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Project 92-229-02February 1993 CanonieEnvironmenlal S
Draft Report
Dechlorination Treatability StudySoilTech Anaerobic Thermal Process andBase Catalyzed Decomposition
••'ertac Site^acKsonviile, .Arkansas
^reoared For:
Hercules incorporatedWilmington, Delaware
Draft Report
Dechlorination Treatability StudySoilTech Anaerobic Thermal Process andBase Catalyzed Decomposition
TABLE OF CONTENTS
LIST OF TABLES
LIST OF FIGURES
LIST OF APPENDICES
1.0 INTRODUCTION
1 . 1 Site Description
1.2 Material Description
2.0 TREATABILITY STUDY APPROACH -f^'ii- .._:•:•••
2.1 ATP Treatability Test
^2.1.1 ATP Treatability Test Procedures^
2.1.2 ATP Treatability Test Sampling and Analysis
IX-.2.1.3 ATP Treatability Test Deviations from the Work Plan
2.2 BCD Treatabtf'itytJest
2.2.1 BCD Treatability Test Procedures
'^2.2 BCD Treatability Test Sampling and Analysis
2.2.3 BCD Treatability Test Deviations from the Work Plan
3.0 ANALYTICAL RESULTS SUMMARY
3.1 ATP Testing Results
3.1 .1 Physical Results
3.1.2 Chemical Results
3.2 BCD Testing Results
PR/W:/82-229/TREAT.RPT IFebruff 24, 19831
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2
3
4
4
5
9
9
10
10
12
12
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14
14
15
17
TABLE OF CONTENTS
(Continued)
PAGE
3.2.1 Analytical Results 17
3.3 Quality Assurance 18
4.0 ATP AND BCD FULL-SCALE TREATMENT ENGINEERING AND
ECONOMIC EVALUATION 20
4.1 ATP and BCD Full-Scale Process Integration ^ 20
.:;:'"
4.1.1 Full-Scale Alternative Recommendation 23
..•.••y<-.4.1.2 Full-Scale ATP and BCD Process^escription 23
^4.2 Full-Scale ATP System Evaluation 24
4.2.1 Moisture Content ^ " " " 25
4.2.2 PartlcpSize 26
4.2.3 Hydrocarbon Content 27.:•'•'''•>'.
'"•^2.4- Material Handling Characteristics 27
4.2.5 Chemical Characteristics 28
4.3 Full-Scale BCD Process 28
4.3.1 Full-Scale BCD Reactor 29
4.3.2 Reagent Addition for Full-Scale BCD Reactor 30
4.4 Full-Scale Treatment Residuals Management 31
4.5 Regulatory Issues and Permitting 32
4.6 Economic Evaluation 33
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TABLE OF CONTENTS
(Continued)
0OS^0000
PAGE
5.0 CONCLUSIONS AND RECOMMENDATIONS
TABLES
FIGURES
APPENDICES
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LIST OF TABLES
TABLENUMBER
2
3
TITLE
Summary of Retort Test Mass Balances forATP Treatability Study Samples
Summary of Combustion Test Mass Balancesfor ATP Treatability Study Samples
Summary of Physical and Chemical AnalysesConducted for ATP and B^D TreatabilityStudies
4 Solids Analytical Results Summary, ATPSystem Bencflk-.Scale Tests
>Combustion Solids TCLP Analytical Results,^P Dechlorination Bench-Scale Tests•y"^^
Condensate Aqueous and Solid Fractions -Analytical Results, ATP System Bench-ScaleTests
BCD Bench-Scale Tests Analytical Results
PFI/W:/92-229/TREAT.LOT IFlbruTy 24, 19931
LIST OF FIGURES
FIGURE DRAWINGNUMBER NUMBER
1 92-229-A11
2 92-229-E12
3 92-229-A13
4 92-229-A14
5 92-229-A15
6 92-229-A16
7 92-229-A17
8 92-229-A18
9 92-229-82^
10 ,^,92-229-A21
1 1 92-229-A19
TITLE
Site Location Plan
Sampling Location Plan
Diagram of Bench-Scale ATP Unit
Wright State University BCD Bench-ScaleReactor .<<;:- ':<
Alternative 'A', Contaminated Solids Treatment
Alternative ...Contaminated Solids Treatment^
Alternative 'C', Contaminated Solids Treatment• .iiX.Alternative 'D', Contaminated Solids Treatment
Simplified Flow Diagram with Dechlorination,SoilTech ATP System
Cross Section, SoilTech ATP System
Evaluation of Optimum Size ATP Unit
PR/W:/B2-229/TREAT.LOT IF*bru*rv 24. 18931
APPENDIX
A
B
C
09
iii ^<0
LIST OF APPENDICES °00
TITLE
ATP and BCD Treatability Study Photographs
Hazen and WSU Treatability Study Reports
ATP System and BCD Process Treatability Study AnalyticalResults
PR\W:\92-663\ACME.LOA IFebruTy 2G. 19831
DRAFT DECHLORINATION TREATAB1LITY STUDYSOILTECH ANAEROBIC THERMAL PROCESS AND
BASE CATALYZED DECOMPOSITIONVERTAC SITE. JACKSONVILLE. ARKANSAS
1.0 INTRODUCTION
Canonie Environmental Services Corp. (Canonie) prepared this Draft Dechlorination
Treatability Study Report on behalf of Hercules Incorporated (Hercules) to demonstrate
thermal desorption and dechlorination treatment technologies for organically-impacted
soils and carbon at the Vertac Site near Jacksonville, Arkansas. SoilTech ATP
Systems, Inc. (SoilTech) conducted the thermal desorption test, and Wright State
University (WSU), directed by Dr. Thomas 0. Tiernan, performed t^Base Catalyzed
Decomposition (BCD) dechlorination test for the study. This treatabttity study was
performed as outlined in the Dechlorination Treatab|li:ty Study Work Plan (Canonie,":i:?
1992b) and Quality Assurance Project Plan (CanonieC,.1992a).
As stated in the work plan, this study/lsKo provide the necessary information tos-''-
evaluate the Anaerobic Thermal Processor's (ATP's) and BCD's applicability for full-^
scale operation at the Vettac Site. The specific objectives stated in the work plan
were to:
1 . Determine the effectiveness of both the SoilTech ATP system and the BCD
process on the materials subject to treatment;
2. Develop parameters for full-scale treatment operation and residuals
management;
3. Establish cost estimates for full-scale treatment;
PRyW;/»2-229/TREAT.RPT IFtxuJry 23, 1 B83I
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4. Define operational constraints and/or limitations with specific respect to this
site; and
5. Identify whether pilot-scale studies are appropriate or advantageous and
determine the potential scope, outcome, and costs associated with such
studies.
To accomplish these objectives, two separate treatability tests were conducted using
1 ) the SoilTech ATP system bench-scale test unit, and 2) the WSU bench-scale BCD^
reactor. Based on the results of these treatability tests, an engineeringi:evaluation was'.}:••'•
performed, and conclusions were made which address the study objectives.
''•'f-y'-'Section 1.0 describes the Vertac Site and the materials^which were tested during this
study. Sections 2.0 and 3.0 contain discussion of the treatability study approach.IA,
and the analytical results, respectively. Section 4.0 presents the
engineering/economic evaluation for full-scale operations. Conclusions and'''•':•:•''''''•>.•
recommendations are included as Section 5.0.
1 . 1 Site Description
Figure 1 shows the Vertac Site location near Jacksonville, Arkansas in Pulaski County.
It is approximately 1 5 miles northeast of Little Rock. In its 60-year history, portions
of the site have been operated as a U.S. Government munitions complex and as a
privately owned herbicide/pesticide manufacturing facility. The property has changed
ownership several times, and is currently owned by Vertac Chemical Corporation
(Vertac). Commercial operations ceased in 1987, and the site is presently under the
management of Hercules with oversight by the U.S. Environmental Protection Agency
(EPA).
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Current operations at the site are limited to remedial measures including treatment of °
surface and ground water by phase separation followed by adsorption through
granular activated carbon. Site waters are collected through drainage ditches and
sumps which surround the central process area to collect surface runoff. Treated
effluent is currently discharged to the Rocky Branch Interceptor Sewer.
1.2 Material Description
As specified in the work plan, site materials tested during this treatability study....•
included site surface soil from the central process area, and spent carbon generated.?•:••'•
from the site water treatment plant discussed above. Sampling locations are shown
on Figure 2. Surface soil was collected within th;e"former chlorination plant siteV'
(Grid 419). and next to the boiler house (Grid 152). These locations and the samples
from these locations are hereafter referenced by the grid numbers. Spent carboniX-
generated from the on-site water treatment system was sampled from a bulk storage
container and several 55-gallon drums stored at the site.'''', .-••';'•::•.
The soil and carbon reportedly contain 2,3,7,8 tetrachlorodibenzo-p-dioxin (2,3,7,8-
TCDD); 2,4'idichlorophenoxyacetic acid (2,4-D); 2,4,5 trichlorophenoxy acetic acid
(2,4,5-T); 2,4,5-trichlorophenoxypropionic acid (Silvex); mono-, di-, and
trichlorophenols; and tetrachlorobenzene.
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2.0 TREATABILITY STUDY APPROACH
This section outlines the treatability study approach. It is consistent with methods
presented in the Work Plan (Canonie, 1992b) and QAPP (Canonie, 1992a) previously
submitted and as modified in discussions and correspondence between SoilTech,
Canonie, Hercules, WSU, and EPA.
During the treatability study, two separate treatability tests were conducted using 1 )
the SoilTech ATP bench-scale test unit, and 2) the WSU bench-scale BCD reactor..-
During both tests, several trials were conducted to establish the opftenal operational^
parameters for the ATP unit, and to confirm data reproducibility of the BCD tests.
Sections 2.1 and 2.2 respectively provide descriptionsArf the ATP and BCD treatability
tests. A
2.1 ATP Treatabilitv Test^
The ATP trea.]^ability testing was conducted by SoilTech between October 19 and 23,
1992 at the^Hazen Research, Inc. (Hazen) Facility located in Golden, Colorado. This
test was witnessed by representatives of Hercules and the EPA. Figure 3 is a
schematic of the ATP test unit.
The following sections contain discussion of the ATP treatability test procedures,
sampling and analysis, and deviations from the work plan.
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2 . 1 . 1 ATP Treatabilitv Test Procedures
The three source samples collected (Grid 152, Grid 419, and spent carbon) were
subjected to the ATP treatability test. This test included four phases:
1 . Feed Sample Characterization;
2. Variable-Temperature Batch Testing (ramp test);
3. Fixed-Temperature Batch Testing (retort test); and
4. Combustion Testing.
During all ramp and retort runs, aqueous and organic liquid condensates were
collected. The condensates recovered were weight and their volumes measured.V'
From these weights and measurements, the material batance closure was determined.
Gas volumes were also measured and recorded for the material balances.
Appendix A contains photographs of the products of the ramp, retort, and combustion^A:.
tests. Appendix B contairTs-Hazen's laboratory report which provides a more detailed
account of th.e treatability test procedures and observations than is provided in this
section. '... /
The following paragraphs outline the procedures and parameters for each phase of the
treatability test.
