESERVING SAMPLES
Number
Name
1
Phenol
2
2-N1trophenol
3
2,4 Dich1orophenol
4
2,4,6 Trichlorophenol
5
4-Nitrophenol
6
4,6-D1n1tro-o-cresol
7
Pentachlorophenol
8
Acenaphthalene
9
Fluoranthene
10
Naphthalene
11
Benz(a)anthracene
12
Chrysene
13
Acenaphthylene
14
Phenanthrene
15
Fluorene
16
Pyrene
17
Benzofluoranthenes
18
Benzo(a)pyrene
A-31
-------
2.	Take 1.0 ml of each extract for GC/FID screening. Store the
remaining extract at 4°C.
3.	As required by the GC/FID screening, filter the extract into a
Kuderna-Danish concentrator and concentrate to 1.0 ml.
The GC/FID screening stage was necessitated by the wide variability of
sample concentrations. Figure A-9 summarizes the semivolatile scheme for
sludge samples.
The XAD-2 cartridge was carefully opened, any silicone stopcock grease
removed with a CH2C12 wetted towel, and the contents transferred to a
preextracted Soxhlet thimble. The XAD-2 material in the Soxhlet was spiked
with surrogate mix and extracted overnight with CH2C12.
To assure analysis of all organics collected during the XAD-2 sampling,
two other samples were taken for each sampling train: a dichloromethane probe
rinse and an impinger catch. For analysis, the dichloromethane rinse was
added to the XAD-2 Soxhlet extractor. The impinger water was acidified to pH
1 with 6N H^SO^ and extracted overnight in a continuous liquid-liquid
extractor. The water extract and XAD-2 extract were then combined, dried with
anhydrous sodium sulfate, and concentrated to 1.0 ml.
Quality control for XAD-2 samples consisted of the analysis of
surrogate spikes, field blanks, and spiked method blanks.
Extract Analysis-
Each of the extracts obtained as described in the previous section was
analyzed for the compounds listed In table A-9 using fused silica capillary
column GC/MS. The instrument operating conditions also are listed.
A-32
-------
Figure A-9. Proposed analysis scheme for phenols/PAH's
1n wood preserving sludges.
A-33
-------
TABLE A-9. FUSED SILICA CAPILLARY COLUMN PARAMETERS
Column:
30m x 0.25 m SE-54 WCOT (JW Scientific)
Splltless Injection Parameters:
Injection mode:	Splltless
Sweep Initiation:	30 sec
Sweep flow:	Greater than or equal to 12 ml/min
Column flow (He)
measured at
atmospheric:	1.0 ml/m1n
Interface:
Temperature:	300°C
Column directly coupled to source (no transfer lines)
Temperature Program:
Initial:	30°C for 2 m1n
Program:	Ramp to 300°C § lO°C/m1n
Hold:	300OC, 15 m1n
Mass Spectral Parameters:
Ionization mode/
energy:	Electron 1mpact/70 eV
Total scan time: 1.0 sec
Mass range:	35 to 475 AMU
A-34
-------
The quality control requirements listed in EPA Method 625 were
followed, including analytical calibration, mass spectrometer tuning to meet
decafluorptriphenylphosphine (DFTPP) criteria, and the use of multiple
internal quantitation. The internal standards used were dg-naphthalene,
d^Q-anthracene, and d^-chrysene.
A.3.2 Analytical Results and Discussion
Volatile Organics—
Voltaile organics (benzene, toluene, ethylbenzene) were determined in
water and sludge samples using a pentane extraction method followed by GC/MS.
Figure A-10 is a chromatogram of a method blank spiked with the compounds of
interest at lyg/g. The solvent contaminants did not interface with the
determination of the compounds of interest.
Figure A-ll is a chromatogram from the analysis of a retort drip
sample. This sample is typical, having very low or no detectable volatile
aromatics. No contamination was detected in the analysis of method blanks.
It was, however, necessary to increase the column bake cycle time after the
injection of several samples: higher-molecular-weight creosote components
accumulated on the column and performance deteriorated without the extra bake
cycle.
Semi volatile Organics—
Phenols and polynuclear aromatics were determined by solvent extraction
and fused silica capillary column GC/MS. An extract prescreening procedure
using GC with FID determined the appropriate extract concentration factors
prior to GC/MS analysis. The prescreening was especially Important with
certain sample types (oil/water separator samples) which were extremely
variable 1n content.
A-35
-------
RIC
01/0V01 IftttlN
SMFUl MI-lMlS-t IWMUL 1NJ .OF-1.0
I, 4M LMELl N 6. 4.1 QUAMi
DATA:
CALIi
MPtise «i
FC43 II
SCANS 1 TO 4W
MNGCG
A •- 1.0 BASEi U 26, 3
1323000.
PMk Idtntlflcitlons:
C ¦ Solvent Contaminant
IS ¦ Internal Standard
B ¦ Btnztn*
WC.
IS

50
1:3?
JSL
-r—i-
tee
5:13
ii | i i
130
it',2
C
JZ2—
M-
i i i i i"
280
6:30
"T~r-
230
8i07
9: <5
' I '
330
11:22
' ¦» i |
m SCAN
li:O0 TIME
Figure A-10. Total 1on current chromatogram of a volatlles standard.
A-36
-------
Figure A-ll. Total 1on current chromatogram for a retort drip
vol atlies analysis.
A-37
-------
Two cases of contamination were detected during the course of the
study. The XAD-2 blanks contained 10 to 200u9 of naphthalene. This is an
XAD-2 contaminant as received from the manufacturing process and indicates an
insufficient washing process prior to field sampling. Only trace levels of
other analytes (1 to 5yg) were detected on the XAD-2. During the GC/MS
injection of a series of thick creosote extracts, a serious
cross-contamination was detected. As much as 0.1 percent sample-to-sample
contamination was detected when using 1-yl capillary syringes. No method for
routine cleaning of these syringes could be found. However, no such problem
was detected with standard 10-vl syringes.
In the dirtiest creosote samples, the overall retention time of many
compounds varied from that measured in the standards. However, the retention
time relative to a nearby eluting internal standard was a reliable
identification criterion. Special care was needed with the benzo(a)pyrene
isomers. Figure A—12 shows the M/E 126 and 252 extracted ion current profiles
for one of the creosote samples. Although standards were not available, the
other isomers were tentatively identified as listed. The two
benzofluoranthenes could not be reliably separated in the presence of so many
other compounds. It was decided to report these two as a single value for all
samples.
Figure A-13 shows the chromatograms from various spots in the creosote
preserving process. A few of the major peaks are identified 1n each
chroma to gram. The creosote at this plant appears to be different from other
creosotes in that the phenol content 1s very low (400 ppm).
Table A-10 presents a log of all samples collected, followed by
tables A-11 through A-23 which present the analytical data.
A- 38
-------
38.8-1
12S .
IN. 4-)
252 .
xe.e-i
RIC * !t*S CHPCHhTGGMMS	CwThi hNIIV I960
01'«Si lJiMnW	CAt.li C4I4681A 03
SMlEi H8e-lS-«15-54 K-( OIL. OF«10,tUw'CONi 0*1612
RANGEl C 1.2200 LUfeELi N 0, 4.0 OOMH: h 0 1.0 BASEs U 20. 3
SCANS 1700 TO 18W
405S.
126.038
* 0.500
12704.
292.075
t 0.500
47040.
r
1790	1000
29i40	30100
SCAN
T1HE
NOTE: Nak A li wirMolwd batao (bH) flMrintfcMM.
fMk 0 1» btntoWpyrww. Nik» I. C, mt C
art twiUtlvily tiriwitlflad »* b«izo(J)fluorwtlmw,
bwio(«)pyr«M, iitd pcryltM.
Figure A-12. M/E 126, 252, and RIC for the benzo(a)pyrene region of a
creosote extract FSCC analysis.
A- 39
-------
ate	ft** nus ti
ll«« tltftM	ODLtl CMIMM M
SfVVlIl B-IMI94I MR HU3MB Si. It. 12		
mm* t i«zm u*u n •. 4.i wm a	•. i.t mii u ». 3
KM m TO I
i«.*i
(b) Creosote oil/water separator — bottom layer
Figure A-13. Chromatograms of creosote solutions through the process.
A-40
-------
tie
IWMi	OMM.UL-aSC 0MM2
* I'O* U«Li M 4.t OM* A «. l.» Mi U M. t
MT«m MUSS7 II	SOM IM TO 2SM
cut! CMflMM II
»»	TJ*
(c) Creosote working solution
IK
mm* iiiim
- mm t> •. i.» Mb « ». t
>*»	TM
(d) Creosote retort drips
Figure A-13. Concluded
A-41
-------
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
TABLE A-10. SAMPLE NUMBER AND IDENTIFICATION
Sample Description
Pond, top layer w/o1l, 1 of 2
Pond, top layer w/oil, 2 of 2
Pond, sludge
Pond, middle layer
Creosote pan evap. liquid, 1700, 9/23/80
Creosote oil/water separator, top layer, 9/23/80
Creosote oil/water separator, bottom layer, 9/28/80
Creosote retort drips, 1158, 9/23/80
Penta fugitive emission, front half
Penta fugitive emission, back half
Penta retort drips, 1138
Penta oil/water separator, top layer
Creosote pan evap. liquid and impinger H2O, front half
Creosote pan evap. liquid and impinger 1 H20, front half,
rinse
Creosote pan evap. liquid and impingers 2 and 3 H?0, test 1,
back half, rinse
Creosote oil/water separator, top layer
Creosote oil/water separator, bottom layer
Creosote pan evap. liquid, pretest
Creosote pan evap. liquid, test 2, front half
Creosote pan evap. liquid, test 2
Creosote pan evap. liquid, test 2 probe rinse
Penta pan evap. liquid, test 2 impinger H20
Penta pan evap. liquid, test 1, front half rinse
Penta pan evap. liquid, pretest 1
Penta pan evap. liquid, test 2
Penta pan evap. liquid, test 1, back half
Penta fugitive emission, test 2, front half
Penta pan evap. liquid, test 2, front half
Penta oil/water separator, top layer
Penta pan evap. liquid, test 1, back half rinse
Penta pan evap. liquid, test 1, front half, impinger H20
Penta oil/water separator, bottom layer
Penta pan evap. liquid, test 3, impinger H2O
Penta pan evap. liquid, test 4, Impinger H2O
Penta pan evap., bottoms from value 6 in. off ground
Penta retort fugitive emission, test 3, impinger H2O
Penta pan evap. liquid, test 3
Penta 40 percent solid in No. 2 fuel oil
Penta retort fugitive emission, test 3, front half, MeCl2
rinse
Penta pan evap. liquid, test 3, fron half, MeCl2 rinse
A-42
-------
45
46
47
48
49
50
51
52
53
54
55
56
57
58
59
60
61
62
63
64
65
66
67
68
69
70
71
72
73
74
75
76
TABLE A-10. Concluded
Sample Description
Penta pan evap. liquid, test 4, front half, MeCl2 rinse
Penta oil/water separator, bottom layer
Penta retort drips
Creosote pan evap. liquid, test 4, impinger H2O
Creosote pan evap. liquid, test 3, impinger H2O
Creosote pan evap. liquid, test 3, front half
Creosote pan evap. liquid, test 4
Creosote retort fugitive emission, test 1, front half, impinger
H20
Creosote oil/water separator, bottom layer
Creosote retort fugitive emmisson test 1, front half, MeCL2
rinse
Penta oil/water separator, top layer and oil
Creosote pan evap. liquid, test 3
Creosote pan evap. bottoms
Creosote retort drips
Creosote pan evap. liquid, test 4, front half, MeCl2 rinse
Creosote oil/water separator, top layer
Creosote working solution, tank 5 (new)
Penta working solution, as used
Penta pan evap. liquid, test 4
MeCl? blank, baker res. anal.
Viking DIH2O, all tests after 9/24
Well No. 4
XAD, penta pan evap. liquid, test 1
XAO blank No. 2
XAD, penta pan evap. liquid, test 4
XAD, creosote pan evap. liquid, test 4
XAD, creosote pan evap. liquid, test 3
XAD, creosote pan evap. liquid, test 1
XAD, penta fugitive emission, test 1
XAD, creosote pan evap. liquid, test 2
XAD, penta fugitive emission, test 2
XAD, creosote pan evap. liquid, test 3
XAD, penta fugitive emission, test 3
A-43
-------
TABLE A-ll. WOOD PRESERVING TEST RESULTS
TEST	XRiqSQIE PAN EVAP	IESI 1
TEST DATE 9/?V80
Liquid )W Sep Top
OW Sep Bot
XAD
COMPOUND
Acurex I.D. #
80-10-015-
-6
-7
¦70
Pentachlorophenol
2.3
0.5
360
0.45
Phenol
<0.5
15
<100
0.08
Fluoranthene
7.8
7.0
3500
0.67
Naphthalene
33
30
18000
2.0
Benzo(a)anthracene
15
11
9800
0.009
Benzo(a)pyrene
7.5
3.9
2400
<0.01
Benzof1uoranthenes
13
10
2200
<0.01
Chrysene
12
7.6
5300
0.007
Acenaphthylene
76
36
2200
0.061
Anthracene
12
8.2
300
0.33
Benzo(gh1)pery1ene
3.2
1.4
<100
<0.01
Fluorene
50
25
11000
0.059
Phenanthrene
35
20
2500
2.00
D1benzo(a,h)anthracene
0.7
120
<0.01
Indeno(l,2,3-cd)pyrene
3.0
<100
<0.01
Pyrene
6.5
5.8
680
0.48
Benzene
<0.1
0.1
26
NA
Toluene
0.1
0.1
140
NA
Ethylbenzene
0.5
<0.1
44
NA
All concentrations In units of micrograms per gram except for XAD collections
which are total milligrams collected.
A-44
-------
TEST CRFOSOTF
TEST 1
TEST DATE
9/23/80
Retort-Drips
COMPOUND
Acurex I.D. #
80-10-015-
-8
Pentachlorophenol
390
Phenol
<20
Fluoranthene
420
Naphthalene
1300
NOTE:
Fugitives Lashes from
Benzo(a)anthracene
870
¥/2b/BU
this XAD

aaaea to
mple by
Benzo(a)pyrene
240
mUtAkfi.
Benzofluoranthenes
700
Chrysene
710
Acenaphthylene
72
Anthracene
1200
Benzo(gh1)perylene
<50
Fluorene
1100
Phenanthrene
2300
01benzo(a,h)anthracene
<50
Indeno(1,2»3-cd)pyrene
Pyrene
<50
370
Benzene
0.3
Toluene
<0.2
Ethylbenzene
<0.2
P*r tnM tXeept ,0r co1,Kt,."s
A-45
-------
TABLE A-13. WOOD PRESERVING TEST RESULTS
TEST CREOSOTE PAN EVAP
TEST 2
TEST DATE 9/24/80
I Pre Test
jLiquid 8:30
-18
.W. Sep ToplO.W. SepBotl XRU
COMPOUND
Acurex I.D. #
80-10-015-
¦1L
-J.L
-72
Pentachlorophenol
3.4
12
3600
<0.1
Phenol
Fluoranthene
11
1500
20
20
33000
23
38
Naphthalene
13
42
33000
310
Benzo(a)anthracene
14
10
23000
0.6
Benzo(a)pyrene
24
610
<0.05
Benzof1 uoranthenes
5.7
530
0.08
Chrysene
8.9
10
19000
0.5
Acenaphthylene
1.2
3400
11
Anthracene
9.9
69000
49
Benzo(ghi)perylene
Fluorene
0.6
0.2
<500
2.5
16
38000
<0.1
170
Phenanthrene
3.2
19
41000
150
D1benzo(a,h)anthracene
0.9
0.2
<500
<0.1
Indeno(l,2,3-cd)pyrene
0.7
0.3
<500
<0.1
Pyrene
16
15
27000
24
Benzene
<0.1
<0.1
<50
NA
Toluene
<0.1
<0.1
<50
NA
Ethyl benzene
<0.1
<0.1
<50
NA
All concentrations 1n units of micrograms per gram except for XAD collections
which are total milligrams collected.
A-46
-------
TABLE A-14. WOOD PRESERVING TEST RESULTS
TEST CREOSOTE PAN EVAP
TEST 2
TEST DATE
9/24/80
liquid n
COMPOUND Acurex I.D. I
	 80-10-015-
¦20
Pentachlorophenol
13
Phenol
14
F1 uoranthene
64
Naphthalene
18
Benzo(a)anthracene
41
Benzo(a)pyrene
1.7
Benzof1uoranthenes
2.1
Chrysene
26
Acenaphthylene
Anthracene
3.7
26
Benzo(ghi)perylene
Fluorene
Phenanthrene
D1benzo(a,h)anthracene
Indeno(l,2,3-cd)pyrene
Pyrene
< 0.4
75
91
0.4
< 0.4
48
Benzene
Toluene
Ethylbenzene
< 0.1
< 0.1
< 0.1
All concentrations In units of micrograms per gram except for XAD collections
which are total milligrams collected.
A-47
-------
TABLE A-15. WOOD PRESERVING TEST RESULTS
TEST CREOSOTE PAN EVAP
TEST DATE 9/25/80
Liquid
COMPOUND
Acurex I.D. #
80-10-015-
¦52
an Bottoms
in:
ing
-53
-57
TEST 3
TO"
¦74
Pentachlorophenol
7.6
260
1700
2.8
Phenol
31
30
400
60
F1 uoranthene
9.3
590
32000
20
Naphthalene
10
680
24000
2800
Benzo(a)anthracene
4.5
390
20000
1.4
Benzo(a)pyrene
0.6
91
600
0.25
Benzofluoranthenes
1.4
190
650
0.69
Chrysene
3.7
240
15000
1.2
Acenaphthylene
0.3
840
5700
30
Anthracene
2.8
260
12000
70
Benzo(gh1)perylene
<0.1
10
<500
<0.1
Fluorene
8.9
660
36000
560
Phenanthrene
15
1100
37000
200
D1benzo(a,h)anthracene
Indeno(l,2,3-cd)pyrene
<0.1
<10
<500
0.1
16
:500
<0.1
<0.1
Pyrene
6.7
440
27000
13
Benzene
<0.1
6.7
26
NA
Toluene
<0.1
1.4
2.7
NA
Ethylbenzene
<0.1
0.3
0.5
NA
All concentrations In units of micrograms per gram except for XAD collections
which are total milligrams collected.
A-48
-------
TABLE A-16. WOOD PRESERVING TEST RESULTS
TEST	CREOSOTE
TEST,3
TEST DATE
'Drips |
Retort
COMPOUND
Acurex I.D. #
80-10-015-
-54
Pentachlorophenol
1800
Phenol
<10
Fluoranthene
200
Naphthalene
1400
Benzo(a)anthracene
1000
Benzo(a)pyrene
200
Benzof1uoranthenes
500
Chrysene
850
Acenaphthylene
180
Anthracene
1500
Benzo(gh1)perylene
40
Fluorene
Phenanthrene
2600
2200
D1benzo(a(h)anthracene
20
Indeno(1,2,3-cd)pyrene
52
Pyrene
1700
Benzene
15
Toluene
<1
Ethylbenzene
<1
All concentrations 1n units of Micrograms per gram except for XAD collections
which are total milligrams collected.
A-49
-------
TABLE A-17. WOOD PRESERVING TEST RESULTS
TEST CREOSOTE PAN EVAP
TEST 4
TEST DATE 9/25/80
Liquid
)W Sep Top
OW Sep Bot
XAD
COMPOUND
Acurex I.D. #
80-10-015-
-47
-56
-49
-68
Pentachlorophenol
0.5
8.3
1300
2.0
Phenol
35
5.2
800
<0.4
Fluoranthene
6.0
140
13000
27
Naphthalene
6.4
200
38000
2800
Benzo(a)anthracene
2.4
60
9200
1.5
Benzo(a)pyrene
0.4
6.1
3000
0.40
Benzofluoranthenes
0.8
15
500
1.7
Chrysene
1.9
50
5400
1.1
Acenaphthylene
0.2
5700
56
Anthracene
1.4
56
8000
56
Benzo(gh1)pery1ene
<0.1
<10
730
<0.4
Fluorene
6.0
110
35000
740
Phenanthrene
12
190
22000
330
D1benzo(a,h)anthracene
<0.1
<10
1500
<0.4
Indeno(1,2*3-cd)pyrene
<0.1
<10
1300
<0.4
Pyrene
4.2
100
10000
20
Benzene
3.4
<0.1
27
NA
Toluene
<0.2
<0.1
0.5
NA
Ethylbenzene
0.3
<0.1
6.8
NA
All concentrations In units of micrograms per gram except for XAD collections
which are total milligrams collected.
A-50
-------
TABLE A-18. WOOD PRESERVING TEST RESULTS
TEST PCP PAN EVAP	 TEST 1
TEST DATE
9/23/80
Retort Drips I OW Sep Top
XAD
COMPOUND
Acurex I.D. #
80-10-015-
-11
-12
-71
Pentachlorophenol
1500
25000
<0.01
Phenol
< 10
<10
<0.01
Fluoranthene
29
21
0.012
Naphthalene
50
1800
0.026
Benzo(a)anthracene
60
<10
<0.01
Benzo(a)pyrene
50
20
<0.01
Benzofluoranthenes
54
20
<0.01
Chrysene
Acenaphthylene
50
60
16
200
<0.01
0.062
Anthracene
Benzo(gh1)pery1ene
47
240
< 10
<10
0.012
<0.01
Fluorene
110
1500
<0.01
Phenanthrene
150
3000
D1benzo(a ,h)anthracene
< 10
< 10
0.14
<0.01
Indeno(l,2,3-cd)pyrene
< 10
< 10
<0.01
Pyrene
24
< 10
<0.01
Benzene
< 0.5
<0.5
NA
Toluene
< 0.5
65
NA
Ethylbenzene
< 0.5
41
NA
All concentrations 1n units of micrograms per gram except for XAD collections
which are total Milligrams collected.
A-51
-------
TABLE A-19. WOOD PRESERVING TEST RESULTS
TEST PCP PAN EVAP TEST 2
TEST DATE 9/24/80