Feed Sample Characterization: The soil samples (Grids 152 and 419) and the carbon
sample were individually homogenized and split for chemical analyses prior to ATP
treatment. Particle-size distribution, moisture content, and ash content were
measured for each of the three samples received.
PRyW:/92-229/TREAT.RPT |F«bruTy 23, 19B31
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Variable-Temperature Batch Test (Ramp Test): This was conducted on the two soil o
samples and the spent carbon. Mineral oil was added to the samples to insure that
an adequate quantity of condensate was produced for subsequent BCD treatment.
The ramp test provides valuable operative information which is used during the fixed-
temperature batch test (retort test). This information is used to evaluate the expected
behavior of the sample during subsequent fixed temperature tests.
Samples were heated in the rotary drum ATP Batch Unit (Figure 3). For the three
ramp runs (Grid 152, Grid 419, and spent carbon) the material was heated from
ambient temperature to 1,200°F, 1,202°F, and 1,277°F, respectively. The end point>•
temperatures for each run were arrived at within approximately two hours. As the
material was heated, the volume and temperatBTfe of generated vapors wereV
measured. When vapor generation decreased to 0.0^4 actual cubic feet per minute
(acfm), the tests were concluded. .%%..,
Effluent from the ramp test included both coked solids, and organic and aqueous'^A
condensates. The coked s.pfhjs produced by all three ramp tests were black and free-
flowing dry material. The condensate product of the first two ramp tests, which were:.-:::
conducted tan .soil samples, produced two phases with an organic phase on top, and
an aqueous phase on the bottom. The spent carbon ramp test resulted in three
distinct layers: an oil layer on top. an aqueous layer in the middle, and a thick black
layer on the bottom.
Fixed-Temperature Batch Test (Retort Test): These tests were conducted on all three
source samples at two different reactor temperatures, 1,000°F and 1,100°F. These
temperatures were selected as they are the temperatures that will likely be
encountered in the full-scale system. Mineral oil was added to each sample to
increase the hydrocarbon content of the feed and act as a carrier oil for the thermally
PRyW:/92-22»/TREAT.RPT IFfboury 23, 19831
07 ^
r*»0CD
desorbed contaminants. An initial sand charge of about 1 kg was used with this test Q
to simulate the 50-percent hot sand recycle as discussed in the work plan.
Table 1 shows the mass of silica sand, oil, and contaminated sample material added
to the ATP bench-scale unit. the mass of effluent coked material and condensate, and
the associated mass balance percentage. For each trial, as gas evolution dropped to
0.004 acfm, the test was ceased.
The products collected during these tests were coked solids and liquid condensate..•••' •.
The liquids were retained for evaluation of the BCD process. The so^ds were sampled^
and then blended for subsequent combustion tests. The following is a summary of
each retort test bench-scale trial, .i::?-
Grid 152 Soil: Trial 1 had a reactor tftmperature of 1,100°F. The treated solidIX.
material was dark gray, el-usty, free flowing, and easily removed from
the reactor*;: No agglomeration of particles appeared to have taken'" A..
place. Thekprganic condensate produced was a uniform brown-black
liquid with no distinctive layers.
Trial 2 had a reactor temperature of 1,000°F. Similar coked solids
were noted after the trial. However, condensate continued dripping
into the reservoir for an extended period of time after gas generation
had stopped. Because the calculated mass balance was
125.7 percent, laboratory technicians and SoilTech management
personnel concluded that scrubber liquids dripped into the condensate
collection vessel. As a result of this problem, the condensate samples
collected from Trial 1 and Trial 2 were scrapped. The retests were
conducted as Trials 3 and 4. However, solids from the two tests were
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unaffected by the problem, and were used for analysis of the coked
product and for combustion testing.
Grid 152 Soil: After taking corrective action for the scrubber problem. Trials 3 and 4
were conducted to generate new condensate samples. Trials 3 and 4
had reactor temperatures of 1,100°F and 1,000°F, respectively.
Condensate produced during these trials was used for subsequent BCD
testing. For both trials, the solids produced were dark gray and very
dusty. No agglomeration of particles appeared to have occurred. The^
condensate collected was dark brown and no distinct layers were
visible.
Grid 419 Soil: Trial 5 and 6 had reactor temperatures of 1,100°F and 1,000°F,
respectively. Condensate and coked solids generated during theseU^
trials were visually similar to products of the Grid 152 soils trials.
Spent Carbon: Trial 7 ai^f-8 had reactor temperatures of 1 ,100°F and 1,000°F,
respectively. After treatment, the appearance of the carbon was: ; unchanged except that it was dry and some dust was present. No
distinct layers were evident in the condensed liquid of either spent
carbon retort test.
Combustion Batch Tests: Combustion test information is summarized in Table 2. For
this test, equal amounts of retort solids from the 1,000°F and 1,100°F trials for both
soil samples (Grid 152 and 419) were blended together and reintroduced to the
preheated rotary drum of the SoilTech ATP Batch Unit. The solids were retained in
the drum and oxidized via the introduction of air. The combustion test yielded coke-
free, dry, sandy, tan-to-brown material with a particle sized character closely related
PR/W:/a2-229/TREAT.BPT IF«bru*ry 23, 19931
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0to the character of the combination of feed solids and the silica sand charge. This 0
0product, which is representative of the end product of the full-scale ATP System, was
sampled and analyzed for Toxicity Characteristic Leaching Procedure (TCLP)
characteristics.
No combustion tests were planned or performed for the spent carbon coked product.
2.1.2 ATP Treatabilitv Test Sampling and Analysis
^^Samples were collected and analyzed or tested during the ATP treatabiiity study to
demonstrate the effectiveness of contaminant removal from the site soils and carbon.
To accomplish this objective, tests and analyses wece- performed for the feed material,
retort tests solids, and combustion tests solids. Tabte 3 summarizes the tests and
analyses which were performed. Section 3.1 presents discussion of the analyticalIA..
results. :i-
WSU laboratories condue.ted all chemical analyses except TCLP, which were
performed by. Vista Laboratories, Inc. in Broomfield, Colorado. Physical testing was
conducted by,.Hazen.
2.1.3 ATP Treatabilitv Test Deviations from the Work Plan
One deviation from the work plan occurred during the ATP treatability test. As
discussed in Section 2.1.2, scrubber liquids passed into the condensate collection
vessel during the Grid 1 5 2 1,000°F retort test. As stated, both retort trials were
repeated as a corrective measure. Solids from the two original tests were unaffected
by the problem, and were therefore used for analysis of the coked product and for
combustion testing.
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ioS0002.2 BCD Treatabilitv Test
The purpose of the BCD treatability test is to evaluate the effectiveness of the BCD
technology in dechlorinating the condensates generated from the ATP. This section
contains a discussion of the BCD treatability test conducted using ATP test
condensates. A schematic of the BCD reactor is shown on Figure 4 and photographs
are included in Appendix A. The test was performed at the WSU Facilities, and
occurred during November and December 1992. All testing was in accordance with
the QAPP and Work Plan as modified in discussions and correspondence between-^
WSU, Canonie, Hercules, and the EPA. This treatability test wa^s witnessed by>•
Hercules and the EPA.
^V"
The following sections contain a discussion of the" treatability test procedures,
sampling and analysis, and deviations-^pm the work plan.i-X..
2.2.1 BCD Treatabilitv fast Procedures\^^
The BCD treatability test included the following procedures:
Condensate Preparation: WSU received three bottled samples from SoilTech
which represent condensates from the two soil samples (Grid 152, Grid 419).
and the spent carbon that were generated during the ATP system treatability
test. These three condensate samples were mixed together and homogenized
to form one sample. A significant quantity of fines were encountered in the
condensate. This sample was subsequently separated into oil, water, and solid
phases. Contaminants were extracted from both the water and solids phases
and added to the oil phase. An aliquot from each of the water and solids
extracts was obtained for analysis. Then the oil phase sample, including the
PR/W:/92-229/TREAT.BPT IFfbnury 23. 19931
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water and solids phase extracts, was split into three samples for subsequent ^
BCD treatability tests. Solid and aqueous phases were extracted and added to
the organic phase to provide a feed product with a high concentration of
contaminants for BCD testing.
BCD Testing: BCD testing of the condensates was repeated for the three split
samples using the apparatus shown on Figure 5. Reagents added to each test
sample included proprietary liquid and solid catalysts, sodium hydroxide, and a
high boiling oil. Reagent ratios for each test were kept constant to verify.-.•
repeatability in the test results. Specific testing procedures-are contained in
Appendix B. This procedure included the analysis of oil samples prior to the
BCD processing, and at the midpoint and con^fbsion of BCD treatment.
1.
Each test sample was added to .^.reheated reagents at 320°C in a treatment
flask. For each test, the followindJaplproximate weight percentages of reagents
and test sample wef.e. used:
Sqljd Catalyst
Sb.dt.am Hydroxide
High Boiling Oil
Liquid Catalyst
Test Sample
1.5 percent
22.0 percent
29.0 percent
14.5 percent
33.0 percent
100.0 percent
As the temperature increased in the reaction vessel, residual water was driven
from the mixture, collected, and separated in a Dean and Stark receiver and
removed from the process. Organic phase condensates were recycled back into
the reactor. The mixture was maintained at a temperature of approximately
PB/W:/92-22a/TREAT.RPT IFxbnJWV 24. 19931
CanonieEnvironmental
12 ^t^CD
330°C for four hours during the BCD testing. It was cooled to room 00
temperature, and a sample was obtained for analysis. This sample represented
the BCD process midpoint. The mixture was a black oil with some solids and
a pH greater than 10.
Additional proprietary liquid catalyst was added to the remainder of the test
material and the new mixture was heated to the reaction temperature of 320°C.
The mixture was held at 320°C to 350°C for four hours while the distillate
from the Dean and Stark receiver was continuously recycled. The mixture was
then cooled and a final sample was taken for analysis. As With the previous. •''
sample, the final treated sample was a black oil with some solids and a pH
greater than 10. ..:::? ::
V'%^
2.2.2 BCD Treatability Test SamplinQ..,and Analysisi S.>
Analytical tests on BCD...:;feed, intermediate, and final processed samples were.•:;: ::;••;:.•:••:••::..performed to demonstrate^nfe effectiveness of the BCD technology in dechtorinating
ATP condensates, and to demonstrate reproducibility of the treatment method.
Additionally, samples of both the aqueous and solid phase of the composite
condensate were collected. Samples were analyzed for the parameters outlined in
Table 3.
2.2.3 BCD Treatabilitv Test Deviations from the Work Plan
The fines encountered in the condensate generated from the bench-scale ATP test
unit resulted in a minor deviation from the work plan. The work plan specified
sampling and analysis of the organic and aqueous phases of the ATP condensate.
Since some fines were present in the condensate and contaminants could be adsorbed
PFVW:/92-229/TREAT.RPT IF«bn>Ty 23. 18831
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to the solid fines, the three condensate phases were separated, and a separate "'
analysis was conducted on the solids. The solids were also removed because they ®
would clog the BCD syringe pump used to pump the test material into the bench-scale
BCD reactor. This problem is significant in bench-scale testing only and will not be
a problem during full-scale operations.
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3.0 ANALYTICAL RESULTS SUMMARY <^00
The ATP and BCD treatability tests analytical results are summarized and discussed
in Sections 3.1 and 3.2, respectively. Quality assurance is presented in Section 3.3.
3.1 ATP Testing Results
As discussed in Section 2.1, the ATP treatability test includes both physical and
chemical testing. The results of these tests and observations are presented in the..•
following sections. % \
3.1.1 Physical Results
Grid 152 Soil: The untreated sample \^as a reddish-colored sandy soil with visible^ .^•'•••-.:.
humic material. There \»yere no particles greater than one inch, and
about 50 percent of the sample passed the 200 mesh sieve. Moisture'"::;- •,•?••.:
content wa:s T 1 . 4 percent; ash content was 85.5 percent.
}The combustion product sample was tan in color, and approximately
25 percent of the material passed the 200 mesh sieve. The lower
proportion of fine material compared to the untreated sample was due
to the presence of sand, which was added during the retort tests.
Grid 419 Soil: The untreated sample was reddish to light brown in color with low
moisture content (5.5 percent) and humic content. Less than
2 percent of the sample was larger than one inch, and about 38
percent of this sample passed the 200 mesh sieve. The ash content
of this sample was 89.5 percent.
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About 18 percent of the combusted product sample passed the 200 00
mesh sieve. This sample was tan in color. Again, the combusted
sample contained a lower proportion of fine material because of the
sand added during the retort tests.
Spent Carbon: The untreated carbon sample was granular and had a moisture
content of 34.3 percent. The ash content was 7.76 percent. No
sieve analysis was conducted on this sample.
^A screw driver was inserted into each sample and pulled out to visually evaluate the
>••sample cohesiveness. None of the samples exhibited any cohesive characteristics.
^•Af
3.1.2 Chemical Results '^•
<t.Vy
Upon receipt at the Hazen laboratory^: the untreated samples were scanned for
beta/gamma radiation; no,-.f:adiation above background levels was detected. Once the''•'w'"<:'
containers were opened,'EI photoionization detector was used to measure organic
vapors in the.samples' headspace. The spent carbon measured 14 ppm, and the soil
samples measared none above background.
A summary of analytical results for the ATP treatability test samples is included as
Table 4. Laboratory reports are presented in Appendix C. The following table is
excerpted from Table 4 and is a summary of 2,3,7,8-TCDD results for the ATP tests.
PB/W:/92-229/TREAT.RPT IFebruwv 23, 19931
16
SUMMARY OF 2,3,7,8 TCDD ANALYSESSOILTECH ATP PROCESS TREATABIUTY STUDY
(Concentrations in ppb)
Sample I.D.
Grid 152 Soil
Grid 419 Soil
Spent Carbon
Feed Material
293
912
0.446
1,000°FRetort Test
ND (0.0087)
0.0534
0.0805
1,100°FRetort Test
ND (0.0014)
0.007
ND (0.0296)
CombustionTest
ND (0.0010)
ND (0.0019)
Not Analyzed
ND = Not Detected - detection limits in parentheses. \
As shown above, 2,3,7,8-TCDD concentrations weryreduced substantially during the'•;-.;.'*•
ATP processing. As expected, removal was more corftplete during the 1,100°F retort
test than the 1,000°F retort test. The only detected concentration during the
1,100°P retort test (0.007 ppb) was fop the feed sample (Grid 419) which originally
contained the highest 2,3,::7,8-TCDD concentration ( 9 1 2 ppb). Combusted product
samples were all nondetec.t for 2,3,7,8-TCDD.
Tetrachlorobenzene was detected in the untreated spent carbon sample at a
concentration of 50 ppm. This chemical was reduced in the treated spent carbon
sample to concentrations of 0 .12 ppm and 0.04 ppm in the 1,000°F and 1 ,100°F
retort test solids. The Grid 419 retort test product had nondetectabie concentrations
of tetrochlorobenzene and a sample feed concentration of 55 ppm.
Herbicides and polychlorinated phenols concentrations were not detected in the retort
or combustion test products.
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0TCLP testing of the combusted soil product samples are shown in Table 5. 0
0Semivolatiles, eight Resource Conservation and Recovery Act metals, and chlorinated
herbicides were not detected.
3.2 BCD Testing Results
3.2.1 Analytical Results
Analytical results for BCD testing are presented in Appendix C, and summarized and.y '
discussed in Tables 6 and 7 of this section. \
Table 6 provides a summary of analytical testing coodtrcted on the aqueous and solids^
phases of the untreated composite condensate sample-? The solids fraction contained
4,890 ppb of 2,3,7,8-TCDD while the water contained only 5.6 ppb of 2,3,7,8-TCDD.IX.
Other contaminants were also detectedlat'much greater concentrations in the solids
than in the water. These.:.i:results demonstrate that the contaminants preferentially'••:• ..;.<:•::..
adhere to the solid particles' rather than becoming dissolved in the aqueous-phase
condensate.
Table 7 provides a summary of the analytical testing for each of the three BCD
treatability tests. These samples were independently tested to evaluate the
repeatability of the analysis and the BCD process. Analytical results are included for
the feed, intermediate, and final BCD process samples. As discussed in
Section 2.2.1, the intermediate sample was collected after approximately four hours
of BCD treatment. The final sample represents about eight hours of treatment.
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These results indicate that concentrations of 2,3,7,8-TCDD, herbicides, chlorophenols.
and tetrachlorobenzene are reduced to a nondetectable concentration after four hours
of treatment in the bench-scale reactor.
3.3 Quality Assurance
Five quality assurance indicators have been utilized to evaluate the data generated by
the WSU laboratory. The QAPP contains a detailed description of these data
evaluation tools and how each is determined. They include:
1 . Analytical precision;
2. Analytical accuracy;
3. Representativeness;
4. Completeness;
5. Detection limits.
Analytical precision and analytical accuracy were measured by analyzing matrix spike
samples and matrix spike duplicate samples from the ATP combusted solids and the••f^'^.
BCD post-treated oil. These samples were chosen for quality assurance/quality••^•''
control (QA/QC) samples because the combusted solids and post-treated oil represent
the final treated products from both the ATP and BCD tests. Appendix C contains
analytical data packages and summary tables of the analytical results and calculated
QA/QC measurements.
Analytical precision for the data is evaluated by reviewing recoverable percent
differences (RPDs) between the analyte measured in the matrix spike sample and the
matrix spike duplicate. The agreement is excellent because RPDs range from
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0 percent to 25 percent, and most are less than 1 5 percent. This is well within the °^ay
range typically achieved using the analytical methods applied.
Analytical accuracy is evaluated by calculating the percent recovery of matrix spike
samples. During this evaluation, average percent recoveries were compared to
representative data cited in EPA Method SW-846. Generally, the comparisons
indicate reasonable agreement between this study's recovery data and the
EPA Method SW-846 data. The results obtained for 2,3,7,8-TCDD in the spiked BCD-
treated products are well outside the expected range, but this is due to the fact that.•:••••!• '%
the level of the added spike was too low considering the magnitude ^f unanticipated. •''•''
interferences from extraneous compounds in the sample matrix.
Representativeness and completeness of the samples-is 100 percent. All samples
obtained and analyzed were of appropriate size and volume, and all the measurements
obtained are judged valid. C •" " "
Detection limits obtained^.during this study are within the range acceptable for
determination of the treatability study objectives.
All laboratory blank samples analyzed had nondetectable concentrations of target
chemicals. Complete data packages including chromatographs for both the ATP and
BCD analyses are available upon request.
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4.0 ATP AND BCD FULL-SCALE TREATMENT ENGINEERING AND 0
ECONOMIC EVALUATION §
The purpose of this section is to evaluate engineering and economic issues relating
to full-scale ATP and BCD treatment of impacted material at the Vertac Site. This
evaluation is based on the data collected in the treatability study, and previous full-
scale treatment of polychlorinated biphenyls (PCB)-contaminated soils. As discussed
in Section 3.0, analytical data collected from the bench-scale tests demonstrate that
the ATP System and the BCD process were effective in removing contaminants from.^
test materials and destroying chlorinated compounds. :^://
This evaluation will assess full-scale engineering issyes related to combining the ATP••:;::/•
and BCD processes and issues specific to each processtechnoiogy. Specific elements
of this evaluation include: y..,.
• Integration of ATP and BCD technologies;^W :.
• Full-scale ATP operation issues;
• Full-scale BCD operation issues;
• Residual management;
• Regulatory requirements;
• Full-scale economics.
Each of these elements is addressed independently in this section.
4.1 ATP and BCD Full-Scale Process Integration
The ATP and BCD bench-scale treatability studies were conducted as separate tests
to demonstrate the effectiveness of each process on the materials subject to
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treatment. Although the tests were conducted independently, they are closely related °
because one of the products of the ATP tests (the contaminated organic condensate)
became the feed material for the BCD dechlorination tests. For full-scale operation,
the ATP and BCD technologies can be integrated in the same fashion as the bench
tests were integrated or in other ways. Four potential full-scale operation process
alternatives have been identified that integrate the ATP and BCD technologies.
Simplified process flow diagrams of these alternatives are presented on Figures 5
through 9 and are explained as follows:
Alternative A: This alternative is similar to the bench-scale testirigR.with relatively
independent ATP and BCD treatment steps (see Figure 5). For this
scenario, contaminants and carrier Qff'will be desorbed from the soil''•'.•'.•'''
utilizing the ATP system. The condensed oil and contaminants
generated from the ATP..$.ystem will be dechlorinated using a separateIX...
BCD reactor. Decontaminated oil from the BCD reactor and reaction
residuals wUI be recycled back to the feed end of the ATP unit as
carrier oil. Th'e only residuals requiring off-site disposal will be process
inventories remaining in the system at the end of the project and any
liquids (such as diesel oil) used for equipment decontamination.
Alternative B: This alternative includes integrated thermal treatment of soils and
dechlorination of contaminants within the ATP unit (see Figure 6).
This alternative is based on full-scale experience with PCB-
contaminated soils. Separate treatment of the condensed oil with a
BCD reactor, as presented in Alternative A, is not included. SoilTech
used a process similar to this to dechlorinate PCBs at the Wide Beach
Superfund Site. For this scenario, dechlorination reagents will be
added with a carrier oil directly into the ATP unit. Dechlorination of
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contaminants will occur within the ATP unit and the hot oil condensing 00
system. This process option provides an advantage in
decontaminating feed soils because both thermal desorption and
dechlorination of contaminants are occurring within the ATP unit.
Condensed carrier oil, along with fresh make-up oil replacing that lost
due to thermal cracking, will be recycled back into the ATP unit. Any
unreacted contaminants and the carrier oil would be "recycled to
extinction" meaning that the only residuals requiring off-site disposal
would be those remaining as process inventory at the end of the^
project, and liquids, such as diesel oil, used for equipment decontami-
nation.