Liquid 17:15 |0W Sep Top
0VI Sep Bot
XAD
COMPOUND Acurex I.D. #
80-10-015-
-25
-29
-32
-63
Pentachlorophenol
70
14000
4Q000
32
Phenol
C
1.2
<10
<10
<0.01
Fluoranthene
5.2
970
3800
1.80
Naphthalene
0.1
1500
3700
3.5
Benzo(a)anthracene
1.6
200
540
0.20
Benzo(a)pyrene
0.1
40
110
<0.05
Benzofluoranthenes
<0.1
110
380
<0.05
Chrysene
1.2
180
520
0.18
Acenaphthylene
0.1
310
140
<0.05
Anthracene'
0.4
180
400
0.30
Benzo(gh1)pery1ene
<0.1
<10
30
<0.05
Fluorene
0.3
850
2700
<0.05
Phenanthrene
2.6
1800
5000
1.8
D1benzo(a,h)anthracene
<0.1
<10
4
<0.05
Indeno(l,2,3-cd)pyrene
<0.1
<10
15
<0.05
Pyrene
3.6
710
3500
1.50
Benzene
<0.2
<10
0.3
NA
Toluene
0.3
<10
27
NA
Ethylbenzene
<0.2
<10
19
NA
All concentrations 1n units of micrograms per gram except for XAD collections
Mhlch are total milligrams collected.
A-52
-------
TABLE A-20. WOOD PRESERVING TEST RESULTS
TEST PCP PAN
TEST 2
TEST DATE 9/24/80
Liquid 9:00 Fugitive XAT
COMPOUND Acurex I.D. I
80-10-015-

-73
Pentachlorophenol
140
5.0
Phenol
0.5
1.3
Fluoranthene
7.9
<0.1
Naphthalene
0.4
3.6
Benzo(a)anthracene
3.7
<0.1
Benzo(a)pyrene
0.1
<0.1
Benzofl uoranthenes
0.1
<0.1
Chrysene
3.7
<0.1
Acenaphthylene
0.1
0.18
Anthracene
1.2
0.03
Benzo(gh1)perylene
< 0.1
<0.5
Fluorene
1.4
0.2
Phenanthrene
9.5
0.3
D1benzo(a,h)anthracene
<0.1
<0.5
Indeno(l,2.3-cd)pyrene
<0.1
<0.5
Pyrene
6.1
<0.1
Benzene
<0.1
NA
Toluene
<0.1
NA
Ethylbenzene
<0.1
NA
All concentrations 1n units of Micrograms per gram except for XAD collections
which are total milligrams collected.
A-53
-------
TABLE A-21. WOOD PRESERVING TEST RESULTS
WOOD PRESERVING TEST RESULTS	TEST PCP PAN EVAP	TEST 3
TEST DATE 9/25/80
1
-IOUID
O.W.SEP TOP
).W. SEP B01
PAN BOTTOMS ~
__________________ -
COMPOUND Acurex I.D. #
80-10-015-
-37
-51
-42
-35
Pentachlorophenol
70
.45,000
, 980
62
Phenol
I
0.4
<10
<10
1.2
Fluoranthene
2.7
2,800
2,000
2.0
Naphthalene
0.1
2,000
220
1.1
Benzo(a)anthracene
1.4
430
290
0.5
Benzo(a)pyrene
< 0.1
96
68
0.05
Benzofluoranthenes
< 0.1
320
190
0.2
Chrysene
1.0
400
420
0.4
Acenaphthylene
0.3
370
1600
0.05
Anthracene
0.4
1100
400
0.5
Benzo(gh1)perylene
< 0.1
7
< 20
<0.1
Fluorene
2.6
2400
2100
1.0
Phenanthrene
2.4
4000
3600
3.5
D1benzo(a•h)anthracene
< 0.1
<10
<20
< 0.1
Indeno(1,2*3-cd)pyrene
< 0.1
28
<20
< 0.1
Pyrene
2.0
1900
1300
1.4
Benzene
< 0.2
1.2
0.2
<0.2
Toluene
< 0.2
77
0.1
0.3
Ethylbenzene
< 0.2
2.3
1.2
<0.2
All concentrations In units of micrograms per gram except for XAD collections
which are total milligrams collected.
A-54
-------
TABLE A-22. WOOD PRESERVING TEST RESULTS
itST	PCP PAN EVAP
TEST 3
i£ST DATE
9/25/80
W
Fugitive XAC

Ketort urips
COMPOUND
Acurex I.D. #
80-10-015-
-69
-75
-38
-43
Pentachlorophenol
45
1.7
h490,000
2100
Phenol
0.85
< 0.01
<1,000
<10
Fluoranthene
6.8
0.012
<1,000
180
Naphthalene
3.9
1.2
<1,000
200
Benzo(a)anthracene
0.38
<0.01
<1,000
80
Benzo(a)pyrene
< 0.3
<0.01
<1,000
5.6
Benzofluoranthenes
< 0.3
<0.01
<1,000
26
Chrysene
0.34
<0.01
<1,000
85
Acenaphthylene
1.7
0.074
<1,000
11
Anthracene
3.0
0.019
<1,000
55
Benzo(gh1)perylene
< 0.5
<0.01
<5,000
<5
Fluorene
4.0
0.30
<1,000
140
Phenanthrene
12
0.18
<1,000
320
D1benzo(a,h)anthracene
<0.5
<0.10
<5,000
<5
Indeno(l,2,3-cd)pyrene
<0.5
<0.10
<5,000
<5
Pyrene
4.2
0.01
<1,000
140
Benzene
NA
NA
<10
0.1
Toluene
NA
NA
12
0.5
Ethylbenzene
NA
NA
31
0.5
All concentrations In units of micrograms
which are total milligrams collected.
per gram except fbr XAD collections
A-55
-------
TABLE A-23. WOOD PRESERVING TEST RESULTS
TEST PCP PAN EVAP
TEST DATE 9/25/80
PCP Working I Liquid
TO-
TEST 4
Soln.
_=5£L
COMPOUND Acurex I.D. #
80-10-015-
•59

Pentachlorophenol
44000
41
24000
Phenol
< 200
0.3
420
Fluoranthene
430
1.2
1400
Naphthalene
3800
0.3
4700
Benzo(a)anthracene
<100
0.9
160
Benzo(a)pyrene
<100
<0.1
<10
Benzof1uoranthenes
<100
<0.1
35
Chrysene
<100
0.7
150
Acenaphthylene
170
0.1
300
Anthracene
230
0.2
600
Benzo(gh1)pery1ene
<200
<0.1
:10
Fluorene
1100
1.7
1400
Phenanthrene
1700
1.5
1200
D1benzo(a,h)anthracene
<200
<0.1
<10
Indeno(1•2«3-cd)pyrene
<200
<0.1
<10
Pyrene
350
0.9
1100
Benzene
<1
<0.2
NA
Toluene
18
0.2
NA
Ethylbenzene
23
0.2
NA
All concentrations In units of micrograms per gram except for XAD collections
which are total milligrams collected.
A-56
-------
Figure A-14 shows samples from the pan evaporation process. It is
clear that the liquid left behind in the evaporator is concentrated in the
high-molecular-weight polynuclear species such as chrysene and
benzo(a)pyrene. These polynuclears do not volatilize to the same extent as
the low-molecular-weight species. Figure A-14(d) is a chromatogram of an
XAD-2 blank extract. Of the compounds of interest, only naphthalene was
detected in the blank. Duplicate blank samples showed 100 and 140pg of
naphthalene. The XAD-2 cartridge extract shown in (d) is an 8,000-fold
dilution of the total extract. The quantitative result for this sample was
2.8g of naphthalene.
Chromatograms from penta process samples are shown in figure A-15. The
use of petroleum distillate as the penta vehicle complicates the chromatograms
immensely. Since it also contains polynuclear aromatic hydrocarbons. The
concentration of penta in these samples, however, was sufficiently high for
reliable quantitation in the presence of the oil matrix. For lower
concentrations than seen here, an additional sample preparation separation of
neutrals from acids would be necessary.
Figure A-16 shows chromatograms from the penta wastewater evaporation
process. Penta was detected in the XAD-2 cartridge. However, the
hydrocarbons appear to the preferentially evaporated as evidenced by the
concentration of penta in the pan bottoms. No contamination from penta was
seen 1n XAD-2 blanks.
A-57
-------
*«„. ..	J?* MUH2 MSI
•1^1 tlilfctt	CMLIi (MMMM
•mil «-ifr*ts-» Mk.cac to ih.iu.-mb
MNKi C I.2SI UMB.I N 9. «.• MM A I. (.• Ml U ». 9
MM t« ro flSf
2I42M.
I >»S-
UA
t JLlIL l L
»>»	TM
(a) Creosote charge liquid to pan evaporator
ftIC
M/Mt IkNiM	Cft.li OMtiiM tl
SMVUl	Ml 0IL*lt MMM6 M.M.I2
Mtti € I.2M UMLt M I. 4.4 MMi « •. l.t Mli U », )
mm* mm it	km m to tm
mm.

i
9M
IM
l(i«
ism
29i«
»i3i	t«
(b) Creosote partially evaporated liquid
Figure A-14. Chromatograms from creosote wastewater pan evaporation process,
A-58
-------
M4P9I *«•«•
•mil otimw %i-n mm. u.«sm i
MNBIl e I,um Utti N f. 4.0 CM
•ff* MMM M	9CMC |«
Ot.li CtMMtt D
M#.u
I « •. I.« Wt U ». ]
r jJUiUi
•lit	!«»«•	*t«	Hi*
SQM
1W
(c) XAD-2 blank
tic
M#ll t?l4M
MMl N-lNn-
MNii C I
L< M ft. 4.1 IMM. !.• IMIi « ». i
•WW #1	SUNS IM TO 2M

SCIM
IH*
(d) Creosote pan evaporator XAD-2
Figure A-14. Concluded
A-59
-------
lie	(MM WIW 91
%\'\*%\ 2t9hm	MLIi (MWM 91
MfUi N-IHIMI 8NIM.UM9C H.M.U
MMKi C 1.2391 LflM.1 N 9. 4.9 MM • 9. 1.9 Mil V 29. )
SOW 199 10 tm
Nfc»l

»«»	TM
(a) Penta working solution
m
9l*#/9l 2i2>i99	OI.li CMM9IC 94
MfUi M9-I9-9I9-49 9UP MMUL-29M6 99.19'12
MMSs C 1.2299 UAi N 9. 4.9 9UM * 9. 1.9 Mi U 29. 1
w* £IMK 91	KM9 199 T9 2299
(b) Penta retort drips
Figure A-15. Chromatograms of penta process samples.
A-60
-------
IMVlli MM#41*42 Ml ONM.MMM
MNKl C I.SIN UAi N I. 4.1 ft!
OATAi MM II
0«.tt OMMIC M
11.12
* •. I.I Mit u ». »
(c) Penta oil/water separator — bottom layer
NIC	WV* Mttt II
\VW* Ili42t«		 CM.il CI2MM M
MMi M-1MIV12 IN 01un(.SF-M. H1-3M M. 14.12
—i 6 i,xm ufti m •. «.# mm * t. i.« bmii v a. i
mm Mioaa
(d) Penta oil/water separator — top layer
Figure A-15. Concluded
A-61
-------
tie
•SMOCTCL
um.1 N I. «.•
can c
i. *.12
t. I.I Mil U
SOWS 149 TO 2SM
L


(a) Penta pan bottoms
RIC
M/tMl ItlftM
¦i« i.:
OUT* MM90 tl
UNLl » ». 4.* MM * l.« Mil U M, 1
(b) Penta XAD-2
3m	«m
TiiM	IIH
km m to an
1IIC
Figure A-16. Chromatograms of samples from penta evaporation process.
A-62
-------
(c) Penta test liquid
Figure A-16. Concluded
A-63
-------
Section A-2
RAW DATA: SOURCE EMISSION SAMPLING FOR HIGH-MOLECULAR-WEIGHT EMISSIONS
A-64
-------
ACUREX CORPORATION
Run /-f+P fiAAi
Acurex Project No.	. 21
Field Dates 2., -2u -VfQ	
Plant			
Sampling Location fi'Aft
Sa-pling Date		
FIELD CREW
Cre* Cnief:		^fotrp	C.		
Testing Engineer: 1	
Engr. Technician: 1	*ty~>
2	fp	k ^iou-i.1^^
Lab Technician: 1 flfTn	^ pc:c c
I	
Process Engineer: 1_
2_
Other:	1
A-65
-------
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A-66
-------
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Date <*-2+-fro	
Sample Location Pc,? g\M.c>	
Test Wo./Type i	

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Molecular weight, stack gas dry
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A- 68
-------
ISOKINETIC PERFORMANCE WORKSHEET (Concluded)
Molecular Might, (tack gas wet
(Ib/lb-mole)
Mdd-B^) ~ 18(8^), (21^(l-,t2i) 4 IBUZjQ
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XI

A-69
-------
ACUREX CORPORATION
Run 2- tv.p Pmo
Acure* Project No.	.2.f>	
Field Dates ^g-2.		
Plant_		
Sampling Location PAnJ g.'ArVS
Sar.pUng Date 9-In-kV	
Crew Chief:
Testing Engineer:
Engr. Technician:
Lafc Techniciar:
Process Engineer:
Other:
FIELD CREW
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A-70
-------
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»0»n lED-O." t
-------
ISOKINETIC PERFORMANCE WORKSHEET
Plant		_ Perform*! by
Date Q-gy-??	
Sample Location PiP t*w
Test No./Type 2 /		
«T . 17.33 (T, ~ 46Q)(VW std ~ Vffi ,td)
e v; T% S?~
where: XI ¦ Percent Isokinetic
Temperature stack gas, average (°F)
Ts

Meter volume (std), 17.6<^| ^ ^ 460^


17,64 yzEZT/ \(or»* w j
*m std
,ctlt
Volume of liquid collected (grams)
Vlc
1 -> ^* •»
Volume of liquid at standard condition (scf)
Vlc x 0.04707
Vw std
C t
1
Total sample time (minutes)
0
i
o
Stack gas proportion of water vapor
». M . <4SiZ>
v. >M * 1. «d to' ~ LfefT
Bwo
-It)
Molecular weight, stack gas dry
(lb/lb-mole)
Md
ofl-W
A-72
-------
ISOKINETIC PERFORMANCE WORKSHEET (Concluded)
Molecular weight, stack gas wet
(lb/lb-mole)
Mdd-s^) 4 18(bwo)! (aiDd-JO 4 lB(«2j&)
Ms
/Sr.
Absolute stack pressure (1n. Hg)
/,„ck ('"• «j0) f , <_£_>
'b * 1M • <—1 * 1S.J
Ps
ai.ao
Stark w»1nrlty (fps)
1	 /T.'vg ~ 460
85.49 (Cp) H,
/ / (	) ~ 460 \
85.49 (_)(V—(_)(_} )
Vs

Nozzle diameter, actual (Inches)
Nd

17.33 (	~ 460)((	) ~ (	))
(	)(	)(	)(	)z
XI

A-73
-------
ACUREX CORPORATION
Run Pr r> PAJugtrfftP
Acurex Project No. ^oiint.9 .7i,	
Field Dates_9-22. 2	<¦
Engr. Technician: 1
Lab Technician: 1 ftg.-r* -t-^gPF-g.'-
2
Process Engineer: 1_
2_
Other:	1
A-74
-------
FiaO MTA
hqt K of *
tribe least* md Tjpe T< G_
NoitCl 1.0. (Wo. 1 ro J A	
»«¦»< Notlturi		
Molecular Wet^it, #rjr, (^|_	
Meter Im WiMbtr IL	
Hetfr Coefficient L--. r.hlV	
• r*ctor ,«nc-	
K - 		
»1M)' • « (	~
»" ¦ K(«d)' (f?)
Trwrw
Hint
\ Clack Tint
V did
\
Ttaa, ala \
te Meter
ftcatlaf .
<«b>. « J
hlocttj
n*«d
teF,).
(a. $0
Orlflca frtiirt
•Ifferenttal
*N). fa. HjO
Taaperatara «F
F*P
Vac Mi
la. Nf

Stack
Frobe
lap!agar
Orfjalc
iMale
0«an
Sat Meter

I»1t. Sz^ioo
Desired
Actaal
la
Oat

S~ CSril
z>o.to»



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-f l-^C-trO	
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$a»ie T—  ^*,e>
Rm ¦¦*¦_ ^		. m ifco
«Nr«ur__b. ft SV	Silk* 6el
Static Fra*s«re. (NjO)		1 (c*S *2d	
FlltaraM*)	;			 	 11* S*SL
3»
•li	laak Check; Ialtlal at rC *
«*	Flaal at	' N*.
Coaaents:
-------
ISOKINETIC PERFORMANCE WORKSHEET
Plant_		 Performed by ^
Date ef.9r.iu 	
Sample Location PcP.rAr-' r-*.t>
Test Wo./Type >-		
fI - 17.33 (T» ~ 460)(»w ,ta * V» std^
where: XI • Percent Isokinetic
Temperature stack gas, average («F)
Ts
\-
Meter volume (std), 17.6+ llo"^


/(^A/fe^ * ulj\
Vm std

Volume of liquid collected (grams)
Vlc
5"
Volume of liquid at standard condition (scf)
Vlc x 0.04707
std
yr.77t
Total sample time (minutes)
e