Alternative C: This alternative includes dechlorination of contaminants within the
ATP unit as described f0.r Alternative B, and a separate BCD reactor'^i.••.•"'•'••••.:•.
for treatment of the ^condensed oil product as described for
Alternatiy&.:.A (see Figure 8). This alternative provides the advantages
of dechlorfiiating the contaminants within the ATP system and the
ability to further dechlorinate chemical contaminants (if necessary)
. /within the condensed oil before it is recycled back to the feed end of
the ATP unit.
Alternative D: For this alternative, dechlorination of contaminants utilizing the BCD
process is not included. The condensed oil generated from the ATP
system, which contains the contaminants, will be incinerated in an
approved incinerator (see Figure 9). While this alternative does not
directly destroy the contaminants, the ATP system concentrates the
contaminants and greatly reduces the overall volume of impacted
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material. This alternative is dependent upon access-to an incinerator 0
permitted to burn dioxin-contaminated wastes.
4.1.1 Full-scale Alternative Recommendation
Based on data collected from the bench-scale tests and full-scale experience with
treating PCB-contaminated soils. Alternative C has been recommended over the other
alternatives for further evaluation in this report. This alternative combines the ATP
and BCD process technologies that were demonstrated in the bench-scale tests. In,.
addition, this alternative includes dechlorination of contaminants- 'Within the ATP"^
system, which has been demonstrated on a full-scale basis for PCB-contaminated soil.
The recommendation of Alternative C is made base^-'on information available at thisV"
time. The collection of additional data may resultlin further evaluation of other
alternatives presented in this report. ...A;:,.i y'^.•:
Alternative A was not recommended because it does not include the dechlorination•<:;. V
••;:.•.•••••::..
of contaminants within the:;ATP unit which, as demonstrated full-scale, could enhance
the overall process. Alternative B, which is potentially feasible based on
dechlorinatton.bf PCB soils, was not selected because the bench-scale tests did not
specifically demonstrate dechlorination within the ATP unit. Alternative D was not
selected for further evaluation because incineration is not a preferred process option
over BCD dechlorination, and an approved incinerator for dioxin-contaminated material
will be required.
4.1.2 Full-Scale ATP and BCD Process Description
The full-scale evaluation for the ATP and BCD integrated process is based on the
SoilTech 10-ton-per-hour (tph) system. A 5-tph ATP system is also available and can
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24 2>000be evaluated, if required, depending on the quantity of material requiring treatment.
Figure 9 shows a simplified process flow diagram of the 10-tph ATP system with BCD
dechlorination. For this integrated process, BCD reagents and recycled BCD treated
condensed oil will be added directly into the ATP unit. The reagents and condensed
oil (carrier oil) will be thoroughly mixed with the contaminated soils within the ATP
unit to enhance the dechlorination reaction. The carrier oil provides a medium for
dispersion of reagents, and for recovery of unreacted contaminants. The ATP unit
provides reaction temperatures up to 590°C, vigorous mixing through the ATP
rotation, and extended residence time through the ATP and the hot oil condensing,..:.•¥: "::-
system. A cross-section of the ATP unit is shown on Figure 10. Carrier oil, unreacted^y
contaminants, and any other hydrocarbons will be desorbed from the soil in the ATP
unit and condensed, such that they can be mixed ..wfth additional BCD reagents forV'
treatment in a heated BCD reactor. %^
•t ...V.A...
The ATP provides temperature, residence time, and mixing which promote the
dechlorination reactions, ...however, the solid-vapor reaction kinetics in the ATP are•••''<, '•::••••:.•.••:--::..likely to be less favorable than demonstrated in the bench-scale BCD tests. Because
of this, the BCD reactor is likely to be an important element of the treatment train.
Treatment of the condensed oil in the BCD reactor will further destroy chlorinated:'.•''
compounds. The treated condensed oil and other BCD treatment residuals will be
recycled to the feed end of the ATP unit virtually eliminating off-site disposal of
residuals.
4.2 Full-Scale ATP System Evaluation
This section discusses the bench-scale data relative to operations of the 10-tph
SoilTech system. The results of the bench-scale tests demonstrate that the ATP
system can effectively treat contaminated materials from the Vertac Site, as
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represented by the samples submitted. Material characteristics meriting special
consideration, or affecting optimum full-scale treatment, are addressed in this section.
Primary feed characteristics affecting SoilTech ATP system full-scale treatment
include:
1 . Moisture content;
2. Particle size;
3. Hydrocarbon content;
4. Material handling characteristics;
5. Chemical characteristics. ^ \.:::••'
These characteristics affect full-scale ATP system o.^eration directly and/or affect the'A::-'''
materials handling and safety requirements of the operation. A discussion of each of
these five primary feed characteristics4s. provided below followed by a discussion of^^•-..
full-scale treated material characteristics aihd treatment costs.
4.2.1 Moisture Content :i.,
Feed moisture, content is a key parameter related to plant throughput, and therefore,
to the unit price of treatment. Ideal moisture content in feed material is in the range
of 5 to 10 percent. At lower moisture content, entrained dust can create problems
in the preheat vapor condensing system. The dust can cause difficulties in maintaining
correct pressure profiles in the internal zones while operating the condensing
equipment cleanly. At moisture contents above 10 percent, the latent heat of
vaporization required to volatilize the moisture from the feed in the preheat zone of
the ATP system becomes a bottleneck, resulting in reduced feed capacity.
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The two soil samples from the Vertac Site had moisture contents of 1 1 . 4 percent and <^0
5.5 percent. A blend of the Vertac Site soils might therefore result in a moisture
content less than 10 percent. Even if the higher moisture content soil were processed
alone, no appreciable reduction in throughput of the full-scale SoilTech ATP system
is envisioned. The spent carbon sample contained 34.3 percent moisture. The best
strategy for treatment of the carbon will be to blend it with the soils prior to
processing so that the moisture content of the feed material is maintained at or below
10 percent. Provided that this objective is achieved, the SoilTech ATP system
throughput will not be limited by moisture content.
'"t.4.2.2 Particle Size
For the SoilTech ATP system to operate at full capacity, less than 40 percent of the
solids to be processed should pass a 2QQ-mesh screen. For the soil sample from Grid..•.•::::;:...
152, 37.6 percent passed 200-mesh, vtr.hich suggests that no throughput limitations
should be experienced. T.he second soil sample (Grid 419), however, contained a
more significant proportion of fine material, with almost 50 percent passing the 200-
mesh screen. If a site representative blend of soils contains more than 40 percent
below 2o6::;imash, then it is likely that throughput could be adversely affected. Some
co-feeding of coarser material may be necessary to provide the required proportion of
particles greater than 200-mesh. This will ensure that the sand seals operate properly
and that efficient heat transfer is achieved between the cooling and preheat zones.
Optimum operation of the SoilTech ATP system might require limiting waste through-
put to 6 to 8 tph while co-feeding coarse material.
In addition to fine material, particle size is required to be less than two inches in
diameter.
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I>00No particles larger than two inches were found in any of the test samples. This °0
indicates that pre-screening and/or crushing prior to processing will not be necessary,
unless larger particles are encountered at the site.
4.2.3 Hydrocarbon Content
The low concentrations of hydrocarbons present in the test samples indicate that a
carrier oil must be added to the feed material for efficient operation of the ATP
System vapor handling equipment. This will probably be one percent or less of the..
wet feed rate. It will be possible to recycle treated oil from the BCD^process for this•w
purpose. Costs associated with the purchase of clean oil and the disposal of treated
oil from the BCD process will thus be minimized. ...; ^
4.2.4 Material Handling Characteristic-W%-j^
Based on observations made on the feed samples, no material handling difficulties are""hA
anticipated. Canonie, however, suggests that the spent carbon be mixed with site
soils to main.lt.ain a constant moisture and BTU content of feed material.
The combusted solids are dusty and contain fine material. The SoilTech ATP system
configuration includes a mechanism to quench, moisten, and neutralize (if necessary),
the treated solids. Quenching the solids will eliminate the potential for fugitive dust
emissions from the SoilTech ATP system.
TCLP analyses of the combusted soil samples for metals, semivolatile organics, and
chlorinated herbicides indicate that further processing of the soil after ATP system
treatment is not necessary.
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The two soil samples did not exhibit any unusual reactivity or corrosivity. No organic
vapor was detected above either soil sample at ambient temperatures in the head
space of the shipping container. Above the spent carbon sample, 14 ppm organic
vapors were detected which indicates that caution should be exercised when handling
this material.
The presence of 2,3,7,8-TCDD and other contaminants at the Vertac Site will require.
consideration in the treatment work plans and safety plans. Site-specie requirements^
concerning the handling and processing of dioxin-contaminated soils will have to be
defined for full-scale operation. •iy^
4.3 Full-Scale BCD Process .r^;<••'•
This section evaluates fu-U^cale implementation of the BCD process. The analytical•'•^.•y^:
data collected from the treatability test indicate that all chemicals of concern were
destroyed t%, nondetectable levels in the treated reaction mixture. As discussed
previously/deiehlorination utilizing the BCD process can be conducted within the ATP
system and/or separately in a BCD reactor. Full-scale implementation of the BCD
process within the ATP system requires adding BCD reagents directly into the ATP
unit. The quantity of reagents required for full-scale BCD dechlorination within the
ATP unit can be estimated based on the bench-scale tests and optimized during full-
scale operation. Bench- or pilot-scale testing could also be conducted to further
evaluate dechlorination within the ATP unit and optimization of BCD reagent
requirements.
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Dechlorination utilizing a separate BCD reactor will require designing and constructing S3
a full-scale reactor. In Australia, a 500-gallon full-scale liquid reactor utilizing the
BCD process has been constructed and operated for treating oil contaminated with
PCBs and pesticides. The BCD reactor design and reagent additions are two primary
issues involved in scaling up the bench-scale process which are discussed in the
following sections.
4.3.1 Full-Scale BCD Reactor
A BCD reactor skid will be required for integration with the ATP systeTn. The skid will•?'••''
include the BCD reactor and associated reagent feed and mixing systems and other
auxiliary equipment. Important design parametersfTnclude safety (particularly fireV'
protection), the volume of the reactor (i.e., residence me), mixing capabilities of the
reactor, reactor heating and temperatu:fe control, the material used to construct the
reactor, and reactor venting, ?;.-
The size and/or number o.f Teactors will be based on the estimated volume of oil
condensate ... generated from the ATP system, the quantity of reagent addition
required, and/the estimated residence time required to dechlorinate chemicals of
concern. Assuming a maximum feed rate of 8 tph using the 10-tph ATP, with a 1
percent oil addition to the feed and 70 percent recovery of feed oil, approximately 1 1 0
pounds per hour of oil-based condensate will be generated. Therefore, a reactor
volume of at least 150 gallons is required considering reagent addition and a 4-hour
residence time. A larger reactor or multiple reactors would allow flexibility in the
integration of the technologies. The bench-scale tests conducted achieved
nondetectable concentrations of chlorinated compounds within four hours based on
the intermediate sample.
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The reactor will be designed so there is adequate mixing of the oil condensate and 0
BCD reagents. Mixing will also enhance uniform temperature throughout the reaction
mixture. The reactor will be designed to maintain a reaction temperature of
approximately 320°C to 350°C based on the BCD bench-scale tests.
The reactor will be constructed of a high-strength, corrosion-resistant metal alloy.
The bench-scale BCD reaction mixtures were highly corrosive due to the addition of
sodium hydroxide with a pH greater than 10.
.•:-<'The BCD reaction will be conducted under atmospheric conditions with the reactor
^vented to the ATP's preheat vapor recovery system. Condensed water vapor, if any,
will be separated and sent to a water treatment system.•<^^
4.3.2 Reagent Addition for Full-Scal&sBCD Reactort^-j^
For the BCD bench-scales-tests, the following reagents were added to the reaction"W^.
vessel. Weight percentages" of the total reaction mixture are as follows:
1 .5 percent
22.0 percent
29.0 percent
14.5 percent
33.0 percent
100.0 percent
Solid'Catalyst•.'"
Sodium Hydroxide
High Boiling Oil
Liquid Catalyst
Test Sample
As a result of adding the above reagents, the total reaction mixture was approximately
three times the weight of the original test sample. While this reagent addition is
feasible for full-scale operation, the use of less reagents would be desirable.
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Specifically, since the condensate generated from the ATP system consists of a high ^
boiling oil, reducing the amount of new make-up oil to the BCD reactor may be
feasible. Reagent addition could be optimized during full-scale operation or through
BCD bench/pilot-scale tests.
4.4 Full-Scale Treatment Residuals Management
The primary treatment residuals generated from full-scale operation of the ATP system
with integrated BCD dechlorination include treated solids, oil condensate and BCD
reaction residuals, flue gas, spent carbon, and wastewater. As discu-ssed previously,'.&•••
the oil condensate and BCD reaction residuals will be recycled to the feed end of the
ATP system. ..:; ::
The 10-tph ATP's flue gas exhaust raters approximately 5,500 acfm, which is about
12.5 percent of the emission rate of anUncinerator with equivalent solids processing
capability. The flue gas will be processed through the ATP system emissions control
system which consists of a cyclone separator, quench system, fabric filters, and
carbon adsorption beds. Spent carbon generated from the emissions control system
will be mixed .with feed material and processed through the ATP system.
Wastewater generated from the vapor recovery system will be treated by an on-site
water treatment system. Based on the moisture content of the Vertac Site material,
less than 5 gallons per minute (gpm) of condensed water will be generated from the
ATP system. After treatment, this water can be used to quench and moisten the
treated solids.
The only residuals requiring disposal or further treatment will be process inventories
remaining in the system at the end of the project. This includes any liquids (such as
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diesel oil) used for equipment decontamination. It may be possible to minimize the Q
quantity and toxicity of residuals by using the BCD reactor to dechlorinate liquids
used for equipment decontamination. The determination of disposal or treatment
requirements for these residuals will need to be evaluated based on regulatory
requirements established for the Vertac Site.
4.5 Regulatory Issues and Permitting
The primary regulatory issues for full-scale operation include the establishment of soil...
treatment standards, air emission standards, wastewater discharges::standards, and
requirements for disposal of treatment residuals remaining at the end of the project.
While the ATP system bench-scale tests demonstrated that concentrations of
chemicals of concern in the contaminated soil could be reduced to nondetectable
levels in most cases, nondetectable colncehtration levels are not practical as a full-
scale treatment standard,.....Soil treatment standards need to be established that can
be achieved by the full-sc-aje system on a high confidence level and can be verified
quickly by on-site analytical methods. For example, treatment standard for 2,3,7,8-
TCDD is expected to be 1 ppb or higher.
Applicable air emission standards and requirements must be adhered to during
operation of the ATP system. Because contaminants are thermally desorbed from soil
before the soil enters the combustion zone of the ATP, the flue gas is suitable for
discharge to the atmosphere after passing through the emissions control system
previously described. In previous full-scale operations at the Waukegan Harbor
Superfund Site and the Wide Beach Superfund Site, the ATP System has met
stringent permit requirements established for treating Toxic Substance Control Act
(TSCA)-regulated soils and sediments.
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As discussed in Section 4.4, less than 5 gpm of treated wastewater will be generated. Q
This water will be used to quench and moisten the treated solids, eliminating the need ^
for off-site discharge.
Treatment residuals remaining at the end of the project will require on-site or off-site
disposal. If any of the residuals contain dioxins, off-site disposal of the residuals may
not be feasible due to the lack of approved treatment or disposal facilities.
4.6 Economic Evaluation
The results of the treatability study indicate that optimum full-scale treatment of
Vertac Site material would be best accornplished,:::tnrough integration of the ATP•;;:;;••"•
technology and BCD technology as described above, .i Specifically, the waste would
be processed in the ATP with the addNpn of BCD reagents, and desorbed reaction
residuals would be transferred to a BCO..: reactor for additional treatment. Residuals
from the BCD reactor would,, be recycled through the ATP. This treatment train, when:::: :A:..
properly operated, would r;esu It in virtually no net residuals for off-site disposal due
to the ATP's.abiiity to thermally crack and consume a fraction of the simple straight
chain hydrocarbons in the soil. This treatment train is very similar to the treatment
train used at the Wide Beach Superfund Site. The potential costs of full-scale
treatment using an integrated ATP and BCD process are discussed in this section.
The costs described in this section are related specifically to the combined ATP and
BCD process. They are based on the results of the ATP treatability tests, SoilTech's
full-scale experience, and extrapolation of the BCD treatability tests. The economic
evaluation has been completed assuming the project could be completed within the
same quality assurance and health and safety framework as SoilTech's previous
Superfund projects involving contaminants regulated under the TSCA. This last
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assumption is necessary because it is difficult to define, at this stage of the ~
evaluation, what quality assurance and health and safety requirements might be
required for a project involving dioxin-impacted material. This assumption provides
a baseline definition of probable treatment costs within a known regulatory
framework.
The economic evaluation assumes use of a 10-tph ATP system. Figure 1 1 relates
typical treatment costs (thermal desorption only) as a function of the quantity of
material to be treated and size of ATP equipment used for treatment. This figure has..^
been developed based on full-scale experience treating PCB-impaeted soils. As.y
indicated, for projects between 7,000 and 36,000 tons, a 10-tph ATP is typically
most economical. Described below are the fixed aarf^ariable costs associated withV-
treatment of material from the Vertac Site, as well as^critical assumptions relative to
the treatment costs, ^..y .^Fixed Costs ,
Fixed costs a.re the costs associated with initiating and concluding the project. They
include preparation of project work plans and project permits, mobilization of
treatment equipment, erection of treatment equipment, startup and shakedown of the
equipment, "proof-of-process," decontamination of treatment equipment, and
demobilization of the treatment equipment. Fixed costs for this project are estimated
to be $ 1 . 5 million to $2.0 million. This component of the project cost could be
extremely sensitive to the quality assurance requirements necessary for the projectin regard to project permits and "proof of process."
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Variable Costs
Variable costs are the costs associated with operation of the treatment system after
the successful conclusion of the "proof-of-process" through the completion of the soil
treatment. Variable costs are incurred on a per-ton basis. For the Vertac material,
variable costs include the cost of labor, utilities, equipment depreciation, subcontract
services, and supplies for the operation and maintenance of the combined ATP and
BCD treatment equipment, as well as any minor residual material disposal.
..Variable costs for treatment of the Vertac material are estimated to be:: $275 to $325
';::.••per ton. Again, this price is sensitive to quality assurance and health and safety
requirements of the project. These costs are "hopper-lio-hopper." The costs assume
the untreated material is provided to SoilTech in a stockpile adjacent to the feed
equipment of the ATP. It also assumes-^e treated material will be removed from thes,. :....
ATP discharge stockpile by others. ;;;.-
The variable costs described-above include operation of the BCD equipment in the
treatment trajn. The component of the variable costs associated with the BCD
technology is,/$70 to $90 per ton of material treated. This cost includes the
depreciation on the BCD capital equipment (including reactor design) and the labor,
reagents, and utilities required to operate and maintain the equipment.
Critical Assumptions
In order to estimate costs for treatment of the Vertac material, several critical
assumptions were made. These assumptions were necessary because the scope of
work is not defined and the project quality assurance criteria are not defined. These
assumptions include the following:
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1 . Costs are for "hopper-to-hopper" treatment of soils. Untreated soil is to be °^NB?
provided in a stockpile adjacent to the feed equipment.
2. The BCD equipment can be scaled up directly from the bench-scale work to
full scale.
3. Treatment equipment operating personnel can work in Level C personal
protective equipment.
..'.' •;•
4. Treatment criteria for 2,3,7,8-TCDD is 1 ppb or higher.
5. Routine confirmation of treatment criteria^an be accomplished on-site onV-
24-hour turnaround by a laboratory equipped with a gas chromatograph.
6. "Proof-of-process" will be coi|i.du'cted following TSCA guidelines one time
only at the onset.pf the project.^w^^
The costs described in this section are inclusive of the scope of work SoilTech would
execute during combined ATP and BCD treatment of the Vertac subject material as
qualified by the assumptions.
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5.0 CONCLUSIONS AND RECOMMENDATIONS
<..037 -.•)
r*»C500
This section presents conclusions and recommendations based on the results obtained
from the ATP and BCD bench-scale results. The recommendations presented herein
are based on full-scale experience in operating the ATP system and associated bench-
scale tests.
As presented in Section 3.0 of this report, the analytical results indicate that the ATP
system and BCD process are effective technologies in removing and/or destroying.;.:••••;:.
chemicals of concern recognized at the Vertac Site. The majority of target^
contaminants were reduced to nondetectable concentration levels in the treated soil
and organic-phase condensate generated from the A-TP bench-scale system.::;:::.-'-" ..:.
Based on the data collected, a full-scale;:&ystem is recommended which integrates theIX...
SoilTech 10-tph ATP system with the ^CTD dechlorination process. This full-scale
ATP system (identified as-Alternative C in Section 4.0 and represented by Figures 7
and 9) includes introducing,.BCD reagents directly into the feed end of the 10-tph ATP
unit and a separate BCD reactor. Dechlorination of target contaminants will take place
in the ATP'^-unft and in the separate BCD reactor. Initial full-scale operation would
reflect the following operating parameters:
1 . The SoilTech ATP system would be initially operated at an average rate of
approximately 6 to 8 tph. This throughput rate was conservatively
established based on the soil fines content identified in the feed soil
samples.
2. A high boiling carrier oil will be added to the feed end of the ATP unit. The
amount of oil will be approximately 1 weight percent of the wet feed rate.
PR/W:t»2-22B/TREAT.RPT (February 23, 19831
CanonieEnvironmental
38 ?.,,,JE>o
The carrier oil will be added for three purposes: 1 ) To insure efficient 00
operation of the ATP's vapor recovery system, 2) to act as a carrier oil for
the desorbed contaminants, and 3) act as a hydrogen donor compound in
the BCD reaction.
3. Reagent additions for the BCD reactor will be directly scaled up from the
bench-scale tests.