Stack gas proportion of water vapor
». Itd &»
V. ,u 4 ltd 4 <**>'
Bwo

Molecular weight, stack gas dry
(lb/lb-mole)
Md
21.M
A-76
-------
ISOKINETIC PERFORMANCE WORKSHEET (Concluded)
Molecular weight, stack gas Met
(lb/lb-nole)
Mdd-B^) + 18(Bwo)* bi-rMl'-W + lSf.8Jg)
Hs
xao3C>
Absolute stack pressure (in. Hg)
Pstack ^2®^ ( -' )
pb ~ 13.6 »~ -nnr
Ps
2 MO
Staek velocity (fas)
I	. /T avg ~ 460
«•«»  
-------
ACUREX CORPORATION
Run V>f>cP gi/Af
Acurex Project No. Iq-HoLIId
Field Dates 1-2-? 2l-<«o
Plant		
Sampling Location W.P -Pa+j gj-Afi.
Sampling Date 1-2 g"- Sr(j	
FIELD CREW
Crew Chief:		C,	/»<	
Testing Engineer: 1	>^-1.	
Engr. Technician: 1_
Lab Technician: I	R C-r*	J
Process Engineer: 1_
2_
Other:	1
A-78
-------
FiaO MTA
r»ft	or
Maat_
Ml

So*1a Lecatlow Pc-P gi/Ap.
sawte t— yfth.t	
i« »»«>	Jfc	
^w*w_jfeak£B5i	
rlf 	
*»
I
VO
**1«* T«
•areartrlc	3^ VSvg>
Static Prtttwt, (y)	
Filter		
//:rt>*
leak Check; Initial at It" * Nf, .W- CCFB
Flaal ft 	" No. 	CFM
laplnoer Telaaes
Initial Final
ffT> 3L 1 ais.1
S"7*. a&.
Prehe Lcnfth mtd Tjpej££_
¦oitd 1.0. (Ha.)	K>/&
OsinJ Moisture	

•taleceler	try, (*<)_
Meter (o« Oiwter t //_
Meter Coefficient^
» Factar	
It ¦	
c»g ,rt•
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Vacaaa
la. Nf
&
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Firtt
l^loier
Organic
Module
Oven
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o
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Desired
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f I /c


-------
ISOKINETIC PERFORMANCE WORKSHEET
Plant		Performed by	w "
Date	—		
Smple location fr- T>
Test No./Tvoe *+ / * ». fc "L.	
tl . 17.33 (Tt 4 460)(Vw >td ~ Vm ,td)
i Tt p~$ n7~
where: *1 ¦ Percent Isokinetic
Temperature stack gas, average (»F)
Ts
%OL-
Meter volume (std), 17


"'6< V^f/V^' * « /
\ std

Volume of liquid collected (grams)
Vic
sr^.o
Volume of liquid at standard condition (scf)
VIc x 0.04707
vw std
&
Total sample time (minutes)
0

Stack gas proportion of water vapor
Vw std .
v„ std * vm std <*4 * {m
Bwo
. lit. 7
Molecular weight, s'tack gas dry
(lb/lb-mole)
Md
V.tf
A-80
-------
ISOKINETIC PERFORMANCE WORKSHEET (Concluded)
Molecular weight, stack gas wet
(Ib/lb-mole)
Md(l-Bw) ~ 18(8^). (2£2y)(l-Jfei) ~ 18Lata)
Ms
%o^Z_
Absolute stack pressure (1n. Hg)
. pstack (1n* H2°>
h * is.* • + "irr
Ps
ZW
Stack velocity (foil
1	 /T.avg ~ 460
«¦« (Cp) (>, „,U \ Ht
11 (	) ~ 460 \
MM <	HV ^ )
vs

Nozzle diameter, actual (Inches)
N d

17.33 (	~ 460)((	) ~ (	))
(	)(	)(	)(	)z
XI

A-81
-------
ACUREX CORPORATION


Run /- £*,*{>
Arnr*x Prolect NO. ?£>">{« VZ , 2 He c /*i
2


3

Engr. Technician:
1

2


3

Lab Technician:
1 G e-rt*
Hc.FFr(L**V

2


3

Process Engineer:
1

2

Other:
1


2




A-82
-------
FiaO OATA
'*9* JL*i_
00
W

*-24~ t*
S«*U Limtw **	f-\
5«pH Tjp«_J	
Kw
a-. »w^v
IrHtrll *r«SMra_ "TRT
Statu Nturt, (NjO)	
FII tar —>i(»)			
laak Chaeks lattlal *	N.
Ftaal at 	' «i.
an
CFH
h»tiw(r »olwei
iffD
lnttUl Final
14° 	f
S1ltc« Cat J (>***&£+<*$
Frafce leofth an4 T— T^-A Ht<3T- 'V
Ootid 1.0. Wo.l VfA	
At(«wd Ntlltarc	
Htltctlr Dclfit, Dry, (N4)_
"»t«r	&\
- —
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• f«cUr • *tT?	
I
'	* (	)'
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9: 34 A*\
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&
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(km
la. Hf
&
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Cawinti:
-------
ISOKINETIC PERFORMANCE WORKSHEET
Mint c,r f-p,./.		 Performed by
Date	**j CoaT-
Test No. /Type / / k ?	
(I > ^>33 (Tt + 460)(VW * Vm std^
5 T§ rs 5JT"
where: XI ¦ Percent Isokinetic
Temperature stack gas, average (°F)
Ts
>11
Meter volume (std), 17-^t) (f* ~
Ax&»\/to- {^=L\
*m std
n- is*
Volume of liquid collected (grams)
Vlc

Volume of liquid at standard condition (sef)
Vlc * 0.04707
Vw std

Total sample time (minutes)
e
3C.P
Stack gas proportion of water vapor
Vw std (HAL)
vw std * ym std + «Z£k>
Bwo
,(*Z f
Molecular weight, stack gas dry
(lb/lb-mole)
Md

A-84
-------
ISOKINETIC PERFORMANCE WORKSHEET (Concluded)
Molecular might, stick gat wet
{lb/lb-mole)
MdU-S^) * ~ IHjtil)
Ms

Absolute stack pressure (In. Hg)
'stack ( c )
\' ' n.t 8 ¦m-mr
P.
M-W-t?
St»rlt w«loe1tv ffosi
		 /T avg ~ 460
85.49 (Cp) (J», H>
/1 (	) ~ 460 \
85.49 (_)(/— ^ (_)(_} )
Vs

Nozzle diameter, actual (Inches)
Nd

17.33 ( ~ 460)({	) ~ (	))
(	)(	)(	)(	)z
XI

A-85
-------
ACUREX CORPORATION
Run %-c.zf.c	gVrtfr
Acure* Project No. *?t'*7	
Field n«tM ^.2? gr.-40	
P1 ar.t			
Se-pling Location cgfco Pa*j	
Sampling Date 1	
FIELD CREW
Cre» Cnief:	fcftm.fi	C ,tN a-R«x	
Testin; Engineer: 1 j~o rr»J	t. iv>	
2		'
Engr. Technician:
Lab Technician: 1 Rc Th ifg ppgj.n»*hJ
2	
Process Engineer: 1_
2.
Other:	1
A-86
-------


Flam
om "J-xr-ira	
T«m Loeabon 0/£C	'
Z*JL-
3»
I
a>
¦V4
Boiowalrc Pmsui«
Slal« Pressure
Slack Pressure
Probe Number
FMtMG£n
ar~
ttlX
tffV.
slSs:

silica
GEL.
EE *23
TIME
«r
Vl°
te>
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Or
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1 1
-------
ISOKINETIC PERFORMANCE WORKSHEET
Mint 	 Performed by jv^gT
Date
Sample Location r .nr., g..^f
Test Wn /Tvpg 2. /*At-
SI • Hs * **0)(Vw ltd * »t(P
5 v; Ft nJT"
where: SI » Percent Isokinetic
Temperature stick gas, average (°f)
T,
nr.
Meter volume (std). 17.6^^ ^


/<223\(%ip+ \
17,64 \T3s3V Wb ~ /
*« std
Tf Pz
Volume of liquid collected (grams)
Vie
ii Wt
Volume of liquid at standard condition (sef)
Vlc * 0.04707
V* std
55-2/
Total sample time (minutes)
e
5"6
Stack gas proportion of water vapor
». ,td aa>
V. «« * ». M (ttill ~ uw

M7
Molecular weight, stack gas dry
(lb/lb-mole)
"d

A-88
-------
ISOKINETIC PERFORMANCE WORKSHEET (Concluded)
Molecular weight, steck get wet
(lb/lb-mle)
Mdd-B^) * 18(BW), -J£Q) * utu/y)
\
2ZJZ
Absolute steck pressure (In. Hg)
W (1«- V) , to.)
'b * u.s • ~ irr
Ps

Stark velocity (fps)
I IT.WJ ~ 460
.5... (Cp) <>, „,)J V, \
	 // (	) ~ 460 \
85.49 C	)« )
vs

Nozzle d1«Mter, actutl (Inches)
"d

17.33 ( _ ~ 460)((	) ~ (	))
XI

(	)(	)(	)(	)l
A-89
-------
ACUREX CORPORATION
Run
Acurex Project No. •tmi.L.TL .10
Field D8tes_l=Jfc2rSLfejjE£	
Plant	
Sampling Location reco P+mi gjjAfr
Sampling Date f-2C-ScO I
FIELD CREW
Cre* Chief:
Testin; Engineer: 1 /Tamw V4p	
2	_
Engr. Technician: 1_
Lab Technician: 1 Retw	HcfPc^io^O
Process Engineer: 1_
2
Other:	1
A-90
-------
F1B.0 MTA
r«fc	tr	
Mart
9-ag-ao

suite
Flltar ¦¦ai(t)	
i
'cm
WWW
Initial Ftagl
ffp 2t£I
1 ffc> «l>
*»t arr
Silica B«l
srer* idle

fraU laaftk amt Tm inAt*r
¦mmi i.«. (a».i -	
kiitmai Nstttara		
Nalacalar Mat#t. K*. (*.)_	
	
NeUr Cmft tela*	.«e»&r*> |r - «re i.
¦ Pactar .q«tc	
K •			
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\ Cladt Ttaa
»n \
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(V. « 3
Valaclty
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-------
ISOKINETIC PERFORMANCE WORKSHEET
P1 ant 2c--Sro	:	
Sample Location AJg/i
Test Ho./Type		
J] ¦ (T$ ~ 460)(Vm ~ Vju jtj)
5 Tt rt S7~
where: *1 » Percent Isokinetic
Temperature stack gas, average (°F)
Ts
n&r
Meter volume (std), 17 ,64^t) ^
/etsaA/caa^ + (-j^) \
°yWi^ Ho /
*m std

Volume of liquid collected (grams)
Vie
7b2 5
Volume of liquid at standard condition (scf)
V1c x 0.04707
*w std
?5-.sr<
Total sample time (minutes)
e
t/S~0
Stack gas proportion of water vapor
*w std . (22£)
V. std * ym std «**«» * U^zT
®wo
. U> 1
Molecular weight, stack gas dry
(lb/lb-mole)
Md

A-92
-------
ISOKINETIC PERFORMANCE WORKSHEET (Concluded)
Molecular weight, stack gas wet
(Ib/lb-mole)
MdO-B^) 4 18(6^), (3^(1-^) ~ 18(&L)
"s
-X-21Z
Absolute stack pressure (In. Hg)
(1». HjO) ... . l_2J
pb * 1 .tmi'nrr
%
aw
Stark velocity ffp«)
i	 /T.avg ~ 460
«5.« (Cp) (>, \ \
/1 (	) ~ 460 \
Vs

Nozzle dimeter, actual (Inches)
Nd

17.33 (	~ «60)((	) ~ (	))
(	)(	)(	)(	)*
XI

A- 93
-------
ACUREX CORPORATION
Run	ftiAP
Acurex Project No. 2t>fCmk.1 .Qr>
Field Date* c.qg ft/--iD
Plant •		
Sampling Locationc.e.£.c> &,)A>
Sampling Date ^.ar>-------
Fiat MTU
£_ * 2=
n«

hwi*unihi r£tt>. P*n. /smt:
t— jOK> 2. «->0^
£££>
LMkONCki taHUI « /^' N../	
	 —
h t*l iMftk iri Tjpf»_
•micI I.I. III.)
>»!¦!( IMftr*
tetania- NM#t. fry.
WtUr — -**r flgy
Nctar Ca*frtcl'(*) (&~)
ill
\ ClMk T1m
XjJB
nsrx \
^MNaT.
IV. «'
•*25'
&
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Mfhwitil
Mh ta. «]•

i2Twi
&
SUek
Ml

Orfwlc
(Malt

tatlMar

71.444
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I
to
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ill
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ta Nrtar
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In. M
Orlfla Nun
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Toper tturc «F

VacaM
fa. N|
'^T •
-------
ISOKINETIC PERFORMANCE WORKSHEET
Plant_		 Performed by
D»te o-<2
-------
ISOKINETIC PERFORMANCE WORKSHEET (Concluded)
Molecular weight, stack gas wet
(1b/lb-mo1e)
Mdd-B^) ~ lSIB^), frMvHUMT/ ) ~ 18(*i£)
\
1
Zi-it
Absolute stack pressure (In. Hg)
- , Pstack ^1ni h20' mrr,
pb4 13.8


Stack velocity (fnsl
¦ /Teavg ~ 460
«•« «,) (>, H,
/ / 4 *60 \
«.•<_>w—^ )
Vs

Nozzle diameter, Ktual (Inches)
Nd

17.33 (	~ 460)((	) ~ ( )r
XI

(	)(	)(	)(	Y
A-98
-------
ACUREX CORPORATION
Run / Pt-P
Acurex Project No. 2o~)ui*2 7.Q
Field Dates
Pl»nt_.		
Sampling Location P^P gfcrfcftr
Smpllng Date S.fl'ie
Crew Chief:
Testing Engineer:
Engr. Technician:
Lab Technician:
Process Engineer:
Other:
HELD CREW



A-99
-------
Fia> MTA
'i*	of
>.
I
I—»
8
zA3=i&-
SmUto twHwPt.P gg-rafeT
T*«		
X
J. Hfltw
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n.*£~
Static hwwt,
Flltar
s teMlal «t ft ¦ Ha. cm
fimI at 2L_r ni'cn
JgtggJijSH
iMtui rjsji
jnr_ 	
/tn>	-io
_£3I_ 	
snjEtM
_ . S\~

frofca iMftb md TtnTFfL
¦n»1 i.o. w».) h/a
•hmH Natstara	
Nalccaltr	try, (M^)_
Hatar >•» Bl^tr £>IU
HHar twffltlw> .. --
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ta IIrtar
Kaaflaf .
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htalti
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kN).
la. |(0
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lifrntiil
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Toparrtara *
slTwI

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Prafea
ta»lagar
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—tS£2_
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ISOKINETIC PERFORMANCE WORKSHEET
Plant	Ece-ls	 Performed by V-^
D«t« <,.?">-kQ 	
Simple Location p^p £ct^7
T«*t No./Type	, /		
%i m	(T$ ~ 460)(VW ttd * st<0
e T% Fs n£~
where: XI • Percent Isokinetic
Temperature stack gas, average (V)
Ts

Meter volume (std), 17
W)
V« std
iu n
Volume of liquid collected (gran)
Vlc
jrs-r
Volume of liquid at standard condition (scf)
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Vw Std
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Total sample time (minutes)
e
/i.tj(ft
Stack gas proportion of water vapor
'w std . («i_^)
*w std * *m std ' +


Molecular weight, stack gas dry
(lb/lb-mole)
"d

A-101
-------
ISOKINETIC PERFORMANCE WORKSHEET (Concluded)
Molecular weight, stack gas wet
(lb/lb-mole)
Md(l-Bw) ~ WtB^). (afcfcMl-j2£I * 1
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sr-if
Absolute stack pressure (In. Hg)
'stack , »,W\ H,
(h > + «o \
vs

Nozzle dimeter, actual (Inches)
Nd

17.33 (	~ 460)((	) ~ (	J)
XI

(	)(	)(	)(	)z
A-102
-------
ACUREX CORPORATION
Run g-Pc.fi
Acurex Project No.	. 2n
Field D.fi q-^-? 2 c. - fen	
Plant			
Sampling Location P»t> ggre^T
Sampling Date 
-------
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ISOKINETIC PERFORMANCE WORKSHEET
Plant			 Performed by \
Date		
Sample Location Pc n C.c- '.7
Test Mo./Type		
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5 7% fl
where: *1 ¦ Percent Isokinetic
Temperature stack gas, average (OF)
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Meter volume (std), 17.64^)^ *
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vie
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Volume of liquid at standard condition (scf)
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Total sample time (minutes)
e

Stack gas proportion of water vapor
vw std . CLi_i)
Vw std * \ std
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.cyo y
Molecular weight, stack gas dry
(lb/lb-mole)
Md

A-106
-------
ISOKINETIC PERFORMANCE WORKSHEET (Concluded)
Molecular weight, stack gas wet
(lb/1b-»ole)
Mdd-B^) ~ 	) ~ 18(	)
"s
2.1 ! Z.
Absolute stack pressure (1n. Hg)
r , '.uck ('»• V> , <-£_>
b 1S.6 ' * 13.6
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Z*fA +
Stack velocity (fps) 	
		 /T avg ~ 460
85.49 (Cp> (>, „,)V\ H,
/ / (	) ~ «0 Y
vs

Nozzle diameter, actual (Inches)
Nd

17.33 ( ~ 460)((	) ~ (	))
(	)(	)(	)(	>z
XI

A-107
-------
ACUREX CORPORATION
Run Pc-P gCT0^7
Acurex Project No. -2e-->^ -1> a /)	
Field Dates g-g?_. 2L-fcD	
Plant_		
Sampling Location Pf P gg/tt-gT	
Sampling Date		
FIELD CREW
Crew Chief:	JS
Testing Engineer: 1_. TWm	m
Engr. Technician: 1_
Lab Technician: 1 /Rf -th mnw.1
2	
Process Engineer: 1_
2_
Other:	1
A-108
-------
FIELD MTA
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Caenenti:
-------
ISOKINETIC PERFORMANCE WORKSHEET
Plant			 Performed by
Date		
Sample Location Pr.P gfffl-er
Test No./Type ? / x*N ?	
«T ¦ 17.33 (Tt ~ 460)(VW ttd ~ V, ,td)
e Ts pI S7~
where: tl ¦ Percent Isokinetic
Temperature stack gas, average (OF)
Ts
-
Meter volume (std), 17'6*(t) (t* I


/(^W,+ UJ\
"•"ySSy\li24* M 1
*m std

Volume of liquid collected (grams)
Vic
5".'
Volume of liquid at standard condition (scf)
VIc x 0.04707
V* std
.2«+
Total sample time (minutes)
0
/<.o
Stack gas proportion of water vapor
Vw std .
\ std * \ std * feuJ
Bwo
o.oi
Molecular weight, sfack gas dry
(lb/lb-mole)
"d

A-110
-------
ISOKINETIC PERFORMANCE WORKSHEET (Concluded)
Molecular weight, stack gas wet
(lb/lb-Bole)
Hdd-B^) 4 lBCB^), (;, ,-)(!- n ) ~ 18( -- )
"s
1
n.nz
Absolute stack pressure (1n. Hg)
r Pstack (1n* h20) A <-JL)
pb + 13.6 • <2129 4 1TT
%

Stack velocity (fos)
		— /T.avg ~ 460
«5.« (C„) (>, K,
M ( ) * 460 \
«s.« (—KV )
Vs

Nozzle diameter, actual (Inches)
Nd

17.33 (	~ 460)((	) ~ (	))
*1

(	)(	)(	)(	)z
A-lll
-------
ACUREX CORPORATION
Run /-f.&ga fiercer
Acurex Project No. ta'lkt/? .
Field Dates	at- 	
Plant		
Sampling Location rrcn Pg-nrcf
Sampling Date		
Crew Chief:
FIELD CREk'
-^>CLtH.C,—C .
Testing Engineer: 1 vfot+w;
2	
Engr. Technician:
Lab Technician: 1	^cta
2 	
Process Engineer: 1_
2_
Other:	1_
2
A-112
-------
HELO MT«
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sa*iinq Location Q£gO. (2.eTae-r.
Counts:
-------
ISOKINETIC PERFORMANCE WORKSHEET
Plant			___ Performed by \\-
Date a-? H-33 (T$ ~ 460)(VW ttd 4 vB ^d)
wtiere: XI ¦ Percent Isokinetic
Temperature stack gas, average (»F)
Ts
6>1rI
Heter volume (std), 17
/**)/<*&* 
Volume of liquid at standard condition (scf)
Vlc x 0.04707
std
£r
Total sample time (minutes)
e
2!
Stack gas proportion of water vapor
». ,td .
K ,td *». ,« • lss<2>