4. The BCD reactor will be operated at reaction temperatures ranging from
320°C to 350°C. ^V
Enough data and information is currently available to^frnplement this system on a full-
scale basis. It is recommended that a soil treatment objective of 1 ppb or higher for
2,3,7,8-TCDD be considered for fuife-scale operation. While the bench testsIX...
demonstrated results superior to this obfective, a more stringent objective is not
practical to consistently .achieve and verify lower treatment standards in the short
timeframe required in full-scale production. During the start-up phase, process
optimization will be required to better define the following operating parameters for.-.- •'•"•'•:'...'•''•\
full-scale operation:
1 . Optimum throughput of contaminated feed material through the ATP system
to consistently achieve the established soil treatment standard;
2. Quantity of BCD reagents fed directly into the ATP unit;
3. Quantity of BCD reagents used for the BCD reactor.
PR/W;/92-229/TREAT.RFT |F»bru*ry 23. 1 9931
CanonieEnvlronmentdl
•~0f-':!
39 00
Further testing could also be conducted to better define optimum BCD treatment 0
parameters required to successfully dechlorinate target compounds. Two areas that
would be investigated further that could provide useful information for full-scale
operation include:
1 . Conduct tests that quantify the extent of dechlorination of target
compounds within the ATP unit to allow optimization of the quantity of BCD
reagents required.
....•2. Conduct additional BCD tests on organic-phase condensatei::generated from
. ••"the ATP system to optimize the BCD reactor operating conditions
(temperature, residence time, reagent concentration, etc.).':;:;;••"•y
Since a larger quantity of impacted soi^ould be required to conduct the above tests,'•'•: .••.••'''''•>.:•.
it is recommend that a "pilot-scale" system be installed at the site. The "pilot-scale"
system would consist ofSoilTech's bench-scale ATP system and a larger BCD reactor.
The bench-scale ATP system is skid-mounted and could be transported to the Vertac
Site. However, as an alternative, the tests could possibly be conducted at SoilTech's
laboratory operated by Hazen in Golden, Colorado depending on the quantity of soil
required. Canonie estimates the cost of conducting the pilot-scale tests could range
from $200,000 to $500,000 depending on the scope of the tests.
The full-scale economic evaluation presented in Section 4.6 assumes the use of a
10-tph ATP system. Fixed and variable costs are estimated for the Vertac Site based
on several critical assumptions. Fixed costs for the project are estimated to be
$1 .5 million to $2.0 million. This component of the project cost could be extremely
sensitive to the quality assurance requirements necessary for the project in regard to
project permits and "proof-of-process".
PR/W:/92-229/TREAT.RPT IFebruw 24, 19931
05CO
40 r*.00
Variable costs for treatment of the Vertac site material are estimated to be $275 to ®
$325 per ton. These costs are "hopper-to-hopper". The costs assume the untreated
material is provided to SoilTech in a stockpile adjacent to the feed equipment of the
ATP. It also assumes the treated material will be removed from the ATP discharge
stockpile by others.
PR/W:/82-229/TREAT.RIT IFfbruwy 23, 18831
0REFERENCES -?
2>0
Canonie Environmental Services Corp., 1992a, "Quality Assurance Project Plan, °DechlorinationTreatability Study, Vertac Site. Jacksonville. Arkansas," October 1992.
Canonie Environmental Services Corp., 1992b, "Work Plan, DechlorinationTreatabilityStudy, Vertac Site, Jacksonville. Arkansas," October 1992.
LIST OF TABLES
TABLENUMBER
2
3
4
TITLE
Summary of Retort Test Mass Balances forATP Treatability Study Samples
Summary of Combustion Test Mass Balancesfor ATP Treatability Study Samples
Summary of Physical and Chemical AnalysesConducted for ATP and BCD TreatabilityStudies \..
Solids Analytical Results Summary, ATPSystem Benc .r-.Scale Tests
VCombustion Solids TCLP Analytical Results,' P Dechlorination Bench-Scale Tests
Condensate Aqueous and Solid Fractions -Analytical Results, ATP System Bench-ScaleTests
BCD Bench-Scale Tests Analytical Results
PR/W:/92-229/TREAT.LOT [Februwy 24. 19931
CanonieEnvironmental
TABLE 1
SUMMARY OF RETORT TEST MASS BALANCESFOR ATP TREATABILITY STUDY SAMPLESDECHLORINATION TREATABILITY STUDY
VERTAC SITE, JACKSONVILLE, ARKANSAS(Weights in grams)
Grid 152 #1 - 1 , 1 0 0 Degrees FGrid 152^1 -1,000 Degrees F
Grid 152#2 -1 ,100 Degrees FGrid 152#2 -1,000 Degrees F
Grid 4 1 9 - 1 , 1 0 0 Degrees FGrid 419 -1,000 Degrees F
Spent Carbon - 1 , 1 0 0 Degrees FSpent Carbon -1.000 Degrees F
VirginFeed
1,006.71,006.6
2,007.62,019.3
:; ''::-.•;: ..:••'•':<•..
1,004.81,001.3
1,012.04.012.9
Input
Silica N
999.01,000.2
1,001.11,020.4
1,005.81,008,3
1,004.91,006.8
lineral Oil
35.634.1
66.666.1 ^
::• .::•••33.9 .33.2
35.133.4
CokedSolids C
1,897.41,883.0 :.
":::
T2,705.1 2,749.6
1,873.91,909.9
1,600.51,604.1
OutputLiquid
;ondensates
147.7667.9
296.2313.9
93.879.1
310.4298.9
Producedt^Gas
^12.315.5
29.421.5
28.418.2
44.142.7
BalanceClosure (Percent) (a)
100.7125.7
98.699.3
97.698.3
95.394.8
Note:(a) Balance closure calculated on a total input basis.
CanonleEnviPR/W:/92-229/TREATTB1 .XLS [2/23/93]
TABLE 2
SUMMARY OF COMBUSTION TEST MASS BALANCESFOR ATP TREATABILITY STUDY SAMPLESDECHLORINATION TREATABILITY STUDY
VERTAC SITE, JACKSONVILLE, ARKANSAS
(Weights In grams)
Retort Combusted ^BalanceSample Source Charge Solids ClosWe (Percent)
v-y-'
Grid 152 50:50 Mix of Grid 152^11,000 and 1,100 Degrees F Trials 1,000.6 1;ia08.6 100.7
I-
- Grid 419 50:50 Mix of Grid 419 l'1,000 and 1,100 Degrees F Trials 1 ,Ol|"J::::-: 999.8 98.9
•'•: .::
000743CanonieEnvircnmental
PR/W:/92-229/TREATTB2.XLS [2/23/93]
TABLE 3
SUMMARY OF PHYSICAL AND CHEMICAL ANALYSIS
CONDUCTED FOR ATP AND BCD TREATABILITY STUDIES
VERTAC SITE, JACKSONVILLE, ARKANSAS
Source Sample 1.0.
Sample Description
Grid 152
ATP Feed Solids
Retort ( 1 . 1 OOF) Solid*
Retort 11.OOOF) Solid*
Combuttion Solid*
Grid 419
ATP Feed Solid*
Retort (1.100F) Solid*
Retort d.OOOFf Solid*
Combuttion Solid*
Spent Carbon
ATP Feed Solid*Retort (1.100F) Solid*
Retort 11.000F) Solid*
Condensate
Solid Phase
Aqueou* Pha«e
Trial 1
BCD Feed
Intermediate BCD
Final BCD
Trial 2
BCD Feed
Intermediate BCD
Final BCD
Trial3
BCD FeedIntermediate BCD
Final BCD
Physical Analyci* Chemical Analyci*
Grain Size Moisture Ach Dioxin |c| Herfaicide* (d) Polychlorinatod Tatra- TCLP«)
Dittribution (a) Content (b) Content phenol* |e| chlorobenzene Ie) SVOC* | 6 RCRA Metal* | Chlorinated Herbicide*
• • • • • • •
• • • •
• • • •
• • • • • • • • • •
• • • • • • •• • • • -v• • • • ^
• • • • • • • • ..;•:•"' • •
• • • • • ••:;: •
• • • '•;:; •• • • .$•••'• •
•f .
• • / K. • •
• • A.-' • •
'•,:*•'••:• • • ••:<n • • • •• • • 1
";: '::::.::: ..y
• • 1 •
• • 1 •
• • • •
• • • •
• • • 1
• • • •
Note*:
a) ASTM D 422.
h} Gravimetric method at 105 degrees celcius for 16 hoursc) Modified EPA Method 8280.
d| Modified EPA Method 8150.
e| Modified EPA Method 8270.
f| Extraction by EPA method 1 3 1 1 , analycic in accordance with USEPA SW 606, third edition.
rfVW /62 2»/SUMItCT XIC
_ 00074.1CailOHteEnvircni'nenlal
TABLE 4
SOUDS ANALYTICAL RESULTS SUMMARY
ATP SYSTEM BENCH-SCALE TESTS
DECHLORINATION TREATABIUTY STUDY
VERTAC SITE. JACKSONVILLE, ARKANSAS
Source Sample 1.0.
Sample Description
Analyte
Dioxin (ppb) 2,3.7,8 TCDD
Herbicides (ppm) 2,4-D2,4,5-TSilvex
Polychlorinated phenols Mono-(ppm) Di-
Tri-
Tetrachlorobenzene (ppm)
Grid 152 Soil
ATP Feed
Solids
293
0.1ND (0.03)NO (0.03)
ND (0.5)ND (0.3)ND(1.0)
ND (0.15)
Retort (1.000F)
Solids
ND (0.0087)
ND (0.005)ND (0.01)ND (0.01)
ND (0.1)ND (0.02)ND (0.08)
ND(0.01)
Retort (1,1 OOF)
Solids
ND (0.0014)
ND(0.01)ND (0.02)ND (0.02)
ND(0.1)ND (0.02)ND (0.08)
ND (OBI).
Combustion
Solids
ND (0.0010)
ND (0.005)ND (0.01)ND(0.01)
ND (0.2)ND (0.02)ND (0.08)
ND(0.01)
Source Sample 1.0.Sample Description
Analyte
Dioxin (ppb) 2,3,7,8 TCDD
Herbicides (ppm) 2,4-D2,4,5-TSilvex"
Polychlorinated phenols Mono- •(ppm) Di-
Tri-
Tetrachlorobenzene (ppm)
. Grid 419 SoilATP Feed
Solids
8t2.
2.i-
2823
9.56.796
55
Retort-:(1 ,OOOF)
SoliW
0.0534
ND (0.005)ND(0.01)ND (0.01)
ND (0.1)ND (0.02)ND (0.08)
ND(0.01)
Retort (1,1 OOF)
Solids
0.007
ND (0.005)ND(0.01)ND(0.01)
ND (0.1)ND (0.02)ND (0.08)
ND(0.01)
Combustion
Solids
ND (0.0019)
ND (0.005)ND (0.01)ND (0.01)
N0(0.1)ND (0.02)ND (0.08)
ND(0 .01)
Source Sample I.D.Sample Description
AnalyteDioxin (ppb) 2,3,7,8 TCDD
Herbicides (ppm) 2,4-D2,4,5-TSilvex
Polychlorinated phenols Mono-(ppm) Di-
Tri-
Tetrachlorobenzene (ppm)
Spent CarbonATP Feed
Solids
0.446
721
459
1603250 .1300
50
Retort (1,OOOF)
Solids
0.0805
ND (0.01)
ND(0.01)ND (0.01)
ND (0.2)ND (0.04)ND(0.1)
0.12
Retort (1.100F)
Solids
ND (0.0296)
ND (0.01)ND(0.01)ND(0.01)
ND (0.1)ND (0.02)ND (0.08)
0.04
ND= Not Detected - Detection limit in parentheses
PR/W:/92-229/TREAT4-7.XLS [2/23/93]
TABLES
COMBUSTION SOUDS TCLP ANALYTICAL RESULTSATP SYSTEM BENCH-SCALE TESTS
DECHLORINATION TREATAB1UTY STUDYVERTAC SITE, JACKSONVILLE, ARKANSAS
0'"315>C-50®
Source Sample I.D.Sample Description
Analvte
TCLP SVOCs (ug/1)
TCLP 8 RCRA Metals (mg/1)
TCLP Chlorinated Herbicides (ug/1)
Grid 152 SoilCombustion
Solids
ND (20-100)
ND (0.02-5)
ND (17-120)
Grid 419 SoilCombustion
Solids
ND (20-100)
ND (0.02-5)•'•'•.
NDO?-!^)
PR/W:/92-229/TREAT4-7.XLS [2/23/93]
TABLES
CONDENSATE AQUEOUS AND SOUD FRACTIONSANALYTICAL RESULTS
ATP SYSTEM BENCH-SCALE TESTSDECHLORINATION TREATABIUTY STUDY
VERTAC SITE, JACKSONVILLE, ARKANSAS
Sample DescriptionAnalvte
Dioxin (ppb) 2.3,7,8 TCDD
Herbicides (ppm) 2,4-D2.4.5-TSilvex
Polychlorophenols Mono(ppm) Di
Tri
Tetrachlorobenzene(ppm)
Solid Phase
4,890
2,10044531
12,20040,8008,600
..•.•••:;rise-
^.•''•'
Aqueous Phase
5.6
275.70.8
2,12TC'680 :!/44
0.8
PR/W:/92-229/TREAT4-7.XLS [2/23/93]
TABLE 7
BCD BENCH-SCALE TESTS ANALYTICAL RESULTSDECHLOR1NATION TREATABIUTY STUDY
VERTAC SITE, JACKSONVILLE, ARKANSAS
CO-T*S>000
Source Sample 1.0.Sample DescriptionAnalyte
Dioxin (ppb) 2,3,7,8. TCOD
Herbicides (ppm) 2.4-02,4,5-TSilvex
Polychlorinated phenols Mono(ppm) Di
Tri
Tetrachlorobenzene (ppm)
BCD Feed
3,520
1,05019415
45.00046.0006,670
510
Final BCD
N0(0.184)
ND (0.08)N0 (0.04)ND (0.04)
N0 (120)N0(20)ND (25)
ND (0.2)
Trial 1Intermediate BCD
ND(0.534)
NO (0.04)NO (0.07)NO (0.04)
N0(200)NO (45)N0(75)
ND (0;$
Source Sample I.D.Sample DescriptionAnalvte
Dioxin (ppb) 2,3,7,8, TCDD
Herbicides (ppm) 2,4-02,4,5-TSilvex
Polychlorinated phenols Mono(ppm) Di .,..••;•..
Tri '•i:.:-.-'- :;.
Tetrachlorobenzene (ppm)
BCD Feed
4,060
1,150,.1:g8
il ,.^
30,00030,5008,300
680
Final BCD
..•A,
ND- ,258)''^..
ND (0.03)ND (0.04)ND (0.03)
ND (250)ND (80)ND (80)
ND (0.8)
Trial 2 ••?'Intermediate BCD
ND (0.223)
ND (0.03)ND (0.02)ND (0.02)
ND (100)ND (15)ND (25)
ND (0.2)
Source Sample: I.D..:
Sample DescripHonAnalyte
Dioxin (ppb) 2,3,7,8, TCDD
Herbicides (ppm) 2,4-D2,4,5-TSilvex
Polychlorinated phenols Mono(Ppm) Di
Tri
Tetrachlorobanzene (ppm)
BCD Feed
3,810
94020916
37,40046,7007,400
450
Final BCD
ND (0.188)
ND (0.3)ND (0.70)ND (0.10)
ND (100)ND (15)ND (20)
ND (0.2)
Trial 3Intermediate BCD
ND (0.152)
ND (0.03)ND (0.07)ND (0.04)
ND(150)ND(30)ND (35)
ND (0.4)
N0= Not Detected - Detection limits in parentheses
PR/W:/92-229/TREAT4-7.XLS [2/24/93]
FIGURENUMBER
1
2
3
4
10
1 1
DRAWINGNUMBER
92-229-A11
92-229-E12
92-229-A13
92-229-A14
92-229-A15
92-229-A16
92-229-A17
92-229-A18
92-229-B20
92-229-A21
92-229-A19
LIST OF FIGURES
TITLE
Site Location Plan
Sampling Location Plan
Diagram of Bench-Scale ATP Unit
Wright State University BCD Bench-ScaleReactor ,<^
Alternative 'A', Contaminated Solids Treatment
Alternative 'B^.Contaminated Solids Treatment
Alternative 'C', Contaminated Solids Treatment
Alternative 'D', Contaminated Solids Treatment
Simplified Flow Diagram with Dechlorination,SoilTech ATP System
Cross Section, SoilTech ATP System
Evaluation of Optimum Size ATP Unit
PRyW:/«2-229/TREAT.LOT IF«bfU*rv 24, 19931
SURFACE SOIL SAMPLELOCATION IN GRID 4 1 9
I i 1
UCEUD;...—.— FENCE
. . . . RAUtOAO
- PBOPEWTY UNf
——— ——— CREEK
C^3 BUHDINC Oft FOUNMrKW
V9 SAMPLE LOCATION
—^——. . PBOODC11W AHE*
————. ccNrfWi. process *w* BOUHOARY
DRAFT
I'.^UI / HlvhHtN
SAMPLING LOCATION PLAN
OECHLORINATION TREATABILITY STUDY
PHEPWCO ros
HERCULES INCORPORATED
CanonieEnvironn i -ltd 1^SSSB3SE
r^
5
0)CMCM
1CM0)
0 Q:
2 bJS m
< 30: =>0 Z
t;
1
<
A
No
-— -«
DATE
VENT IINES TO EXHAUST
r -i ——^——i^—i l l 1 X1 | X"10^ 01)1 1 1 ^
, GAS | ( /} HLIU) \.COLLECTOR , •—/ TRAP (X^
| - ^ ^
L J<£)
<- |
nPRESSURE Q-SAMPLE yBOMB 5
frt
. T
-EGEND:
Q> SAMPLING LOCATIONS
< HDI 1 01WAII.R 1 HAILK /
, ! I TWAILH HiAIII H
MS
M A M
ISSUE / REVISION \wn B. CK'O Bi M-L) u.
•>
Q
¥
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rc
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^SECONDARY<\COOLER
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G>©
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DRY GASMETER
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BATCHPYROLYSIS
OR;OMBUSTION
UNrrPROCESSOR
^
SCRTEMP-
ERATURECONTROL
UNrr
-c-p
DlD
cDATE: 1-20-93
SCALE NONE
-1
TC-8 CHARCO/ FILTER
CARTRID
TC-5
/
ORIVEMOTOR
3
HIIROGENPURGE
CAS
OMPUTER ——t-
RINTER
(OPIIONAI)
AGRAMECHLOR
HERC
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^
c
MULTIPOINr CONDITIONER - OUIPUI - RECORDER
23456789101 11 21 31 415161 7181 9;0212223
^4- 11)
DRAFT2—25—93
OF BENCH SCALE ATP UNITNATION TREATABILITY STUDY
r'nri'ARFn FOR
;ULES INCORPORATED
nieEnvlroi imentdl-
- .r
•—11C-93SANO
5 PSI3 RUPIURE—1 AIR DISK
^AIR
»———————
EMERGENCERELEASE
WATERBATH
THERMOCOUIHERMOC011IHERMOCOUTHERMOCOUIHERMOCOUIHERMOCOUTHERMOCOUTHfRMOCOUTHERMOCOUTHERMOCOUIHERMOCOUTHERMOCOUTHERMOCOUTHERMOCOUSPARESPARECONDFNSAIECAS FLOW VGAS RATE -COMU GASCOMB GASCOMB GASSPARlSPARL;,
rir'i lor i 1 DRYING NUMBERFIGURE 5 J 92-229-A.1.5.