0
Molecular Might, stack gas dry
(16/ lb-mole)
Md
w .y**-
A-1I5
-------
ISOKINETIC PERFORMANCE WORKSHEET (Concluded)
Molecular Might, stack fas wet
(lb/lb-mole)
Mda-B^) ~ ib(6w)i ~ uijbO
"s
1
jn.n-
Absolute stack pressure (In. Hg)
Pstack <1n' H20) a (—11
' ia.t ' • <2* ~ tjt
Ps

Stack velocity (fps)
/	 /T,a*g ~ 460
8S.« (C„) (>C, M,
/ / (	) ~ 460 \
Vs

Nozzle diameter, actual (Inches)
Nd

17.33 (	~ 460)((	) * (	))
XI

(	)(	)(	)(	)Z
A-116
-------
Section A-3
RAW DATA: TOTAL HYDROCARBON AND SPECIFIC LOW-MOLECULAR-WEIGHT DETERMINATION
A-117
-------
DATA COLLECTED: 9/23/80
A-118
-------
-------
-------
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DATA COLLECTED: 9/24/80
A-126
-------
-------
I
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-------
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A-132
-------
-------
-------
-------
&
-------
DATA COLLECTED: 9/25/80
A-137
-------
-------
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APPENDIX B
CHARACTERIZATION OF MULTIMEDIA EMISSIONS FROM
SPRAY EVAPORATION OF WOOD PRESERVING WASTEWATERS
CONTENTS
B-l Program Description and Results
B-2 Raw Data ~ Sample Identification and Field Data
B-l
-------
SECTION B-l
PROGRAM DESCRIPTION AND RESULTS
This field test program was conducted at a wood treating plant
utilizing a spray pond evaporation device to reduce its generated wastewater
volume. The program was designed to determine the organic emissions from the
spray pond and the resulting sludge layer, as well as the input wastewater.
Each stream was qualitatively and semiquantitatively analyzed for organic
compounds, including volatile organics, chlorinated dibenzo-p-dioxins,
chlorinated dibenzofurans, chlorinated phenolic compounds, and polynuclear
aromatic hydrocarbons (PNA's).
A cryogenic sampling system developed by the University of Arkansas was
used to collect samples of the spray pond emissions. The sampling system
collected six simultaneous samples at a single location at different heights
above the pond surface. This program was focused on determining if organic
emissions were discharged to the air during evaporation and on attempts to
determine if the transport mechanism could be established: possible
mechanisms were simple evaporation or aerosol drift. In addition, a
comparison between the cryogenic sampling system and resin trapping methods
was conducted.
B-3
-------
B.l TEST SITE
The wood treating facility selected for field sampling employs two
treating cylinders utilizing the closed steaming process. Both cylinders can
treat wood using pentachlorophenol (penta) formulations, and one cylinder is
designed to use either penta or creosote. Table B-l presents a summary of the
treating production matrix for the field test period. Wood products treated
at the plant consist almost entirely of Southern yellow pine in the form of
utility poles and lumber.
Wastewater and byproducts generated as a result of the treating process
are discharged into discrete oil/water separators. Each separator has a
capacity of 10,000 gal. Primary separation is carried out as a batch process
with an average retention time for separation of 18 hrs. The tanks are
operated manually, and the recovered treating formulation is returned to the
appropriate bulk storage tank. Creosote wastewater is discharged directly
into the spray pond. Wastewater from the penta primary oil/water separator is
further treated by a three-zone gravity separator employing a skimming device
to recover any remaining penta residue; after treatment the wastewater is
discharged into the spray pond.
Figure B-l presents a diagram of the spray pond showing its dimensions
and the placement of spray nozzles. Pond water is recirculated to the spray
nozzles by a pump situated in the northeast corner of the pond. The spray
pond is operated 24 hrs/day unless local wind conditions cause excessive
drifting of the generated spray. Figure B-2 presents a photograph of the pond
in operation.
B-4
-------
TABLE B-l. PRODUCTION MATRIX (ft3)
Period 11-18-80 to 11-20-80
Creosote	Penta
11-18	1,403	2,721
11-19	3,013	2,749
11-20	1,432	3,039
Total	5,848	8,509
Southern yellow pine — utility poles
B-5
-------
Figure B-l. Diagram of spray pond layout.
B-6
-------

Figure B-2. Photograph of spray pond.
B-7
-------
B .2 FIELD TEST PROGRAM
The sampling program conducted included each of the tests described
below:
•	Determination of atmospheric characteristics at the spray pond
•	Fugitive emission sampling at the spray pond using University of
Arkansas concentration profile apparatus (CPA) in conjunction with:
— Cryogenic U-tubes
-- Tenax traps
-- XAD-2 cartridges
•	Liquid grab samples of spray pond wastewater
•	Solid samples of spray pond sludge and soil samples in areas near
to spray pond
Table B-2 presents a summary of the field test matrix for the sampling
period. The following subsections describe the methods and procedures
employed during sampling.
B.2.1 Fugitive Emission Sampling at the Spray Pond
Sampling of fugitive emissions from the spray pond was conducted using
the concentration profile apparatus (CPA) developed by the University of
Arkansas, College of Engineering, Fayetteville, Arkansas. The CPA used during
the field test program consists of three devices and some auxiliary support
equipment described as follows.
Wind Velocity Profile and Direction Indicator
This device consists of a mast with cup anemometers positioned at 20
cm, 40 cm, 80 cm, 160 cm, 240 cm, and 320 cm and a wind direction vane mounted
on top. Anemometer rotation speed and wind direction is transmitted to
appropriate recorders operated by a 12-volt (lead/acid) battery. The unit was
B-9
-------
TABLE B-2. SUMMARY OF SAMPLES COLLECTED
Sample
Air samples —
spray pond non-
isokinetic sampling
Liquid samples --
composited grab
sampling
Solid samples --
composited sludge
sampl ing
1
4-XAD2, cryogenics
and field volatiles
using Tenax
1-composite
1-composite
2
4-XAD2, cryogenics
and field volatiles
using Tenax
1-composite
1-composite
3
4-XAD2, cryogenics
and field volatiles
using Tenax
1-composite
1-composite
B-10
-------
obtained from C. W. Thorntwaite Associates (Model 106). Figure B-3 presents a
diagram of the device as assembled for field use.
Pry Bulb Temperature Device
This device consists of a small metal cup filled with modeling clay,
centered in a short section of white PVC pipe to shield the clay from radiant
energy. These units are mounted on the mast with the cup anemometers using
the same spatial arrangement described for the wind velocity profile mast.
The temperature of the clay is measured periodically using a hand-held Doric
digital temperature indicator and a small RTD thermocouple. Figure B-3 also
presents a diagram of the dry bulb temperature devices as they were used in
the field.
Air Sampling Device
This assembly is not an off-the-shelf item but was designed and
constructed by the University of Arkansas College of Engineering. The device
consists of a 2m mast equipped with holders at six positions for small
(300 ml) Dewar flasks and U-tube cryogenic traps. Tube extenders, upstream of
the traps, allow precise sample heights to be chosen and maintained. The
downstream side of the U-tube traps are connected to Matheson No. 602 air
rotometers. Flow is maintained by a portable hand-evacuated vacuum tank which
was modified during the course of testing to operate from a Thomas Teflon
diaphragm vacuum pump. Figure B-4 presents a diagram of the construction
details for this device. Figure B-5 presents a detailed construction view of
the Dewar flask bracket assembly. Figure B-6 presents a photograph of the CPA
in sampling position.
Sampling fugitive emissions from the spray ponds was performed using
the CPA in conjunction with three different sample collection methods. These
B—11
-------
Figure B-3. Diagram of wind velocity profile and direction indicator
and dry bulb temperature devices.
B-12
-------
Figure B-4. Construction details of air sampling device.
B-13
-------
Figure B-5. Detailed construction view of the Dewar flask bracket assembly,
B-14
-------
Figure B-6. Photograph of CPA in sampling position.
B-15
-------
included cryogenic U-tube traps, and Tenax and XAD-2 microreticular
adsorbents. In all cases the sampled gas/aerosol was routed through a
specially modified midget impinger prior to entry into the appropriate sample
trap. The midget impingers modified the Smith-Greenburg design by shortening
the impinger stem which raised the impaction plate above the liquid collection
area. The purpose of this modification was to separate and collect the
aerosol fraction of the sampled stream, ultimately extending the effective
sampling time of the cryogenic U-tube traps by limiting the amount of
freezable material entering the trap. Figure B-7 presents a diagram of the
modified Smith-Greenburg midget impinger. The modified impingers were used in
conjunction with all three sampling methods for the purpose of uniformity.
Cryogenic U-tube traps were constructed from 316 stainless steel
tubing, 1/4-inch O.D. by .020-inch wall thickness. Each tube was packed with
glass beads ranging in size from 1.00 to 1.05 mm, purchased from B. Braun
Melsungen, AKTIENGESELLSCHAFT, W. Germany. A small pyrex glass wool plug was
inserted into each end of the packed U-tubes to retain the beads. Figure B-8
presents a diagram of the completed sampling device. Prior to use in the
field the tubes were analytically cleaned.
To effect sampling with the cryogenic U-tubes, the CPA was positioned
at the optimum downwind location of the spray pond. The sample devices then
were affixed to the CPA at the appropriate heights, with the body of the trap
immersed in a liquid oxygen (LOX) bath. After sealing the sample inlet end of
the U-tube, a leak test was performed by applying at least 10 inches of
Mercury vacuum to the system and checking the rotometers for flow indication.
If flow was noted, appropriate measures were taken to correct the leak.
B—17
-------
Figure B-7. Diagram of modified Smith-Greenburg midget impinger.
B-18
-------
316 Stainless steel
fmgtlok nut
Pyrex glass wool
&
A
ol
316 Stainless steel tube
V O.D. x .020" wall
1.00 to 1.05mri
Glass bead packing
Fi-
gure B-8. Cryogenic l)-tube construction.
B-19
-------
After completion of a successful leak check, the specially modified
midget impingers were connected and the actual sampling was begun. During the
sampling period, the flow through each sample was maintained at 100 cc/min by
adjusting the fine flow control valve mounted at the inlet of the rotometer.
Figure B-9 presents a photograph of the cryogenic U-tube sampling device in
sampling position (immersed in LOX bath).
The sample run was terminated when two or more sample U-tubes became so
restricted with frozen material it was no longer possible to maintain the
desired flow rate.
At the completion of sampling, the midget impinger and sample U-tubes
were removed from the CPA and sealed. The U-tubes were placed on dry ice and
maintained under dry ice conditions during their transport to the Mountain
View, California laboratory. The modified Smith-Greenburg midget impingers
were rinsed with methylene chloride in the field analytical laboratory. All
rinses were collected and stored in precleaned 50 ml Wheaton glass sample
vials with Teflon-lined septum caps. Rinses with methylene chloride prior to
the next sample run were retained as blank solvent samples for that run.
The second type of trap for sampling in conjunction with the CPA
utilized Tenax-GC microreticular adsorbent resin. The Tenax traps were
constructed from 1/4-inch O.D. 2-rrm bore pyrex tubing cut to 4-inch lengths.
Prior to packing with Tenax, the tubes were muffled at 400°C for 4 hrs. The
tubes were packed with Tenax GC, 80/100 mesh, using a small swatch of pyrex
glass wool (also muffled) in each end to hold the adsorbent in place. The
tubes were attached to the CPA with 316 stainless steel Swagelok nuts and
Teflon ferrules to ensure a leakfree seal. Figure B-10 presents a diagram of
the completed Tenax trap sampling device.
B-20
-------
Figure B-9. Photograph of cryogenic U-tube sampling device in sampling
position (immersed in LOX).
-------
Teflon ferrolf
316 stainless steel Swagelok nut
Pyrex glass wool insert
Pyrex glass capillary tube
Tenax GC adsorbent

i >ttd



4"
Figure B-10. Diagram of Tenax trap sampling devi
-------
Sampling with the Tenax traps was conducted in the same manner as
described for the cryogenic U-tube traps, except the Tenax traps were operated
at ambient temperatures. Also, the sampling duration was increased to
approximately 120 min since the Tenax traps are not prone to flow restrictions
caused by a buildup of frozen material. Figure B-ll presents a photograph of
the Tenax trap sampling device and Smith-Greenburg midget impinger in sampling
position.
The XAD-2 sampling device utilized XAD-2 adsorbent resin. The traps
were constructed from 5-inch lengths of 1/2-inch O.D. 316 stainless steel
tubing. Each end of the tubing was fitted with 1/2-inch to 1/4-inch Swagelok
reducing tube unions to connect the trap to the the CPA. Prior to packing the
tubes with XAD-2 resin, the entire unit was muffled at 400°C for 4 hrs. The
traps were then packed with XAD-2 resin, 80/100 mesh, using a small swatch of
pyrex glass wool (also muffled) inserted in each end to retain the packing.
Figure B-12 presents a diagram of the completed XAD-2 sampling device.
Sampling with the XAD-2 traps was conducted in the same manner as
described for the Tenax sampling devices. Figure B-13 presents a photograph
of the XAD-2 sampling device and modified Smith-Greenburg midget impinger in
sampling position.
B.3 ANALYTICAL METHODS AND RESULTS
Samples from the spray pond test site were received on November 25,
1980. The samples were assigned consecutive laboratory identification numbers
and stored at 4°C until analyzed.
Analyses were conducted for volatile and semivolatile organics.
Volatile organics analyses were based on variations to EPA Method 624.
B-24
-------
Figure B-11 - Photograph of Tenax trap sampling device and modified
Smith-Greenburg midget impinger in sampling position.
-------
316 stainless steel 1/2" O.D. x 0.035"
wall tubing
XAD-2 adsorbent
K-
5"
Figure B-12. Diagram of XAD-2 trap sampling device.
-------
Figure B-13. Photograph of XAD-2 sampling device and modified
Smith-Greenburg midget impinger in sampling position.
B- 29
k
-------
Semivolatile organics (phenols and polynuclear aromatics) analyses were based
on sample preparation variation to EPA Method 625 in conjunction with fused
silica capillary column GC/MS.
B.3.1 Analysis of Volatile Organics
The analytes of interest were benzene, toluene, and ethylbenzene. The
sludge wastewater and Tenax trap samples were analyzed for these components.
SIudge
A l.Og aliquot of the mixed sludge was weighed into a 15-ml crimp top
vial. Pentane (9 ml) and l-brom-2-chlorpropane (10 yg) were added as internal
standards. A 1-ul aliquot of this diluted sample was injected in a
0.2-percent Carbowax 1500 on a Carbopack C packed GC column in a Finnegan 1020
GC/MS instrument. Analysis and quantitation were conducted per EPA Method 624
using the internal standard method.
Quality control for the volatiles analysis entailed the analysis of a
method blank and a method standard spiked at 10 yg/g of sludge.
Water Samples
Water samples were analyzed for volatile organics using EPA Method 624
and 1- to 5-ml samples. The surrogate compounds dg-benzene and dg-toluene
were added to each sample.
Tenax Traps
Traps were prepared from Tenax GC (Applied Science) in 1/4 x 4 inch
glass tubes. Prior to sampling, every trap was spiked with d^-benzene
(100 ng) to assure recovery of the trapped samples.
The exposed Tenax trap contents were transferred to the laboratory in
the 12 x 1/8 inch stainless steel tubes used in the Tekmar LSC2 purge and trap
B-31
-------
device. The reassembled traps were purged with helium to remove air and then
thermally desorbed for analysis per EPA Method 624.
B.3.2 Analysis of Semivolatile Organics
Semivolatile organics analyzed are listed in table B-3. These analyses
were conducted by variations to EPA Method 625 in the sample preparation and
use of fused silica capillary column GC/MS to determine these compounds.
Sample Preparation
Sludge
The following procedure was used to prepare sludge samples:
1.	Place 10.Og of the sludge in a clean 250-ml brown bottle. Add
10.Og of anhydrous sodium sulfate and 100 ml of pesticide grade
dichloromethane. Shake occasionally and allow to sit overnight at
room temperature.
2.	Take 1.0 ml of each extract for GC/FID screening. Store the
remaining extract at 4°C.
3.	As required by the GC/FID screening, filter the extract into a
Kuderna-Danish concentrator and concentrate to 1.0 ml.
The GC/FID screening stage was necessary due to the wide variability of
sample concentrations. Figure B-14 summarizes the semivolatile extraction
scheme for sludge samples.
XAD-2 Cartridges
The XAD-2 cartridge was carefully opened, any silicone stopcock grease
removed with a CH^C^ wetted towel, and the contents transferred to a
preextracted Soxhlet thimble. The XAD-2 material in the Soxhlet was spiked
with surrogate mix and extracted overnight with CH^ C^. The extract was
B-32
-------
TABLE B-3. SEMIVOLATILE ORGANICS ANALYZED IN WOOD PRESERVING SAMPLES
Compound
Name
1
Phenol
2
2-Nitrophenol
3
2,4, Dichlorophehol
4
2,4,6 Trichlorophenol
5
4-Ni trophenol
6
4,6-Dinitro-0-cresol
7
Pentachlorophenol
8
Acenaphthene
9
Fluoranthene
10
Naphthalene
11
1,2-Benz(a)anthracene
12
Chrysene
13
Acenaphthylene
14
Phenanthrene
15
F1uorene
16
Pyrene
17
Benzof1uoranthenes
18
Benzo(a)pyrene
B-33
-------
Figure B-14. Proposed analysis scheme for phenols/PAH's in
wood preserving sludges.
B-34
-------
concentrated to 1 to 100 ml based on the amount of extractable material
present.
Quality control for XAD-2 samples consisted of the analysis of
surrogate spikes, field blanks, and spiked method blanks.
Impinger Catches
Midget impinger catches were composited for analysis in the
laboratory. Each composite water sample was extracted per EPA Method 625.
The extracts were concentrated to 0.5 ml for analysis.
U-Tubes
U-tubes were rinsed into a 0.40-ml vial with dechloromethane.
Anhydrous sodium sulfate was added to each vial and the vials shaken. The
extract was concentrated to 0.5 ml for analysis.
Soils
Soil samples were extracted as follows:
1.	Weigh a 50g aliquot into a 250-ml centrifuge bottle. Add surrogate
standards.
2.	Adjust the pH of the sample to 12.0 with 6N NaOH
3.	Add approximately 30 ml of water and homogenize for a few seconds.
Add 60 ml of methylene chloride, homogenize briefly again, withdraw
the homogenizer, and rinse it into the sample with water then with
5 to 10 ml of methylene chloride.
4.	Centrifuge the sample aliquot at 1,400 rpm for 5 min to reduce
formation of an emulsion layer at the water/methylene chloride
interface. Withdraw the extract using a 25-ml Mohr pipet.
5.	Perform an additional two extractions by adding 60 ml methylene
chloride, homogenizing, and centrifuging as indicated above
B-35
-------
6.	Acidify the sample to a pH less than 2 using 6N HC1. Add the acid
drop-by-drop with constant mixing to prevent foaming.
7.	Extract the sample again as described in sections 1.3 to 1.6,
keeping the addition of water to a minimum
8.	Combine and dry the extracts by passing through a drying column
packed with 10 cm of anhydrous Na2S0^. Concentrate to a final
volume of 1 ml using a K. D. apparatus equipped with a calibrated
receiver.
Extract Analysis
Each of the extracts obtained as described in the previous section was
analyzed for the compounds listed in table B-4 using fused silica capillary
column GC/MS. The instrument operating conditions are listed in table B-4.
The quality control requirements listed in EPA Method 625 were
followed, including analytical calibration, mass spectrometer tuning to meet
decafluorotriphenylphosphine (DFTPP) criteria, and the use of the multiple
internal standard quantitation method. The internal standards used were
dg-naphthalene, d^Q-anthracene, and d^-chrysene.
B.3.3 Analytical Results and Discussion
The qualitative results from the spray pond test program are shown
below. The sample log which corresponds to this discussion is presented in
table B-5.
U-tubes
Samples A8, A10, A12, A16, A18, A20, A22, A24, and A7 were analyzed for
volatiles. Sample A20 contained benzene at 12 ng, toluene at 19 ng, and
ethylbenzene at 9 ng. All the others were not detected or less than 5 ng was
collected.
B- 36
-------
TABLE B-4. FUSED SILICA CAPILLARY COLUMN PARAMETERS
Column:
30m x 0.25m SE-54 WCOT (J & W Scientific)
Split!ess Injection Parameters:
Injection mode:	Splitless
Sweep initiation:	30 sec
Sweep flow:	+12 ml/min
Column flow (He)
measured at
atmospheric:	1.0 ml/min
Interface:
Temperature:	300°C
Column directly coupled	to source (no transfer lines)
Temperature Program:
Initial:	30°C for 2 min
Program:	Ramp to 300°C at 10°C/min
Hold:	300°C, 15 min
Mass Spectral Parameters:
Ionization mode/energy:	Electron impact /70 eV
Total scan time:	1.0 sec
Mass range:	35 to 475 AMU
B-37
-------
TABLE B-5. SAMPLE LOG
Sample No.
1
Impinger No.
2
Impinger No.
3
Impinger No.
4
Impinger No.
5
Impinger No.
6
Impinger No.
7
Mell blank
1A

2A

3A
L0X test No.
4A

5A

6A

7A
Blank U-tube
8
Impinger No.
9
Impinger No.
10
Impinger No.
11
Impinger No.
12
Impinger No.
13
Impinger No.
B-l

B-2
XAD-2 cartri
B-3

C-l

C-2
Tenax Trap,
C-3

C-4
(Bottom)
C-5

C-6
Tenax Trap,
1A
2A
3A
4A
5A
6A
1, 1335 to 1358, 11-18-80
1A (XAD-2 B-l)
2A (Tenax C-l)
3A (XAD-2 B-2)
4A (Tenax C-2)
5A (XAD-2 B-3)
6A (Tenax C-3)
dge, Run No. 1, 11-18-80
1502 to 1717
Run No. 1, 11-18-80
Run No. 3, 11-19-80
B-38
-------
TABLE B-5. Continued
Sample No.
C-7
C-8
C-9
(Top)

14
Impinger rinse 1A

15
Impinger rinse 2A

16
Impinger rinse 3A
Impinger contents, test
17
Impinger rinse 4A
11-19-80 (Tenax)
18
Impinger rinse 5A

19
Impinger rinse 6A

20
Mell blank
11-19-80
21
Impinger rinse 2B

22
Impinger rinse 2B

23
Impinger rinse 3B
Impinger contents, test
24
Impinger rinse 4B
11-19-80 (Tenax)
25
Impinger rinse 5B

26
Impinger rinse 6B

A8
U-tube (Bottom)

A9
U-tube

A10
U-tube
Test No. 4, 11-19-80
All
U-tube
1147 to 1317
A12
U-tube

A13
U-tube (Top)

A14
U-tube (Bottom)

A15
U-tube

A16
U-tube
Test No. 5, 11-19-80
A17
U-tube
1425 to 1508
A18
U-tube

A19
U-tube (Top)

27
Impinger rinse IB
(Bottom)
B- 39
-------
le
28
29
30
31
32
33
34
35
36
37
38
B4
B5
B6
B7
B8
B9
39
40
41
42
43
44
45
TABLE B-5. Continued
Impinger rinse
2B


Impinger rinse
3B

Impinger contents, test
Impinger rinse
4B

11-19-80
Impinger rinse
5B


Impinger rinse
6B
(Top)

Impinger rinse
IB (Bottom)

Impinger rinse
2B


Impinger rinse
3B

Impinger contents, test
Impinger rinse
4B

11-19-80
Impinger rinse
5B


Impinger rinse
6B
(Top)

XAD-2 (Bottom)



XAD-2



XAD-2


Test No. 6, 11-19-80
XAD-2


1536 to 1645
XAD-2



XAD-2 (Top)



Impinger rinse
IB


Impinger rinse
2B


Impinger rinse
3B

Impinger contents, test
Impinger rinse
4B


Impinger rinse
5B


Impinger rinse
6B


No sample



XAD-2 (Bottom)



XAD-2



XAD-2


Test No. 8, 11-20-80
XAD-2


0811 to 1111
XAD-2



B-40
-------
TABLE B-5. Continued
Sample No.



45
Impinger rinse B1


46
Impinger rinse B2


47
Impinger rinse B3
Test
No. 8, 11-20-80
48
Impinger rinse B4


49
Impinger rinse B5


50
Impinger rinse B6


B16
XAD-2 (Top)


B17
XAD-2 (Bottom)


B18
XAD-2


B19
XAD-2
Test
No. 9, 11-20-80
B20
XAD-2
1037
to 1237
B21
XAD-2


B22
XAD-2 (Top)


51
Impinger rinse IB


52
Impinger rinse 2B


53
Impinger rinse 3B
Test
No. 9, 11-20-80
54
Impinger rinse 4B


55
Impinger rinse 5B


56
Impinger rinse 6B


CIO
Tenax Trap (Bottom)


Cll
Tenax Trap


C12
Tenax Trap
Test
No. 10, 11-20-80
C13
Tenax Trap
1319
to 1521
C14
Tenax Trap


C15
Tenax Trap (Top)


57
Impinger rinse (Bottom)


58
Impinger rinse


59
Impinger rinse
Test
No. 10, 11-20-80
60
Impinger rinse


61
Impinger rinse


B-41
-------
TABLE B-5. Continued
Sample No.
62	Impinger rinse (Top)
63	Impinger rinse (Bottom)
64	Impinger rinse
65	Impinger rinse	Test No_ u> n.20.80
66	Impinger rinse
67	Impinger rinse
68	Impinger rinse (Top)
C16	Tenax Trap (Bottom)
C17	Tenax Trap
C18	Tenax Trap	Test No. 11, 11-20-80
C19	Tenax Trap	1544 to 1744
C20	Tenax Trap
C21	Tenax Trap (Top)
C22	Tenax blank
C23	Tenax blank
B26	XAD-2 blank
B29	XAD-2 blank
Sample Log — Wastewater and Sludge
100	Pond sludge 11-2-80 (0830)
101	Pond sludge 11-2-80 (0830)
102	Pond sludge 11-2-80 (0830)
103	Pond wastewater (pump discharge) 11-2-80 (0830)
104	Pond wastewater (pump discharge) 11-2-80 (0830)
105	Pond wastewater (pump discharge) 11-2-80 (0830)
106	Sludge spray pond 11-19-80 (1215)
107	Pond grab sample (surface) 11-19-80 (1015)
108	Pond wastewater (pump discharge) 11-19-80 (1045)
109	Pond sludge (5 ft from edge) 11-19-80 (1215)
B-42
-------
mple I
110
111
112
x 113
x 114
x 115
116
117
118
119
120
121
x 122
x 123
TABLE B-5. Concluded
Farmers pond (bottom core sample) 11-19-80 (1000)
Farmers pond (behind RR tracks) 11-19-80 (0145)
Farmers field (3-part core soil sample) 11-19-80 (1050)
Farmers pond V0A
Pond V0A (pump discharge) 11-19-80 (1045)
Pond V0A (surface water) 11-20-80 (0820)
Flor tank sludge to drying bed — CZ 1-19-80
Aeration tank after flor tank -- CZ 1-19-80
Condenser pond 	flock tank -- CZ 1-19-80
Condenser pond VOA
Aeration tank VOA
Sludge VOA
Wastewater from separator 11-20-80 (0930)
Wastewater before pond 11-20-80 (0910)
B-43
-------
Samples A9, All, A13, A17, A19, Al, A6, A21, A23, and A25 were analyzed
for phenols and polynuclear aromatics. All results except the following were
negative. The detection limit was 1 ug collected for all samples.
Sample	A9	Al 1	Al
Pentachlorophenol	41	5.2	4.0
Fluoranthene	1.4	1	1
Pyrene	1.1	1	1
Phenanthrene	1.7	1	1
Figure B-15 is a reprensentative chromatogram from a U-tube extract.
XAD Cartridges
Samples Bl, B2, B3, B5, B7, B9, Bll, B14, B16, B18, B20, B22, B26, and
B29 were extracted and analyzed for phenols and polynuclear aromatics. No
compounds were detected to a detection limit of 1 yg. The detection limit for
naphthalene in these samples is 10 yg due to a minor contamination of the
XAD-2. Figures B-16 and B-17 compare the chromatograms from an XAD-2 blank
and a sample.
Tenax Traps
All Tenax traps CI through C23 were analyzed for benzene, toluene, and
ethyl benzene. These compounds were not detected in any samples. Due to a low
level of Tenax contamination, the detection limits were O.t ug for each of
these compounds.
Waters, Sludges, and Soils
These samples were analyzed for volatile aromatics, phenols, and
polynuclear aromatics as listed in tables B-6 and B-7. Figure B-18 is a
typical chromatogram for a volatiles analysis. Figure B-19 is a chromatogram
from a pond sludge extract.
B-44
-------
TABLE B-6.
WOOD PRESERVING TEST RESULTS
TEST SITE:
TEST Spray Pond Samples
TEST DATE
COMPOUND Acurex I.D. #
A80-11-043
100-102+lpo
103-105
107 [
-87 I
5P Pond bla+dv*
108
Description
B»nfAtVSPSKArlAl r
Composite slu
ge Comp.Wa
-88
renwcn luropneno 1
Ib.OOO
15
2.2 ]
H>na At Pum
16
Phenol
<50
<0.1
<0.1 I
<0.1
Fluoranthene
5800
3.0
5.7 1
2.7
Naphthalene
1500
4.0
6.3 1
2.3
Benzo(a)anthracene
Benzo(a)pyrene
2600
20
0.4
<0.1
1.4 I
o.i 1
4.5
<0.1
Benzof1uoranthenes
87
0.1
0.5 I
0.1
Chrysene
2000
0.6
1.6 J
6.2
Acenaphthylene
230
0.1
0.3 I
0.1
Anthracene
1700
0.7
1.6 I
0.7
Benzo(gh1)perylene
67
<0.1
<0.1 I
<0.1
Fluorene
5600
1.7
3.7 J
2.0
Phenanthrene
9000
6.4
12 j
7.4
D1benzo(a,H)anthracene
<50
<0.1
<0.1 1
<0.1
Indeno(1,2p3-cd)pyrene
85
<0.1
<0.1 1
<0.1
Pyrene
4400
1.6
2.9 1
1.1
Benzene
NA
NA
NA |
NA
Toluene
NA
NA
NA 1
NA
Ethylbenzene
NA
NA
NA 1
NA
All concentrations In units of micrograms per gram except for XAD collections
which are total milligrams collected.
B-45
-------
WOOD PRESERVING TEST RESULTS
TEST SITE:A1gbam2r
p-jgld I.D.
COMPOUND Acurex I.O. #
	A80-11-043

Phenol
Fluoranthene
Naphthalene
Benzo(a)anthracene
Benzo(a)pyrene
Benzof1uoranthenes
Chrysene
Acenaphthylene
Anthracene
Benzo(ghi)perylene
Fluorene
Phenanthrene
Indeno(l,2,3-cd)pyrene
Pyrene
Benzene
Toluene
Ethylbenzene
TABLE B-7.
TEST
Spray Pond
TEST DATE
JL2Z.

114
-97
-98
-100
Wastewater
750
17
41
66
<10
<10
<10
<10
<10
<10
<10
58
24
D1benzo(a,h)anthracene
<10
<10
21
NA
NA
NA
I Wastewater lSpray PomT
1160	fto
48
23
120
<10
<10
<10
<10
<10
17
<10
22
67
<10
<10
15
NA
NA
NA
0.015
<0.005
<0.005
115
-101
Pond Pump
NA
0.015
0.040
<0.005
All concentrations 1n units of micrograms per gram except for XAD
which are total milligrams collected.
collections
B-46
-------
RIC	DATA: BNA4314 il	SCANS 100 TO 2200
01/06/81 15:10:00	CALI: C010381B il
SAMPLE: A80-11-043-H A-2 IU=TOTAL FU=.5 1UL=20NG D8,10,12
RANGE: G J,2200 LABEL: N 0, 4.0 QUAN: A 0, 1.0 BASE: U 20, 3
100.01	1862970.
00
1
-Pi
--j
RIC

I	
500
8:20
4-
1
yl
AjUW.Uk.
—[	i	r——I—
1000
16:40
1500
25:00
2000
33:20
SCAN
TIME
Figure B-15. Total ion current chromatogram U-tube extract.
-------
RIC
01/10/81 15:29:06
SAMPLE: A8G-11-043-34 B9 1UL=20NG 08,10,12
RANGE: G 1.2200 LABEL: N 0, 4.0 QUAN: A
DATA:
CALI:
BNA4334 «1
C0110818 12
SCANS 100 TO 2200
0/ 1.0 BASE: U 20, 3
100.0-1
2015230.
RIC
oo
CD
-W±L L
1
A -. -^i - ^ f
I860
16:40
1500
25:u0
2000
35:2€"
SC UN
TH1F
Figure B-16. Chrcmatogram from XAD-2 sample.
-------
RIC	DATA: BNA4347B #1	SCANS 106 TO 2200
01/12/81 17153:00	CALI: C611281A #3
SAMPLE: A80-11-043-47 B26 BLANK 1UL=20NG 08,10,12
RANGE: G 1,2200 LABEL: N 0,	4.0 QUAN: A 0, 1.0 BASE: U 20, 3
875520.

Ldt
I i

500
ft: 2d
1000
16:40
y i
-i	¦	1	r-
2000
33:20
SCAN
TIME
Figure B-17. Chromatogram from an XAD-2 blank.
B-49
-------
PIC
12	li:21:06
SAMPLE I PONB Wjh N0115 lHL»130i». •j'JPP.is
ftMGE: C 1. 680 Lh6£Li H a, 4.0 WhN: m 9.
31? 3h3
161
Benzene
dg-Benzene
206 ,
AJL
256
AJV
237
JL
0«Trt: MHO115 (1
CHLI: FC43 «i
.e bhses ij ;y
<53
SChNS 58 To 6
-------
100.8-1
01/14/81 12:28:00	SJJl	J[146
SAMPLE: A08-11-843-88 0UPL,0F=18 1UL=28NG 08,18,12 """"H «
RANGE: G 1,2280 LABEL: N 8, 4.8 QUAN: A 8, 1.8 BASE: U 28, 3
SCANS 188 TO 2288
RIC

50?
8:20
1888
16:48


	1	r
1588
25:80
2880
33:20
1589248
SCAN
TIME
Figure B-19. Total ion current trace of pond sludge extract.
B- 51
-------
The composite pond water sample (Field I.D. 103+104+105 and Lab I.D.
80-11-043-83) was also analyzed for oil and grease by standard methods. The
measured value was 160 mg/1.
Impinger Catches
Impinger catch samples were composited as follows:
o Sample 1 - Sample 6
o Sample 7 + Sample 20
o Sample 8 - Sample 13
o Sample 14 - Sample 19
o Sample 21 - Sample 26
Each of these composite samples was concentrated and analyzed for phenols and
semi volatiles. No compounds were detected to a detection limit of 1 yg.
Figure B-20 is a chromatogram of a typical impinger extract.
B-52
-------
RIC	DATA: BNA3125 *1136
01/13/81 15t58:00	CALI: C0U381A «3
SAMPLE! A80-11-043-125 COMP	ANAL PROCI FU=0.5ML 1UL=20NG [18,10,12
RANGE: G 1,2200 LABEL: N 0, 4.0 QUAN: A 0, 1.0 BASE: U 20, 3
SCANS 100 TO 2200
76672.
JljJ
JJ

1000
16:40
1500
25:00
2000
33:28
SCAN
TIME
Figure B-20. Typical chromatogram of an impiriger extract.
B-53
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SECTION B-2
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ggatheson
FLOWMETER CALIBRATION- Scale Reading vs.
Flow Rate
AIR
tube WO. 602
SER. HO. TYPICAL
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M602-IA
-------
CONVERSION TABLE - SENSITIVE ANEMOMETER
(For Cup Assemblies with Serial Nos. above 92)
34.48
59.98
85.47
June 1959
Counts per Minute to	Centimeters per	Second	After N.B.S. Calibration
Counts 0	1	2	3	4	5	6	7	8	9
0	-11.5«	14.09	16.64	19.19	21.74	24.29	26.83	29 38	31 93
10	37.03	39.58	42.13	44.68	47.23	49.78	52.33	54.88	57*43
20	62.53	65.07	67.62	70.17	72.72	75.27	77.82	80.37	82.*92
30	88.02	90.56	93.11	95.66	98.21	100.76	103.30	105.85	108*40	110*95
AO	113.50	116.05	118.60	121.15	123.70	126.25	128.80	131.35	133 90	136*45
50	138.99	141.54	144.09	146.64	149.19	151.74	154.29	156.84	159.39	16l!94
60	166.59	166.98	169.49	171.98	174.49	176.99	179.49	181.99	184 49	186 99
70	189.49	192.00	194.49	197.00	199.49	202.00	204.50	207.00	209*50	212*01
80	214.50	217.00	219.51	222.00	224.51	227.00	229.51	232.01	234 51	237*01
90	239.52	242.01	244.52	247.01	249.51	252.02	254.51	257.02	259.52	262!o2
100	264.52	267.03	269.52	272.03	274.52	277.03	279.53	282.02	284 53	287 03
110	289.53	292.03	294.53	297.03	299.54	302.03	304.54	307.04	309 54	312 04
120	314.53	317.02	319.54	322.04	324.54	327.05	329.54	332.05	334.55	337 05
130	339.55	342.00	344.45	346.91	349.36	351.81	354.27	356.72	359.17	361 62
140	364.08	366.53	368.98	371.44	373.89	376.34	378.79	381.25	383.70	386 15
150	388.61	391.06	393.51	395.97	398.42	400.87	403.32	405.78	408.23	410.68
160	413.14	415.59	418.04	420.49	422.95	425.40	427.85	430.31	432 76	435 21
170	437.67	440.12	442.57	445.02	447.48	449.93	452.38	454.84	457 29	459 74
180	462.19	464.65	467.10	469.55	472.01	474.46	476.91	479.37	481.82	484 27
19 0	4 86.72	4 89.18	491.63	494.08	496.54	498.99	501.43	503.88	506.34	508.79
200	511.24	513.65	516.05	518.46	520.87	523.27	525.68	528.08	530.49	532.89
210	535.30	537.70	540.11	542.51	544.92	547.32	549.73	552.12	554.53	556.93
220	559.34	561.74	564.15	566.55	568.96	571.36	573.77	576.18	578.58	580.99
230	583.39	585.80	588.20	590.61	593.01	595.42	597.82	600.23	602.62	605.03
240	607.43	609.84	612.24	614.65	617.05	619.46	621.86	624.27	626.67	629.08
250	631.48	633.89	636.30	638.70	641.11	643.51	645.92	648.32	650.73	653.13
260	655.54	657.93	660.34	662.74	665.15	667.55	669.96	672.36	674.77	677.17
270	679.58	681.98	684.39	686.79	689.20	691.60	694.01	696.42	698 82	701.23
280	703.63	706.04	708.43	710.84	713.24	715.65	718.05	720.46	722.86	725.27
290	727.67	730.08	732.48	734.89	737.29	739.70	742.10	744.51	746.91	749.32
B-69
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APPENDIX C
CHARACTERIZATION OF EMISSIONS FROM THE DISPOSAL
OF WOOD PRESERVING WASTES IN AN INDUSTRIAL BOILER
CONTENTS
C_1 Program Description and Results
C-2 Raw Data: Preliminary and Isokinetic Source Emission Sampling
C-3 Raw Data: Total Hydrocarbon Determination
C-4 Raw Data: Specific Low-Molecular-Weight Hydrocarbon Determination
C-l
-------
SECTION C-l
PROGRAM DESCRIPTION AND RESULTS
The Resource Conservation and Recovery Act (RCRA) is expected to cause
generators of hazardous wastes to dispose of their wastes within plant
boundaries. One disposal option is the thermal destruction of the waste in a
steam boiler. This field test program was conducted at a wood preserving
facility using a 40,000 lb/hr pile-burning watertube boiler cofiring a mixture
of wood waste and penta/creosote wastewater. The program was designed to
determine the destruction and removal efficiency of the organic compounds
contained in the wastewater. Input materials (including the wood waste and
sludge) and output materials (including mechanical collector ash, baghouse
hopper ash, and bottom ash) were analyzed, and pertinent data for a material
balance evaluation were collected. All samples were qualitatively and
semiquantitatively analyzed for organic compounds, including chlorinated
phenols, chlorinated dibenzo-p-dioxins, chlorinated dibenzofurans, and
polynuclear aromatic hydrocarbons (PAH's) contained in each stream.
This program focused on the gaseous emissions discharged from the stack
and the ash streams which result during combustion and pollution control.
Making balance estimates was difficult since ash and fuel flowrates were not
metered by the operator. Estimates were made of each stream and of the
appropriate material balance evaluation of the destruction and removal
efficiency performed (see section 7).
C-3
-------
C.l TEST SITE
The wood treating facility selected for field sampling employs six
retorts using the steaming process to treat a variety of domestic and imported
wood products. The treating process can treat wood with penta, creosote, or
waterborne preservative formulations. Table C-l presents a summary of the
total production during the field test period.
TABLE C-l. SUMMARY OF TREATING PRODUCTION MATRIX FOR THE PERIOD
JULY 21 THROUGH JULY 25, 1980
Product	Penta	Penta	Fire
treated (ft3) (heavy oil) (light oil) Creosote CCA* retardant**
Utility	poles 7,962	—	2,712	37
Pilings	1,088	—	7,044	400	—
Lumber	440	1,860	1,753	6,583	1,717
Plywood	—	—	—	—	962
*CAA = copper chromate arsenate (waterborne)
**Waterborne formulation
Wastewater and byproducts generated as a result of the individual
treating processes are handled by discrete oil/water separators. The
recovered preservative fractions are returned to bulk storage tanks for reuse
in the process. Separated sludges and wastewater are routed to a storage
tank; eventually, when quantity is sufficient to ensure economic handling of
the waste, they are sent to the steam boiler for disposal. Figure C-l
presents a schematic of the plant wastewater/preservative recovery system.
Estimates of 5,000 to 8,000 gal/day of wastewater generation during normal
treating operations were made.
C-4
-------
-10,000 gallon ea.
settling tanks
Creosote
storage
tank
7.00C
gal.
To
boiler"
Boiler
make-up
water
Waterborne|__
and washdown
(Recovered creosote)
5-zone gravity
separator and
steam coil
heating
Sludge
tank (Sludge/waste)
(polish)
Sludge/waste
/vr v

PCP

storage

tank t
Sludge/waste
Storage
tank
Wastewater
Corregated plate
separator
PCP
./ v.
Water-
borne
Holding
tank
>15,000
gallons
Figure C-l. Schematic of plant wastewater/preservative recovery system.
C-5
-------
The boiler, manufactured by Wei Ions Company, was designed to produce
40,000 Ib/hr of steam used for space heat, the treating cycle, and other plant
process operations. The boiler unit which consists of both a cell and a
furnace can be fired using both cell and furnace or separately depending on
plant process demand.
The boiler fuel supply system consists of transfer and metering
conveyors, wet and dry fuel silos, two metering bins for cell and furnace, and
a constant running screw conveyor to charge the fuel to the cell and furnace
for burning. Both constant-feed screw conveyors have been modified to allow
the mixing of hog fuel with sludge and/or wastewater from the treating plant.
The furnace also is equipped with a ram charging device for loading
irregular-shaped and oversized wood scrap into the boiler.
The unit is equipped with a multicone and two baghouses to reduce
particulate emissions from the boiler. Figure C-2 presents a schematic of the
boiler plant. Figure C-3 presents a photograph of the boiler plant. The
plant estimates that it burns 20 unitsday of hog fuel during normal
operation. (One unit.« 200 ft^ = 200 lbs dry Douglas Fir = 4,000 lbs
Douglas Fir at 50 percent moisture - 16 MBtu at 50 percent moisture.)
C.2 FIELD TEST PROGRAM
The sampling program included each of the tests described as follows:
•	Determination of preliminary flue gas stream characteristics
•	Isokinetic source sampling of boiler flue gas
•	Total hydrocarbon determination of boiler flue gas
•	Specific low-molecular-weight hydrocarbon determination of flue gas
using gas chromatography (GC)
C-6
-------
Fuel oil tanks
Sludge tank
.Bunker Incline conveyor
Wet
fuel
o

Wastewater
tanks
Feedwater
pump
' "s	Metering
Furnace convey°r
convevor
5r
Dropout
box
Cell
(below)
Boiler
furnace
(below)
Forced air
ducting
Ram
charger
Deaerator
feed water pumpI
.Multlcone
mechanical
collector
Deaerator tank
Heat
Exchanger
I.D. fans
Baghouse
no. 2
Baghouse
no. 1
Pit conveyor
Figure C-2. Schematic of boiler plant.
C-7
-------
•	Composite sampling of:
—	Boiler bottom ash
—	Multicone hopper ash
—	Wood waste fuel
—	Sludge/wastewater fuel
•	Grab sampling of:
—	Baghouse hopper ash
—	Bulk penta in aromatic treating oil
—	Bulk creosote
The sample collection matrix is shown in table C-2. The following subsections
describe the equipment and techniques employed during sampling.
C.2.1 Preliminary Measurements
Preliminary gas characteristics were determined using EPA Methods 1
through 4 (Federal Register, Volume 42, No. 160, August 18, 1977). Using
these criteria, the required number of sampling points was established. W1th
the boiler operating under normal load conditions, two traverses were
conducted at right angles to one another on the south stack (No. 2).
TABLE C-2. SAMPLE COLLECTION MATRIX
Sample
number
Air samples
Outlet stock

Solid Samples

Wood waste
and sludge
Boiler
bottom ash
Mech. hopper
ash
Baghouse
ash __
1
1-XAD, GC
1-compos1te
1-Grab
1-composite
1-grab
2
1-XAD, GC
1-composite
1-grab
1-composite
1-grab
3
1-XAD, GC
1-compos i te
1-grab
1-composite
1-grab
4
1-XAD,GC
1-compos -fte
1-grab
1-composite
1-grab
C-8
-------
Figure C-3. Boiler plant.
m"'. -
1
C-9
-------
Figure C-4 presents a schematic of the stack cross section and traverse point
locations. Gas velocity measurements were taken using a calibrated 6-ft
S-type pitot tube connected to a 0- to 1-inch Magnehelic Series 200 gauge
manufactured by Dwyer Instruments Company, Michigan City, Indiana. Exit gas
temperatures were measured using a.Chromel-Alumel (Type K) thermocouple and a
digital thermal indicator manufactured by Doric Incorporated. Table C-3
presents a summary of the velocity/temperature profile data.
Preliminary gas moisture content was calculated using psychrometric
data. Successive moisture values, as determined during the actual test runs,
then were used to update the preliminary calculated values. Exit gas
molecular weight was determined by standard orsat analysis before and after
each test run. The raw data collected in the field are presented in
section C-2 of this appendix.
C.2.2 Isokinetic Source Sampling of Boiler Flue Gas
Sampling of high-molecular-weight organic emissions from the outlet
stack was performed using the EPA Method 5 isokinetic sampling train as shown
in figure C-5. The train consists of an in-stack filter, a heated glass-lined
probe, an XAD-2 polymer sorbent trap, and impingers. The first impinger, a
modified Greenburg-Smith (without an impaction plate), was empty, followed by
~
an XAD-2 polymer sorbent trap and a Greenburg-Smith impinger charged with
100 ml of 30-percent hydrogen peroxide. The third impinger was also an empty
modified Greenburg-Smith, followed by a silicon dioxide drying trap to protect
the vacuum pump and sampling module from moisture. Figure C-6 presents a
photograph of the sampling train in sampling position on the south stack.
For each isokinetic source test, a sample was drawn from the fan outlet
(at a predetermined constant velocity point) through a probe fitted with the
appropriately sized nozzle. Four complete sets of samples were collected.
C-ll
-------
Sampling Locations
Traverse Point Number
South Port East Port
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
Location from Inside Stack Wall
3/4
2-7/6
4-3/16
6-3/4
10-1/4
19-3/4
23-3/16
25-5/8
27-1/2
29-3/16
North
Sampling
ports
5
N
30"
Figure C-4. Schematic of traverse point locations, south stack, no. 2.
C—12
-------
TABLE C-3. SUMMARY OF VELOCITY/TEMPERATURE PROFILE DATA FOR SOUTH STACK

South port

East port
Location
(inches aP H20)
Temperature
(inches aP H20)
Tempegature
1
0.39
248
0.56
290
2
0.51
268
0.43
290
3
0.55
286
0.54
319
4
0.59
325
0.60
346
5
0.61
335
0.65
357
6
0.65
345
0.71
355
7
0.64
347
0.74
359
8
0.64
351
0.75
362
9
0.60
353
0.74
363
10
0.53
355
0.68
364
C—13
-------
Heated Teflon sampling line
Figure C-5. Schematic diagram of an XAD-2 high-molecular-weight mass
particulate sampling train.
C-14
-------
Figure C-6. Modified EPA Method 5 sampling train in sampling position
on south stack.
C—15
-------
All sampling was conducted during normal boiler operation. Table C-4 presents
a summary of the pertinent isokinetic source test parameters. The raw field
data are presented in Section C-2 of this appendix.
At the completion of source sampling, the sample train and probes were
transported to a field laboratory. Samples were transferred from the sample
trains to specially cleaned and labeled storage containers. The probe nozzle,
probe, and connecting lines were cleaned also and recovered samples were
transferred to the appropriate storage containers. Immediately following
sample recovery, all samples were iced in the field and maintained under those
conditions during transport to the analytical laboratory.
C.2.3 Total' Hydrocarbon Determination of Boiler Flue Gas
A Model 400 total hydrocarbon analyzer (THC) manufactured by Beckman
Instruments of Fullerton, California, was used to continuously monitor total
hydrocarbons in the sampled gas stream at the south stack. This analyzer uses
the flame ionization detection (FID) method. The analyzer output was recorded
using a Model 585 strip chart recorder manufactured by Linear Instruments
Corporation, Irvine, California.
The FID was operated using zero grade 1.0 hydrogen fuel and zero air
supplied by Airco Industrial Gases, Santa Clara, California. Hydrogen fuel
and zero air pressure were set at 207 kPa (30 psi) and 104 kPa (15 psi),
respectively, using internal differential pressure regulators in the analyzer.
Sampling was conducted using the system shown in figure C-7. The gas
sample was extracted from the stack via a 7-micron, sintered, stainless steel
Model No. SS-4 FE-7 filter manufactured by Nupro Valve Company of Willoughby,
Ohio. The filter removed fine particulates which, if allowed to pass into the
THC analyzer, could occlude the FID sample inlet capillary. A 0.006m 0.0.
C—17
-------
TABLE C-4. SUMMARY OF ISOKINETIC SOURCE TEST PARAMETERS
Test
No.
Date
Test period
(24-hr clock)
Sample
time
(min)
Barometric
pressure
(inches Hg)
Sample
volume
(scf)
Average
stack gas
temp (OF)
Molecular
weight
(lb/lb mole dry)
Percent
moisture
Percent
isokinetic
1
7/22/80
1000-1600
360
30.57
12.79
318.9
29.29
12
98.0
2
7/23/80
0850-1450
360
30.00
17.34
331.1
29.28
7.2
100.4
3
7/24/80
0850-1450
360
30.69
25.81
342.0
29.43
5.0
100.0
4
7/25/80
0800-1350
350
30.75
30.643
367.4
29.37
7.9
105.3
-------
7pm sintered stainless steel filter
¦ 0.006 cc stainless steel orobe
— — — To stack
'Three-way stainless steel solenoid valve
Heat traced Teflon sample line (3C.48m)
Heat traced Teflon connecting line
Teflon diaphragm vacuum pump
Unburned
hydrocarbon
Strip
chart
recorder!

Calibration
gases

2 ml injection
loop and
backflush valve
Gas
chromatoqraph
(FID)
Strip
chart
recorder
est
8
T

Figure C-7. Schematic of unburned hydrocarbon and gas chromatograph
sampling system.
C-19
-------
stainless steel probe connected the filter unit to the heated sampling line
via a three-way stainless steel solenoid valve. This valve allowed the
introduction of sample gas or calibration gas depending on which mode of
operation was desired. A 12.2m, heat-traced, 0.01m 0.0. Teflon sample line
manufactured by Technical Heaters, Inc. of San Fernando, California, was used
to transport the sample to the vacuum pump. Sample line temperature
controllers were supplied by the manufacturer. A Teflon-coated diaphragm
vacuum pump manufactured by Thomas Industries of Sheboygan, Wisconsin, was
used to pull the sample through the lines. From the gas vacuum pump exit, the
sample was split and routed to the analyzers via short lengths of heated
Teflon line.
Prior to operation and calibration, the completed sampling system was
operated at approximately 297°K above normal sampling and calibration
conditions, and was purged for several hours with zero nitrogen to remove any
traces of residual hydrocarbon contamination in the lines. During this
"bake-out" procedure, stainless steel tube unions, filters, and probes were
heated using a propane torch. Before and after each test, a leak test was
performed on the sampling system, followed by calibration of the THC analyzer
using zero nitrogen (0.5) and a mixture of 535 ppm methane in nitrogen.
During calibration, the three-way valve was positioned to block the sample
probe and filter, allowing the calibration gas to pass into the heat-traced
sample line. Introducing the calibration gases at this location ensured the
sample gases and calibrations gases were treated in the same manner,
nullifying possible undesirable effects due to absorption or wall loss in the
sampling line and system.
The raw data from this test sequence are contained in section C-3 of
this appendix.
C-20
-------
C.2.4 Specific Low-Molecular-Weight Hydrocarbon Determination of Flue Gas
Periodical ly, benzene, toluene, and ethylbenzene concentrations were
determined in the boiler flue gas. Small portions of the sampled gas routed
to the total hydrocarbon monitoring system were diverted and injected into a
Varian Model 3700 gas chromatograph (GC)fitted with an FIO. Figure C-7
depicts the sampling system. Using a sample valve fitted with a 2-cm3
injection loop, the sample was injected into a 6-ft x 1/8-in O.D. stainless
steel column packed with 1 percent SP100 on Carbopack (80/100) mesh.
Calibration standards for the compounds of interest were prepared
onsite using a 50L Teflon bag and the methods outlined in "Evaluation of
Emission Test Methods for Halogenated Hydrocarbons," (Vol. I>
EPA-600/4-79-025, March 1979). Table C-5 presents the results of the analysis
and a chronology of sampling/injection time during the field testing period.
Resultant chromatographs indicate that the components of interest were
not detected at concentrations less than 0.1 ppm in the sampled gas. These
data are in close agreement with previously presented data for the total
hydrocarbon analysis. The raw data from these tests are contained in
section C-4 of this appendix.
C.2.5 Composite Sampling
Composite samples of the multicone hopper ash, boiler bottom ash,
woodwaste fuel, and sludge/wastewater were collected during the field sampling
period. Sampling at these locations was performed at approximate 1-hr
Intervals during each test run. Samples were obtained by collecting and
transferring equal bulk aliquots of the material into precleaned sample
storage containers. Figure C-8 shows of each sampling location.
C-21
-------
TABLE C-5. SUMMARY OF SPECIFIC LOW-MOLECULAR-WEIGHT HYDROCARBON
DETERMINATIONS OF FLUE GAS
Date
Time

Procedure
Results*
7-21-80
1623
Inject
calibration standards
—
7-22-80
1044
Inject
flue gas sample
<0.1 ppm

1055
Inject
flue gas sample
<0.1 ppm

1110
Inject
zero gas
	

1548
Inject
flue gas sample
	
7-23-80
0944
Inject
flue gas sample
<0.01 ppm

1100
Inject
flue gas sample
<0.01 ppm

1304
Inject
flue gas sample
<0.01 ppm

1319
Inject
flue gas sample
<0.01 ppm

1336
Inject
calibration standards
	

1342
Inject
flue gas sample
<0.01 ppm

1349
Inject
flue gas sample
<0.01 ppm

1426
Inject
flue gas sample
<0.01 ppm

1507
Inject
flue gas sample
<0.01 ppm
7-24-80
1040
Inject
calibration standard
. T-

1113
Inject
calibration standard
	

1130
Inject
calibration standard
	

1240
Inject
flue gas sample
<0.1 ppm

1215
Inject
zero gas
	

1400
Inject
calibration standard
	

1415
Inject
calibration standard
„

1430
Inject
calibration standard


1449
Inject
flue gas sample
<0.01 ppm
7-25-80
0828
Inject
calibration standard


0845
Inject
calibration standard
	

0913
Inject
flue gas sample
<0.01 ppm

0940
Inject
zero gas
	

1000
Inject
flue gas sample
<0.01 ppm

1015
Inject
C]-Cg calibration standard
——

1125
Inject
Ci-Cg calibration standard


1201
Inject
flue gas sample
<0.01 ppm

1206
Inject
flue gas sample
<0.01 ppm
~Concentration of sought components
C-22
-------
Fuel oil tanks
Sludge tank
Bunkeir incline conveyor
Wet
fuel
ic
'	Meteri no
Wastewater
tanks
Feedwater
pump
' "s	Metering
Furnace conveV°r
convevor
Dropout
box
Fuel sample
Cel
(below)
Boiler
furnace
(below)
Forced air
ducting
Boiler bottom
ash sample
charger
Deaerator
feed water pumpI
.Multicone
mechanical
-j collector
Deaerator tank
Heat
Exchanger
Outlet
itaci'
Method 5
test
I.D. fans
Baghouse
hopper ash sample
Baghouse
no. 2
Baghouse
no. 1
Multiclone ash
sample
Pit conveyor
Figure C-8. Composite and grab sampling locations.
C-23
-------
C.2.6 Grab Sampling
Grab samples of the baghouse hopper ash, bulk penta in heavy aromatic
testing oil, and bulk creosote were collected during the field sampling.
Baghouse No. 2 hopper ash samples were collected at the end of each test run
when the hoppers were emptied. Grab samples of the penta and creosote
treating formulations were supplied by plant personnel.
C.3 ANALYTICAL METHODS AND RESULTS
Samples from the boiler test site were received on July 29, 1980. The
samples were assigned consective laboratory identification numbers and stored
at 4°C until analyzed.
C.3.1 Analytical Methods
Analyses were conducted for volatile organics, semi volatile organics
and metals. Volatile organics analyses were based on variations to EPA
Method 624. Semivolatile organics (phenols and polynuclear aromatics)
analyses were based on sample preparation variations to EPA Method 625 in
conjunction with fused silica capillary column GC/MS. Metals analyses were
conducted using standard atomic absorption techniques.
Analysis of Volatile Organics
The analytes of interest were benzene, toluene, and ethylbenzene. Only
the sludge samples were analyzed for these components.
A l.Og aliquot of the mixed sludge was weighed into a 15-ml crimp top
vial. Pentane (9 ml) and l-bromo-2-chloropropane (10 vg) were added as
internal standards. A 1-yl aliquot of this deluted sample was injected in a
0.2-percent Carbowax 1500 on a Carbopack C packed gas GC in a Finnegan 1020
GC/MS instrument. Analysis and quantitation were conducted per EPA Method 624
using the internal standard method.
C-24
-------
Quality control for the volatiles analysis entailed the analyses of a
method blank and a method standard spiked at 10 yg/g of sludge.
Analysis of Semivolatile Organics
Semi volatile organics analyzed are listed in table C-6. These analyses
were conducted by variations to EPA Method 625 in the sample preparation and
the use of fused silicon capillary column GC/MS to determine these compounds.
Sample Preparation
The sludge samples were prepared as follows:
1.	Place 10.Og of the sludge in a clean 250-ml brown bottle. Add
10.Og of anhydrous sodium sulfate and 100 ml of pesticide grade
dichloromethane. Shake occassionally and allow to sit
overnight at room temperature.
2.	Take 1.0 ml of each extract for GC/FID screening. Store the
remaining extract at 4°C.
3.	As required by the GC/FID screening, filter the extract into a
Kuderna-Danish concentrator and concentrate to 1.0 ml.
The GC/FID screening stage was necessary due to the wide variability of
sample concentrations. Figure C-9 summarizes the semivolatile extraction
scheme for sludge samples.
The XAD-2 cartridge was carefully opened, any silicone stopcock grease
removed with a CH2cl2 wetted towel, and the contents transferred to a
preextracted Soxhlet thimble. The XAD-2 material in the Soxhlet was spiked
with surrogate mix and extracted overnight with CH2C12. The extract was
concentrated to 1 to 100 ml based on the amount of extractable material
present.
C-25
-------
TABLE C-6. SEMI VOLATILE ORGANICS ANALYZED IN WOOD PRESERVING SAMPLES
Compound Number
Compound Name
1
Phenol
2
2-Nitrophenol
3
2,4 Dichlorophehol
4
2,4,6 Trichlorophenol
5
4-Nitrophenol
6
4,6-Di n i tro-o-cresol
7
Pent a
8
Acenaphthene
9
Fluoranthene
10
Napthalene
11
Benz(a)anthracene
12
Chrysene
13
Acenaphthylene
14
Phenanthrene
15
Fluorene
16
Pyrene
17
Anthracene
C-26
-------
Figure C-9. Proposed analysis scheme for phenols/PAH's in wood
preserving sludges.
C-27
-------
Quality control for XAD-2 samples consisted of the analysis of
surrogate spikes, field blanks and spiked method blanks.
Ash Samples—
20.Og of the flyash were placed in a clean Soxhlet thimble then sp'k d
with surrogates at concentrations of 100 yg. Each sample was extracted with
CH2C12 overnight and concentrated to 1.0 ml. Quality control for ash
samples consisted of the use of surrogate spikes and the analysis of a method
blank and a spiked sample.
Extract Analysis—
Each of the extracts obtained as described in the previous sections
were analyzed for the compounds listed in table C-6 using fused silica
capillary column GC/MS. The instrumental operating conditions are listed in
table C-7.
The quality control requirements listed in EPA Method 625 were
followed, including analytical calibration, mass spectrometer tuning to meet
decafluorotuphenylphospline (DFTPP) criteria, and the use of the internal
standard quantitation method.
Analysis of Metal Species—
Metals were analyzed by standard methods. Sludge samples were
vigorously acid-digested prior to analysis for metals using atomic absoprtion
techniques.
C.3.2 Results and Discussion
The quantitative results for the incineration test are given in
tables C-8 to C-10. To summarize, the incineration process gives rise to very
low or undetectable levels of airborne volatile pollutants. The bottom ash
from this process does contain significant concentrations of uncombusted
material. Day 1 samples were not analyzed.
C-28
-------
TABLE C-7. FUSED SILICA CAPILLARY COLUMN PARAMETERS
Column:
30m x 0.25m SE-54 WCOT (J J
Sp1 it less Injection Parameters:
Injection mode:
Sweep initiation:
Sweep flow:
Column flow (He)
measured at
atmospheric:
Interface:
Temperature:
Column directly coupled to
Temperature Program:
Initial:
Program:
Hold:
Mass Spectral Parameters:
Ionization mode/energy:
Totoal scan time:
Mass range:
W Scientific)
Splitless
30 sec
>12 ml/min
1.0 ml/min
300°C
source (no transfer lines)
30°C for 2 min
Ramp to 300°C o 10°C/min
300°C, 15 min
Electron impact/70 eV
1.0 sec
35 to 475 AMU
C—29
-------
TABLE C-8. ANALYTICAL RESULTS FOR TEST DAY 2
Compound
Bottom
ash*
Baghouse
ash*
Mechanical
hopper ash*
Sludge*
CAI**
2-Nitrophenol
<0.5
<1.0
<0.5
<10
36
Penta
<0.5
<1.0
<0.5
740
<10
Phenol
<0.1
<0.5
<0.1
1200
2
Fluoranthene
92
0.7
0.5
2200
<1
Naphthalene
10
10
10
1300
280
Benzo(a)anthracene
7.6
<0.5
<0.1
160
<1
Benzo(a)pyrene
1.4
<0.5
<0.1
<20
<5
Benzof1uor anthene***
9.3
<0.5
<0.1
52
<5
Chrysene
1.2
<0.5
<0.1
180
<1
Achenaphthylene
4.4
<0.5
<0.1
130
<1
Anthracene
4.5
<0.5
<0.1
760
<1
Benzo(ghi)perylene
<0.5
<1.0
<0.5
<20
<5
Fluorene
0.6
<0.5
<0.1
1200
<1
Phenanthrene
24
6.9
0.6
1800
<1
D i benzo (a, h) an thr acene
<0.5
<1.0
<0.5
<20
<5
Indeno(l,2,3-cd)pyrene
<0.5
<1.0
<0.5
<20
<5
Pyrene
29
<0.5
<0.1
1200
<1
Benzene
NA****
NA
NA
1.9

Toluene
NA
NA
NA
12

Ethylbenzene
NA
NA
NA
17

*	Concentration in units of ug per gram
**	Total yg collected
***	Mixed isomers
****	Not analyzed
C-30
-------
TABLE C-9. ANALYTICAL RESULTS FOR TEST DAY 3
Compound
Bottom
ash*
Baghouse
ash*
Mechanical
hopper ash*
Sludge*
CAI**
2-Nitrophenol
<0.5
<1.0
<0.5
<10
74
Penta
<0.5
<1.0
<0.5
260
120
Phenol
<0.8
<0.2
<0.1
1000
<2
Fluoranthene
15
0.2
0.6
340
3
Naphthalene
18
3.9
6.5
1000
1100
Benzo(a)anthr acene
0.6
<0.2
<0.1
120
<1
Benzo(a)pyrene
0.1
<0.2
<0.1
<30
<5
Benzofluoranthene***
0.9
<0.2
<0.1
64
<5
Chrysene
0.7
<0.2
<0.1
120
<1
Achenaphthylene
3.0
<0.2
<0.1
68
<1
Anthracene
1.0
<0.2
<0.1
250
<1
Benzo(ghi)perylene
<0.5
<1.0
<0.5
<20
<5
Fluorene
0.8
<0.2
<0.1
420
<1
Phenanthrene
31
3.0
0.5
590
<1
Di benzo(a,h)anthracene
<0.5
<1.0
<0.5
<20
<5
Indeno(1,2,3-cd)pyrene
<0.5
<1.0
<0.5
<20
<5
Pyrene
7.9
<0.2
<0.1
310
<1
Benzene
NA****
NA
NA
<1.0
NA
Toluene
NA
NA
NA
3.7
NA
Ethylbenzene
NA
NA
NA
5.7
NA
* Concentration in units of pg per gram
** Total vg collected
*** Mixed isomers
**** Not analyzed
C-31
-------
TABLE C-10. ANALYTICAL RESULTS FOR TEST DAY 4
Bottom Baghouse Mechanical
Compound	ash* ash*	hopper ash* Sludge* CAI**
2-Nitrophenol
<0.5
<1.0
<0.5
<10
<10
Penta
<0.5
<1.0
<7.4
80
<10
Phenol
<0.6
<0.3
<0.1
1400
2
Fluoranthene
1.4
6.2
1.7
170
<1
Naphthalene
9.6
5.1
2.2
560
140
Benzo(a)anthracene
<0.1
<0.5
<0.1
27
<1
Benzo(a)pyrene
<0.1
<0.5
<0.1
<10
<5
Benzofluoranthene***
<0.1
<0.5
<0.1
14
<5
Chrysene
<0.1
<0.5
0.3
28
<1
Achenaphthylene
<0.1
<0.5
<0.1
24
<1
Anthracene
0.2
<0.5
0.2
92
<1
Benzo(ghi)perylene
<0.5
<2.5
<0.5
<20
<5
Fluorene
<0.1
<0.5
<0.1
180
<1
Phenanthrene
3.0
7.3
0.4
330
<1
Dibenzo(a,h)anthracene
<0.5
<2.5
<0.5
<20
<5
I n deno (1,2,3-cd) py r ene
<0.5
<2.5
<0.5
<20
<5
Pyrene
0.4
<0.5
<0.4
140
<1
Benzene
NA****
NA
NA
<1.0
NA
Toluene
NA
NA
NA
9.0
NA
Ethylbenzene
NA
NA
NA
10
NA
* Concentration in units of ug per gram
** Total ug collected
*** Mixed isomers
**** Not analyzed
C—32
-------
Volatile Organics—
Low levels of volatile aromatic hydrocarbons are present in creosote
(figure C-10). These levels are greatly reduced in the waste sludge. The
total hydrocarbon content of the stack gas was <0.01 ppm.
The detected levels of aromatic hydrocarbons in the sludge samples were
close to the detection limit. The reported levels have been corrected for
method blank contribution. The accuracy of the method at these low nanogram
levels is poor. Since the injection of organic extracts on the volatiles GC
column led to the accumulation of higher-molecular-weight aromatics. It was
necessary to bake out the column at 200°C after every few analyses.
Semivolatile Organics
The application of fused silica capillary column GC/MS to this project
allowed for greatly improved compound identification over that obtainable with
packed column methods. Polynuclear aromatic isomers such as phenanthrene/
anthracene and benz(a)anthracene/chrypene can be resolved by this method. But
the Finnegan 4000 capillary injection system is subject to a high degree of
front-to-back discrimination. In the split/splitless mode of injection, the
sample first is volatilized in the injection port then recondensed at the head
of the column. This process results in a substantial variation from injection
to injection in the fraction of a given component in the sample placed on the
column. An extra degree of random error is introduced into the determination
of early eluting compounds (phenol and maphthalene) by decreasing the
precision of the analysis. To correct for this effect, the early eluting
compound quantitations were corrected using the recovery of the surrogate
spike, dg-naphthalene.
Figure C—11 is a chromatogram from the analysis of semivolatile
organics in a sludge sample. The major identified peaks are labelled. There
C—33
-------
100.0-1
RIC
09/1040 20:59:06
SAMPLE: U0274 UOA 1UL INJ
gMGEi C I, 550 LABEL: N
DATA: U0274S «1
CALI: US0006 «1
0, 4.0 QUAH: A 0, 1.0 BASE: U 20, 3
SCANS 1 TO 550
0
1
GO
-P*
Peak 194 -
Peak B
Peak C
Peak 260 -
Peaks E -
-	Benzene
-	Toluene
-	Ethylbenzone
-	Internal standard
-	Solvent Impurities
460992.
-------
nrr	DATA* WP8818 ft
89/16/88 12ll3l88	CALIs C991580A *3
SMPUEs HP8018,07-827-27 S.	8.M--18NG 018
RMQEi G 1.2888 LMELt H	8. 4.8 (WANs A 0. 1.8 BASEs U 28, 3
SCANS 188 TO 2888
Peaks numbered as per
table X.
8:28
16:40
1508
25:08
2080 SCAN
33:20 TIME
Figure C-ll. Total ion current chromatogram of waste sludge extract.
-------
are clearly a large number of organics present in addition to those of
interest to this program. Figure C-12 is a chromatogram from a bottom ash
extract. Only the polynuclear aromatics were detected in ash samples; no
phenols were detectable.
Table C—11 compares the content of the raw creosote, the working penta
solution, the sludge wastewater, and the fuel (sludge and wood chips) for
representative compounds. From this data, it is apparent that the
incineration fuel is similar in relative proportion to the starting
preservative solutions. The major changes through the process are dilution,
first with water and then with wood chips.
As shown in the data tables, the ash samples contained ppm quantities
of polynuclear aromatics. Whether these arise from unburned fuel or by
partial combustion is not known. The absence of phenols in the bottom ash is
evidence in favor of the latter hypothesis. Only naphthalene and low levels
of phenols were detected in the XAD-2 cartridge samples; naphthalene was
consistently detected. Penta and 2-nitrophenol were detected at low but
significant levels only in the samples from days 2 and 3. There is no simple
explanation of the nitrophenol: this compound was never detected in a sludge
or ash sample. Figures C-13 and C—14 are chromatograms of the day 3 XAD-2
cartridge extract and an XAD-2 blank cartridge, respectively.
Metals
The results of the metals analyses are shown in table C-12. This
information will be used to evaluate ash partitioning effects and flowrates of
the ash streams.
C-36
-------
0
1
CO
180.0-1
RIC
RIC	DATA: MP2711 »1
89/22/90 14i18:08	CALIs C091980A «3
SAMPLE: MP2711,07-027-llS,BN+A,R£RUN,0.5UL=10NG 010
RANGE: G 1.2000 LABEL: M 0. 4.0 OJANj A 0, 1.0 BASE; U 20, 3
ft"
SCANS 100 TO 2000
1353
war-
453632.
1656 l8.16 1914
1500
25:00
2000 SCAN
33:20 TIME
Figure C-12. Total ion current chromatogram of bottom ash extract.
-------
TABLE C-ll. SELECTED COMPONENTS IN WOOD PRESERVATIVE
SOLUTIONS AND INCINERATION FUEL
	Concentration ng/q	
Compound
Creosote	Penta	Sludge	Fuel
Phenol
8000
4,000
1,200
12
Naphthalene
24,000
660
900
18
Penta
1,700
16,000
260
15
Phenanthrene
37,000
1,200
850
18
Toluene
1,400
NA
8
NA
C-38
-------
RIC	DATA: HP2741 *1	SCANS 186 TO 2000
09/22/90 19:22:08	CALI: C831980A 13
SAMPLE: 07-827-41 BH+A 0.5UL=18NG Die
8:20	16:46	25:00	33:20 TIME
Figure C-13. Total ion current chromatogram of an XAD-2 extract.
-------
RIC	DATA: HP22R »1	SCANS 100 TO 2860
09/18/90 16:04:00	CALI: C091580A *3
SAMPLE! MP0022 RERUN.9.5UL*10HG 018,08,027-038,XAO BLANK BN+*,FU=2.0ML
Figure C-14. Total Ion Current Chromatrograro From an XAD2 Blank Cartridge.
-------
TABLE C-12 METALS ANALYSIS
m.

As
Be
Cd
Zn
Cr
Cu
Pb
Mi
M
Sb
Hg
Se
T1
Bottom ash day 2
0.35
1.0
0.02
2.0
1.0
29.0
1.0
0.6
0.06
5.0
1.0
5.0
0.1
Bottom ash d s«y 3
40.5
0.7
0.02
5.0
0.6
57.0
1.0
0.5
0.06
5.0
2.0
10.0
0.1
Bottom ash day 4
73.0
1.0
0.02
8.0
1.1
29.0
1.0
0.4
0.06
5.0
0.9
10.0
0.1
Baghouse ash d«\y 2
0.53
0.4
0.3
750.0
2.9
230.0
1500.0
0.4
0.1
25.0
5.0
5.0
0.1
Baghouse ash day 3
11.4
0.4
0.4
750.0
4.4
305.0
1500.0
0.4
0.1
38.0
12.0
10.0
0.1
Baghouse ash d^y 4
49.0
0.2
0.3
500.0
3.4
225.0
1200.0
0.2
0.1
28.0
11.0
10.0
0.1
Ned. hopper ash day 2
0.02
2.0
0.1
90.0
1.9
85.0
100.0
0.3
0.06
5.0
3.0
10.0
0.1
Med. hopper ash day 3
6.5
0.9
0.02
40.0
2.0
120.0
10.0
0.3
0.06
5.0
4.0
5.0
0.1
Med. hopper ash day 4
0.88
0.9
0.02
30.0
1.8
70.0
10.0
0.2
0.06
5.0
2.0
5.0
0.1
Sludge day 2
6.8
0.001
0.02
10.0
2.7
36.0
1.0
0.2
0.06
0.05
0.01
0.05
0.001
Sludge day 3
3.5
0.0009
0.02
7.0
2.6
48.0
1.0
0.2
0.06
0.25
0.01
0.05
0.001
Sludge day 4
8.1
0.0009
0.02
3.0
2.0
19.0
1.0
0.2
0.06
0.16
0.02
0.10
0.001
-------
SECTION C-2
RAW DATA: PRELIMINARY AND ISOKINETIC SOURCE EMISSION SAMPLING
C-43
-------
ACUREX CORPORATION
Acurex Project Ho.
Field Dates -p-Sil
Run AJ« /
30Ibbl.
- Sro
Sampling Location^
Stac-k tot 7.
Sampling Date

-to
Crew Chief:

FIELD CREW
Testing Engineer:
1
M . K, On I fee
2


3

Engr. Technician:
1
B. C .
2


3

Lab Technician:
1


2


3

Process Engineer:
\

?

Other:
1


2




C-44
-------
TRAVERSE POINT LOCATION FOR CIRCULAR DUCTS
DATE . n - -a.) - 80		
SAMPLING LOCATION	„ g 	
INSIDE OF FAR WALL TO
OUTSIDE OF NIPPLE, (DISTANCE A) -33 	
INSIDE OF NEAR WALL TO
OUTSIDE OF NIPPLE,(DISTANCE B) 3 	
STACK 14)., (DISTANCE A • DISTANCE B) Jn in.	
NEAREST UPSTREAM DISTURBANCE	.
NEAREST DOWNSTREAM JKSTURBANCE		
CALCULATOR			SCHEMATIC OF SAMPLMG LOCATION
TRAVERSE
POINT
NUMBER
FRACTION
OF STACK I.D.
STACK 1.0.
PRODUCT OF
COUMBtANDS
(TO NEAREST I* INCH)
DISTANCE B
TRAVERSE POINT LOCATION
FROM OUTSIDE OF NIPPLE
(SUM OF COLUMNS* 15)
1
¦ 03 Co
3© M#



Z
.oiz
c
2 >u


J.



V-.20
M. W

*






r




ID

-------
PRELIMINARY VELOCITY TRAVERSE
imte -)-21-9G
LOCATION S ru.fL ul	S
STACK IP SO'
BAROMETRIC PRESSURE, In. Hf 3P 3C
STACK GAUGE PRESSURE, in. ty •*. 3U
OPERATORS	, STgPnf
SCHEMATIC OF TRAVERSE POINT LAYOUT
TRAVERSE
POINT
NUMBER
VELOCITY
HEAD
toPjJ.ln.tyO
STACK
TEMPERATURE
<•

- »

AVERAGE

«36T*.
TRAVERSE
POINT
DUMBER
VELOCITY
HEAD
fept), to.H^O
STACK
TEMPERATURE
(ty, *r








































































AVERAGE


EPA (Oil) 233
4/72
C-46
-------
DRY MOLECULAR WEIGHT DETERMINATION
COMERTS:
mat 7-32	
mnmvm&aMm^iiroo ^ ^ m ^
1—ftpg—6g»g	
—				r^g'.Tf g>»ge.ir	
	¦mi III 1*°* -PRT	m*F **T.T	
mmnm—^bbSaS	
S. RUN
1
2
l
mmcE

¦MKKM^KRTOF
GAS
ACTUM.
«CT
nam.
KKM
KT
ACTtML
REABMG
1ST
BET
VOLMK
¦otTrtwr
STACK CM (DRV MSB)
co*
v>

*.*-
y>

V>
Y>
**/m
/.? su
QjgffETBACIIMLO}
KMM6MMI«CnML
€0^MEMMQ
n.z
tH.%
1*7.2.
/*.sr
l\Z
/V.v
/*.#
»/M
y.*7 5fc
COpcr bkhmlco
KAMK MB ACTUM.
9fKMmet
rt.Z
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n.z
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a/m
0
mffCTBMMM
laCTMbCORCMMQ
tro.
90.V
tern.

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to>.%
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TOTAL

era am m
4.7?
-------
ISOKINECTIC SAMPLING WORKSHEET
Reformed by
Date "7'22'iO	
Sample Location	Aj-7.
Test Wo./Type / /ifccz 	
K ¦ 782.687 (Cp)2 (1-B»0)2 Pt Hj
, . _	K 2 M Pm
<-)* (£L3J (J®1)
C-48
-------
ISOKINECTIC NOZZLE CALCULATION
AND
SAMPLIN6 RATE CALCULATION
Performed by
Date		
Sample Location Cpx.* AJa?
Test No./Type ./
Nd -/ AH TS V25
V°^/
where: N4

C-49
-------
not MM
( of 3
0
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MM«nt	-yr>»r
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Probe Lenfth art Tin g"f t>vP6V
NmmI l.o. (Wo.1 .g»fg»
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H»lac«1«r M«1*t. Dry, (H^l 3^2^
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WW*	• ?.o?1
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-------
ISOKINETIC PERFORMANCE WORKSHEET
Performed by \xA^ar
Oate		;
Sample Location	Aj»2
test No./Type / J	^
*1 ¦ 17*» (T» * w"v» std ~ std>
i 7S i; ^F~
where: XI * Percent Isokinetic
Temperature stack gas, average (OF)
Ts
JtV.'i
Meter volume (std), 17^ + Ufl6^
/teaM/fcao) ~ (-ff£ \
"•"VSJ/Wj* ™ )
y
m std

Volume of liquid collected (gram)
*'c

Volume of liquid at standard condition (scf)
VIc x 0.04707
*w std
m.r?
Total sample time (minutes)
e
2UO
Stack gas proportion of water vapor
»..« . <22>
V. std * y. ,u ~ (4&»?
8WO

Molecular weight, stack gas dry
(lb/lb-mole)
"d

C-53
-------
ISOKINETIC PERFORMANCE WORKSHEET (Concluded)
Molecular weight, stack gas wet
(lb/lb-mole)
' Hdfl-B^) ~ 18(8^), e2£)(l-.£21) * 18(^t)
Ms

Absolute stack pressure (In. Hg)
-------
7-SZ-to Ta-JT I
SAMPLE HANDLING LOG	^	_
Task No.			Recorded by	^ , CL mH
Run
No.
Sample
No.
Activity
Date
Time
Personnel
Remarks
/

5 UAy./W«S«.W
" I

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ywwwiyiii
-------
ACUREX CORPORATION


Run fi)0 2.
Acurex Project No.
-i en trt-2
Field Dates 1-2i

60
Samollna Location /0«*2
Samollno Date '•J-.J'Z-C'ft


FIELD CREW
Crew Chief:

R .c_. s
Testing Engineer:
Engr. Technician:
Lab Technician:
Process Engineer:
Other:
1

2

3

1
R. . L . CntPhrtL*sC
2

3

1

2

3

1

2

1

2



C-56
-------
DRY MOLECULAR WEIGHT DETERMINATION
CMCRIS:
mm				
lltWifllhBIM /Q9C	
IWUHTHI	SOO 9 	
SMPIE TYPE (ME, MTEOMTER, CONTMNWS CMI)	
— .lil ¦ l— OPt^T .--.tu. r-yg .TC	C.rffLti	
MMimnAMK
ffHolF
¦WW		
N. RUN
1
i
1
AVEMCE

MUCULMVEIMTOF
CAS
ACTUM.
REMMNG
jcr
ACTUM.
REAM*
NET
ACTML
AEADMC
NET
MET
vm.uk
MLmiEff
STACK CAS (ORV MM
q,. ft/ft**
CO;
V>
v>
y.v
v.*


+M
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if 51
Offers actmlo*
mmmmmnam.
C%«CMMG)
ifr.Sr
!*>
n.v
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~Sr.v-
/V.2.
lt.%
*/w
yr?c>
COocr is actum, co
wmmmmncnm.
9i*uamsi
-

—

-

o
a/M
o
PtMTBMHMB
| ACTMLOONCMMQ

Sri. 1



£/.C
9I-2Z
am
32.7 7

TOTAL

iriOMzm
417
-------
FIELD DATA
Ptga J	of 3
¦ate "I - * -•»*>
K"
«¦*!• Ucet1*_Jd2tfJ6^rIL3L.
Sw»1« T— XHfV - A, H.
tai linker 	X
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Filter Unlitsl		
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riMl at <*»
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J *1. CFM
htlwtf Www
final
Initial
M
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rn f
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H J k_.
Silica Gal
?-o n*> <\
Probe lenfth .and Type .!_¦>
Motzal I.D. (*».)_
ksswad Nolstara
C/.\sr
1\IT
Molecular Height, Dry, (B^)	
Meter Soi lk*>er	 0*4-
TTTT
W
Hater Coefficient	
¦ Factor /("I'i	
K ¦*
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to')
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5^«»l \
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ta* Hrtar
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Velocity
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lata*
la. Hf

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lapinfer
Or^wlc
Nodule

fiat Nctar

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Oven
la
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76


76
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 1 . 4£.^| |
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Wl

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-------
P»ge 2.

V ClKk T*h
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6as Meter
fteailnf .
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Velocity
Head
Orifice Pr
Differ**
(AH), In.
ess«re
Twperatare OF

r«p
Tacuwi
In. Hg
A«g.
Tr»
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mrm
itlal
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Stack
Profce
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Orgatlc
Nodule

(as Hater
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In
Art
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C-13 V- j


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V,r,
'ft
-------
ISOKINETIC PERFORMANCE WORKSHEET
Performed bv
0#te	~>-2'X-*n	
Sample Location	Aj*. ?
Test Wo./Type P / vAK-?f
tl - 17>33 (T» 4 460)(v" 'td + v» »t<0
i v; ^ Nd2
where: XI ¦ Percent Isokinetic
Temperature stack gas, average (°F)
T#
ZSl.(
Meter volume (std), 17.^ 4


/(	A * (^f} \
i7-6HWWj +
Vm std

Volume of liquid collected (grams)
Vlc
J&Sr.Y
Volume of liquid at standard condition (scf)
Vlc x 0.04707
std
rw
Total sample time (minutes)
e
Suo
Stack gas proportion of water vapor
v. ltd . <£2»
>U *.td • ttiiJfc.

.67 2.
Molecular wight, stack gas dry
(lb/lb-mole)
V

C-61
-------
ISOKINETIC PERFORMANCE WORKSHEET (Concluded)
Molecular weight, stack gas wet
(lb/lb-mole)
. Md(l-Bw0) + lBCB^), * 18(ifi22.)
Ms

Absolute stack pressure (in. Hg)
P t k {1n. H.O) {£±)
pb + uac 15.6 - irnr


Stack mlorlty (fp«)
,	 /T.avg + 460
«•«» . V-
C-62
-------
SAMPLE HANDLING LOG	_ 0
To* No. tmt.fm'?		Recorded by JP*X\qs
Sun
No.
Sample
No.
Activity
Date
Time
Parsonnel
Remofki
SL
CcrtM^
(HUUe^A.
t-21-%

E>c3$k.
—
1


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3 tuJZ
-------
Teak No.
SAMPLE HANDUNG LOG
Recorded by	CriPS
Run
No.
Sample
No.
Activity
Date
Time
Peisonnel
Remarks


w »l r^-Q

f> r&






,y.
-------
ACUREX CORPORATION
Run	A*e> 3
Acurex Project No. 2o~)6>(a?
Field D'tes	
Sampling »«v*tion 2.
Sampling Date •7-2V--gC»	
FIELD CREW
Crew Chief:
Testing Engineer: 1 /»*. ft. C.h-,P<
2	
Engr. Technician: 1 £ L . S-rfP^r/ug
2	
Lab Technician: 1_
Process Engineer: 1_
2_
Other:	1_
C-65
-------
ISOKINETIC NOZZLE CALCULATION
AND
SAMPLING RATE CALCULATION
Performed by
Date 7-gf-frp	
Sample Location Oth-<-(	)/
Nd

ah - ic (Nd)4 i (AP)
s
where: AH » Pressure differential across the orifice meter (1n H2O)
Nozzel diameter, actual (inches)
"d
.3 1 2
Temperature of gas meter (°F)
Tm
10
Temperature of stack gas (°F)
Ts
SZO
Stack gas velocity pressure (in H2O)
AP

(<__> (_)' j&j ifji iia)
AH
j.fr
Na?1c number W2.iT l.Utsf4
MM4
t.w
C-66
-------
ISOKINETIC SAMPLING WORKSHEET
Peformed by
Date n-Zt-kO
Sample Location .S-nA-ci^
Test No./Tvoe 3 / XAftg - p-j
K ¦ 782.687 (Cp)g (1-8^)2 P5 Md
where: K * Content of fixed end assumed parameters (dlmenslonless)
Pltot coefficient (dlmenslonless)
Cp
.»i
Water vapor In the gas stream
(proportion by volume)
Bwo
.or
Absolute stack gas pressure (1n. Hg)
Ps
30.71.
Molecular weight, stack gas dry
Ob/lb-mole)
Hd
n.z
Orifice coefficient (dlmenslonless)
K0

Molecular weight, stack gas wet
(lb/lb-mole) Vl-B^) ~ ^(B^)
"s
*Sr-t1
Abolute meter pressure (1n. Hg)
pm
?D
782.687 (JV_)2 (l-^£)2 (3«.?2i (yj.)
(-JSk)2 (2Lil) (22*1)
K

C-67
-------
DRY MOLECULAR WEIGHT DETERMINATION
co—rwri:
mm -T-lY'g-Q	
KWHJKfEgMtCLBOO lf-/Q	
vmuminctm	aj» Z		
SMTU vm «AC, IKTEGMTCB. COaTMRMS CUM £./?* S 	
Hm.mm.mm gfoAn r.rifZ
a/m
0
K2PETSMMB
ACTUM. CD MENMO
/
-------
Date 1-2V-Z0
ISOKINETIC PERFORMANCE WORKSHEET
Performed byW\?^
Sample '	?-	
Test M" /Ty^P 9 / *-Ats-7 , ^
yT . 17.33 (Ts * 460)(Vw 8td * Vm Std^
-	-	~	Mtf2
where: <1 • Percent isokinetic
Temperature stack gas, average (°F)
h
"SH7.0
Meter volume (std), 17 -64^-—^ ^t~V Hlg^
35t>.e*r" *©.*>1
/(	)\/&Ml) * (T^) \
17-M W/WdJ^ir-/
y
*» std

Volume of liquid collected (grans)
Vie

Volume of liquid at standard condition (scf)
VIc x 0.04707
V* std
HZYI
Total sample time (minutes)
e
ZteO
Stack gas proportion of water vapor
std « ^^
V. ,t< (_)*(_)
®wo
.eO
Molecular weight, stack gas dry
Ob/lt»Mle)
Md
Fj.HZ
C-69
-------
ISOKINETIC PERFORMANCE WORKSHEET (Concluded)
Molecular weight, Stack gas wet
(lb/lb-mole)
Md(l-8W) + 18(8^), gMSH 1-.04.7) ~ m^l)
Ms

Absolute stack pressure (in. Hg)
pstack <1n* H2°> . , }
\ * ",ckiu '¦ ¦ laa ~ -ror
%
>.? 2.
Stark (fpt)
r.. IT avg + 460
8S.4S (Cp) (>, nt-
^ JL_ (I Q*z,) * 460 \
85,49 iiaso j
vs
M'j.S-O
Nozzle diameter, actual (Inches)
*d
.:r:r
¦? r-J>, OJf_?
17.33 (."H2.a4 460)(grg() + £	))
(jfeo) mm co.n) (.use,*
XI
/ ^5. e 07
C-70
-------
nm m*
ftut ' of 1


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Km			0
-------
To* No. JOHo\o"L
SAMPLE HANDLING LOG
Recofded by
Run
No.
Sample
No.
Activity
Date
Tim«
Personnel
Re ma ties

Nxni

o'jero

CO CtjSt. or.^-» _
0*760
• } 'Z *¦'< ' ! ?, un>&C-
o
PVLtMe*.	C#4Wg*^
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firynMg,- fnv^A.^r*^*^
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o"i. Celt.
tfio

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tt-zo
rtpiMrt.ff
/
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-------
Twk No. lo-ttrnWi .	WX*~ '	W *"	Recorded by
Si
Sample
No.
Activity
Date
Time
Personnel
Remarks
.J



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• »
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Comments
-------
ACUREX CORPORATION
Run_J^jt_
Acurex Project No. .5blieUt	
Field Dates ^-ap.ac^n	
Sampling Location Crand ^Jo ?.
Sampling Date v9r-»a	
FIELD CREW
Crew Chief:		R.d .		
Testing Engineer: I	tA C,* >V ^	
2	
Engr. Technician: 1	P i.. '*tci»^p_/o<
Lab Technician:
Process Engineer: 1_
2_
Other:	1
C-76
-------
^>OoR,TH
DATE.
LOCATION.
HACK 1.0..
7- 2C-&P
¦S'lTrf'.r.
PRELIMINARY VELOCITY TRAVERSE
M2LL
jzr.
BAROMETRIC PRESSURE, In. H| TP-IT"
STACK GAUGE PRESSURE, ta. HjO	+.-SJ
OPERATORS-^Rfii, SYgPrrg.(V.i	
8C0F
'J (Si
TRAVERSE
POINT
NUMBER
VELOCITY
HEAD
(&pc>. ta^O
STACK
TEMPERATURE
(T,), *F
' F*vr
•S-fc
sno
z \
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3 (
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^TA»e-<
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SCHEMATIC Of TRAVERSE POINT LAYOUT
TRAVERSE
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NUMBER
VELOCITY
HEAD
inJ^O
STACK
TEMPERATURE
(Tt>. *F








































































AVERAGE



C-77
-------
ISOKINECTIC N0Z7LE CALCULATION
an:
SAMPLING RATE CALCULATION
Performed by.
Date	.
Sample Location	
Test No./Type	
«„ ¦/1H T- VB
where: Kg ¦ Nozzel diameter (inches)
Average pressure differential across the
orifice meter <1n. H2O)
AH

Temperature stack gas, average (°F)
Ts
2L1- *
Temperature of gas meter, average (°F)
Tm

where: AH • Pressure differential across the orifice meter (in HgO)
Nozzel diameter, actual (Inches)
«d

Temperature of gas meter (°F)
Tm

Temperature of stack gas (°F)
h

Stack gas velocity pressure (in H2O)
AP

(i—> (_)~ iigj (_>)
AH

Magic number ( 1*
K(Nd)4

C-78
-------
ISOKINETIC PERFORMANCE WORKSHEET (Concluded)
Molecular weight, stack gas wet
(Ib/lb-mole)
Mdtl-B^) + 18(BW), (	)(1-	} ~ I8(	)
\

Absolute stack pressure (In. Hg)
WOr.H20) (__)
t> 13.S • 1	' TJX
%

velocity (fps)
1	 /T avg ~ 460
85.49 
-------
DRY MOLECULAR tEtGHT OETERMNATKM
MDD;
Mil	7-ac->>o	
MMWfllhH—	iXlQ	
C-me.*. IQoZ.	
SMFU TTPC IMC. CTEOMTCB. COWTMOB CMB)		
fMrncM wmtm S>*t^-T rr FvtWr r.+x.	
iMUHwiff i*»r		
orv*rm		
N. RUN
GAS
1
i
i
MCMCC
KT
VOLWC
MLTVlKIt
mcauMcioiTOF
STACK CM (OUT BMOt
ACTVM.
KT
MINI
KT
aciMi
iknmc
m
CO2
$-.1

5". Z

5". 5

.T2M.
"rw
n
O^RCTBACTVN.0?
KMMCMWMTML
CO^NUMQ
'*.r
fJ.S
/y.$-
n.z
/?.(*
/s.s

*/»

COfKT B ACTUM. CO
tummmmtenm.
0,KMNQ
0

o

0


»/»

WET BM BOB
| ACTUM. CO KMMQ

9t-r

?/.?

n.r

¦/»


TOTAL
Vi.V?
CMAh|Z»
OI
-------
ISOKINETIC PERFORMANCE WORKSHEET
Performed tor  4 *<0)(Vw ltd ~ v» ttd^
i	5?"
where: SI • Percent Isokinetic
Temperature stack gas, average («F)
T«
161.4
Meter volume (std), 17^ ^
/(!S2lA/(£2f) 4
4w /
*¦ std
ssv.in
Volume of liquid collected (grew)
"c
6S).o
Volume of liquid at standard condition (tcf)
V1c x 0.04707
*w ltd
3O04&
Total simple time (minutes)
e
3 SO
Stack gu proportion of water vapor
v. „„ (S±S
l£J#»UOill
"wo
.07^
Molecular weight, stack gat dry
(lb/lb-mole)
"d
Tfi.Z!
C-81
-------
ISOKINETIC PERFORMANCE WORKSHEET (Concluded)
Molecular weight, stack gas net
(lb/lb-mole)
wa-B^) ~ i8(8w), mim-tri) ~ ui^j


Absolute stack pressure (In. Kg)
. %ttc, H". y> (Jr.)
pb ~ 13.{ ¦ . U22S.) ~ "inr
>s
30 ni
Stack velocity (fnO
r [T.avg ~ 460
km (cp) (>, „r
. . •7i+~}<» (\ (36.").^ ~ 460 \
85.49 (%l )(V	M „	w„	 I
\ teast)«3*2) /
v«
Sc>.%o
Nozzle diameter, actual (Inches)
"d
.3'3
17.33 4C0)(£M>r) ~ (	))
*1
tos-.V
(2SL )(£»!) (2£^)(Jj2)z
(n.-n) (^->.*0 (tr\nsT)

C-82
-------
Fi&iwn
'•»» I &
Frrt« Laagtk mt £' fvtCH
InmI I.#. Ih.l S^il
tonMl Kilitan	I 	
Nil«i1r	try. (W^)	
Nttcr Ms llir OCtY	
IkUr twWklwt O.UYU
¦ F«t«r	
K • '
KWO* » » < >* • fe-IST
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riaai at /fc4_e i). -o#i cm
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\ ei«dtTiH
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(<•). « »
fttettjr
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Ml

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la 1
Mar
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tan. ta*.«no
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Tuy- 1 *£ I
SAMPLE HANDLING LOG	0 ^ rs
To* No. toluui		Recorded by ftWvdi*?
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No.
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-------
SECTION C-3
RAW DATA: TOTAL HYDROCARBON DETERMINATION
C-87
-------
TOTAL HYDROCARBON DATA
7-22-80
C-89
-------
I...,

[
n
MW>»".p
-------
•» V'rf
""<1 W |» «

C-91
-------
-------
C-93
-------
TOTAL HYDROCARBON DATA
7-23-80
C-95
-------
{•
f f
1 '
-------
-------
-------
-------
TOTAL HYDROCARBON DATA
7-24-80
C-161
-------
001
I
r
i
C-102
I	!
U
' I
II
-------
C-103
-------
n
¦L I j r-;= I jft
C-104
-------
C-105
-------
TOTAL HYDROCARBON DATA
7-25-80
C-107
-------
r
C-108
-------
C-109
-------
r
c-iio
M
-------
SECTION C-4
RAW DATA: SPECIFIC LOW-MOLECULAR-WEIGHT HYDROCARBON DETERMINATION
C-lll
-------
-------
SPECIATION DATA
7-22-80
C-113
-------
...
—-
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SPECIATION OATA
7-23-80
C-117
-------
-------
$*•"»<.« fCl«A ¦
CNTiMMvS	SM">-
Lm. U>~W -STHCK. WJ

ffeivN
C«uT*H)i«i DCMrfbSM)#.
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Stoc* IkAt S*wrct
ComthmwS	Smu
CwC. -St»*K. A*d"Z.
SU>*K To>/V2j-*o
A**«Ju*t i»#>».'
-------
I
-------
SPEC I AT ION DATA
7-24-80
C-123
-------
r>
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f
po
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1
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0
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SPECIATION DATA
7-25-80
C-131
-------
-------
-------
o
CO
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-------
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