EXHAU5TFAN
r@7~\.-' VENT TOLABORATORYHOOD WITH
HEPA / CARBONHLIER
PLE - SHELI TEMP 1PIE - SHELI TEMP 2PLE - SHLII TEMP 3PLE - WAIL IEMP 1PLE - WALL TEMP 2PLE - HOT VAPOR ENT TEMPPLE - HOT SAND TEMP 1PLE - HOI SAND TEMP 2PLE - STA1 SAND TEMPPLE - VAPOR TO CONDENSERPLE - PRIM COND WATER TEMPPLE - CONDENSATE TEMP.PLE - SEC COND WATER TEMPPLE - WET GAS FINAL TEMP
BOTTIE PRI '-.SURE 'F<ATE - I'll.ll/'l
INIlLRAL IDMCIION (18 )ANAI »51S 1 1
ANAL»SIS - III
DEAN AND STARKRECEIVER
CONDENSER FORSOLIDS INLET
THERMOCOUPLESSYRINGE PUMP
DRAFT2—25—93
WRIGHT STATE UNIVERSITYBCD BENCH SCALE REACTOR
DECHLORINATION TREATABILITY STUDYPREPARED FOR
HERCULES INCORPORATED
CanomeEnvironmentalISSUE / REVISION ,'WN Hi cr.'D Hi "I'-D Bi
DATE- 1-20-93SCALE- NONE
FIGURE 4DRAWING NUMBER
^1
CONTAMINATEDSOILDS
SOILTECHm^p'^^SYSTEM;::
TREATED SOLIDS
MAKE-UPOIL
DECHLORINATIONREAGENTS
CONDENSEDOIL
^.QCD^^REACTOR::::
BCD TREATED OIL ANDREACTION RESIDUALS
DRAFT2-25-93
ALTERNATIVE •A'CONTAMINATED SOLIDS TREATMENT
DECHLORINATION TREATABILITY STUDYPREPARED FOR
HERCULES INCORPORATED
CanonieEnv iron mentalISSUE / REVISION IWN Hi .m Hi Al ' l )
DATE 1-20-93
SCALF- NONEFIGURE 5
BCD^ DECIILORINATION- REAGENTS< .———————————
0) _______^^_____________,CN |. .^.^•/:://:•'•'•':•'•'•'•':////:'/: :'::/•'//::: |
^ ^^^'SOiU'ECH^^ ^^KT'0———————— ——————^ ::f::::: ^^ ———————————————^ TREATED SOLIDS
11 ::y:fisY.STEMi
CONDENSEDOIL
MAKE-UP1^______________\_________Oil:_________
DRAFT2-25-93
ALTERNATIVE 'B'CONTAMINATED SOLIDS TREATMENT
DECHLORINATION TREATABILITY STUDYPREF^ARFD FOR
HERCULES INCORPORATED
AT—\————————r-^j——i CanonieEnvironmentcil^~^~ ISSUE/REVISION ^.^7^:______________________| -^ | nGURE 6 U^ ^
BCDDECHLORINATION
REAGENTS
CONTAMINATEDSOILDS
:SOILTECH:::::::::;:::::::;: ATP?;:^-SYSTEM^
TREATED SOLIDS
MAKE-UPOIL
DECHLORINATIONREAGENTS
CONDENSEDOIL
••^.BCD^^.REACTORii:
BCD TREATED OIL ANDREACTION RESIDUALS
DRAFT2-25-93
ALTERNATIVE •C'CONTAMINATED SOLIDS TREATMENT
DECHLORINATION TREATABILITY STUDYPKEPARED FOR
HERCULES INCORPORATED
CanonieEnvlronmentali'-;;>ur / RIVI'.ION PATE: 1-20-95
SCAIl NONrFIGURE 7
.QRV!3ER••:.» 229 -A I/
CARRIEROIL
CONTAMINATEDSOILDS
SOILTECH•::::::i:::;•:\::::.::::::ATP:•::;:::::::::::
::;TREATED SOLIDS
CONDENSEDOIL
INCINERATIONOF CONDENSED OIL
DRAFT2—25—93
ALTERNATIVE 'D'CONTAMINATED SOLIDS TREATMENT
DECHLORINATION TREATABILITY STUDYPIWAREO FOR
HERCULES INCORPORATED
CanonieEnvironmentalISSUE / REVISION 'WN B-i CK'O BY At1 f » Hi
DATE: 1-20-93
SCALE- NONE FIGURE 8IMBER
'18
LOW TEMP. STEAMAND HYDROCARBONVAPORS FLOW
FEEDSTOCKS
SPENT SOLIDSTAILINGS
HYDROCARBONAND STEAMVAPORS FLOW
AUXIllARl-BURNERS
COMBUSTIONAIR FLOW
DATE ISSUE / REVISION K'[) Hi ^r'll H
W L1'LN<,LI HUM "fACIUh PKUI-LyJDK FUR IKEA1MINI 01(III roNTAMIIIArfO WA'>I[S". W TACIUK. RU HIICi'1',AO'.IKA ANNUAL SI'RING (-ONrrRiNCF "ADVAMCI Sin rHKOllUM HLLOVih. UVl UPGRADING IK.HNUlOl.rIIAIIII .IIINE, I')B7
CROSS SECTION
SOILTECH ATP SYSTEM
2-25-93 DECHLORINATION TREATABILITY STUDYPREPARED FOR
HERCULES INCORPORATED
CanomeEnvirrnmentalI l)A1E 1-20-93
SCALE NONEFIGURE 10
MOST ECONOMICALLY FAVORABLE ATP SYSTEM1 0 TPH 25 TPH5 TPH
QUANTITY OF CONTAMINATED MATERIAL EVALUATION OF(THOUSANDS ON TONS) OPTIMUM SIZE ATP UNIT
DECHLORINATION TREATABILITY STUDYPREPARED FOR
DRAFT2-25-93
HERCULES INCORPORATED
CanonieEnvironmentalISSUE / REVISION )WN H] CK'D iil V II B IDATE: 1-20-93
SCALE: NONEFIGURE 1 1
DRAWING NUMBER
l Mmo i
HE-TS-152-SSX-011200 F Ramp
15.1-46427-1-S2
Grid 1 5 2 soil sample after ramp run.
HE-TS-152-SSX-011100 F Retort
15.2-46427-1-S2H
Grid 1 5 2 soil sample after 1 .100°F retort run.
HE-TS-152-SSX-011000 F Retort
15.3-46427-1-S2L
Grid 1 5 2 soil sample after 1,000°F retort run.
\\\ . l s - 4 | ' ) - s ^ \ - , i l
l : f l l l 1 - K.nnp
i'" i - 4 « 4 2 ' : ^ 2
Grid 4 1 9 soil sample after ramp run.
HE-TS-419-SSX-01H O O F Retort
15.5-46427-2-S2H
Grid 419 soil sample after 1 ,100°F retort run.
^ HE-TS-419-SSX-011000 F Retort
15.6-46427-2-S2L
Grid 419 soil sample after 1,000°F retort run.
IIF.-.SC-IX 4-OSO-011100 F Retort
15.10-46427-3-S2H
Spent carbon sample after 1,100°F retort run .
H F . - ^ < - I X 4-( »s< ) - i » l
lUOO I-' Rcloi- t
1 5 . 1 1 - 4 ( ) 4 2 " ' ^ - ^ 2 1 .
Spent carbon sample after 1,000°F retort run.
HE-TS-152-SSX-01Composite Combustion
15.7-46427-1-S3
Grid 1 5 2 composite retort sample after combustion run.
HE-TS-419-SSX-01Composite Combustion
15.8-46427-2-S3
Grid 419 composite retort sample after combustion run,
Syringe pump for controlled injection of liquid sample.
Recycling Dean & Stark-type receiver for collecting distillate for removal or recycle.
Organic and aqueous phase condensate collected in recyclingDean & Stark-type receiver.
Treated reaction products in BCD round bottom reaction flask.
APPENDIX B
HAZEN AND WSU TREATABILITY STUDY REPORTS.•'-•'''
1 . HAZEN RESEARCH, IN.G.. SOILTECH ATP SYSTEMS, VERTACTREATABILITY STUDY ^S.
2. WRIGHT STATE UNIVERSITY BCD TREATMENT OF SOILTECH ATPSYSTEMS, W: CONDENSATES
Copy No..HRI Project 7684-15
VERTAC TREATABILITY STUDY
Prepared by: Approved by:
:^Jerome P. Downey /fProject Manager ./
Hazen Research, Inc.
TABLE OF CONTENTS
Page
INTRODUCTION AND SUMMARY
BENCH-SCALE TEST DESIGN AND PROCEDURESAPPARATUSPROCEDURES
Thermal Desorption TestsCombustion Tests
RESULTS AND OBSERVATIONS 6CHARACTERISTICS OF FEED MATERIAL AND PROCESS RESIDUES 6
Source Samples 6Products 7
PROCESS RESULTS AND PERFORMANCE DATA 19
APPENDIX
Hazen Research, Inc.
INTRODUCTION AND SUMMARY
Hazen Research, Inc. conducted a series of bench-scale treatability tests on two soil samples and a
spent carbon sample, contaminated with Code F020 to F023 wastes, from the Vertac Remediation
Site in Jacksonville, Arkansas. The samples were prepared by Weston as requested by AlbertLefranc. These samples were in compliance with Hazen and SoilTech, Inc. shipping protocols. Thesource samples consisted of six 2-gallon pails (two duplicate pails in three coolers) and weredesignated as follows: HE-TS-152-SSX-01 (HRI No. 46427-1), HE-TS-419-SSX-01 (HRI No.
46427-2), and HE-SC-DC4-OSO-01 (HRI No. 46427-3).
The treatability tests were conducted to demonstrate the effectiveness and applicability of theSoilTech Anaerobic Thermal Process (ATP) System in removing organic contamination from these
samples. SoilTech has contracted with Hazen to conduct bench-scale treatability tests on soil,
sediments, and sludges containing wastes regulated under the Toxic Substance Control Act (TSCA)and the Resource Conservation and Recovery Act (RCRA). SoilTech has elected only to have Hazen
perform the treatability tests and selected analytical procedures described herein; interpretation of
analytical data is performed by SoilTech.
The treatability tests were performed from October 19 through October 23, 1992. The treatabilitytesting program consisted of 11 thermal desorption runs and two combustion runs.
Representative samples of the three source samples, as well as condensate, coked, and combusted
products were shipped to Dr. Thomas Tieman, Wright State University, Dayton, Ohio for
environmental analyses. Representative samples of the two combusted products were sent to VistaLaboratories, Broomfield, Colorado for Toxicity Characteristic Leaching Procedure (TCLP) tesung.
Hazen Research, Inc.
BENCH-SCALE TEST DESIGN AND PROCEDURES r*»0(-•")
The bench-scale ATP test unit, or batch reactor, was designed to simulate the conditions present in ".the preheat, reaction, and combustion zones of SoilTech's commercial ATP System. SoUTechevaluates the effects of the process variables on product quality by testing the feedstocks on a benchscale. Material balances and product closures are calculated by Hazen at the conclusion of each testas a quality control check.
Additional analytical work is performed to fully characterize the batch test products and to determinethe effects of thermal treatment. In the Venae treatability study, samples were shipped to Dr. ThomasTieman. Wright State University, Dayton, Ohio. and Vista Laboratories, Broomfield, Colorado.Analytical results are reported directly to SoiITech; Hazen does not evaluate the effectiveness ofthermal desorption in the batch tests.
APPARATUS
The bench-scale test unit is an electrically-heated, rotary-drum reactor with internal measurementsof 14 inches in diameter and five inches in length. The reactor drum can be rotated at speeds rangingfrom three to 16 revolutions per minute by an electric, variable-speed drive assembly. The reactoris heated by electrical elements installed on the outside of the steel reactor shell. Two slip ring seriesprovide electric power to the heaters and obtain the thermocouple outputs. Nine thermocoupleslocated in or around the reactor measure the temperatures of the steel shell (at various locations), thesolid charge within the shell (bed temperature), and the temperature of the exiting vapor. Thethermocouple signals are digitally displayed and continually processed by a strip chart recorder toindicate the heating profile. The reactor is charged and unloaded through a five-inch access port witha quick-lock cap.
A pipe passing axially through the reactor drive assembly introduces nitrogen purge gas into thereactor during each test run. The nitrogen passes through a gas meter, a rotary seal, and into thereactor feed pipe. The nitrogen flow is discontinued once the reactor has been charged and the
charge portal sealed. The purge gas, steam, and organic vapors generated while processing the
sample exit the reactor and pass through a two-stage condenser system.
Hazen Research. Inc.
30COt^-0
The primary condenser is a water-cooled, stainless steel, double-pipe heat exchanger. The condenser CDis inclined at approximately 45° to allow the condensed liquids to drain by gravity into the collection °reservoir. The aqueous and organic fluids accumulate in the reservoir, while the gases disengage andpass upward through a secondary condenser tube (also a water-cooled, double-pipe heat exchanger)situated vertically above the reservoir. Any liquids that condense within this device also drain intothe condensate trap. The condensed liquids are recovered and submitted for chemical analysis.
Gases emerge from the secondary condenser, pass through an impinger to remove any remainingmoisture or organic mist, and are then discharged through a wet gas meter into a plastic (Tedlar) gascollection bag. The meter measures the total volume of gases evolved during each batch test In thisstudy, the gases were pumped from the Tedlar gas collection bag through a carbon column to thelaboratory gas cleaning system.
PROCEDURES
Thermal Desorption Tests
Three source samples were tested in this treatability study. Two of the source samples were soilsamples and the third source sample was a spent carbon sample. Characterization data provided bySoilTech indicated the F020 to F023 contamination levels of the source samples could range from600 to 40,000 pans per billion (ppb). The samples were also reported to contain other organic andinorganic contaminants. The contaminants included: volatile organic carbons (VOCs) inconcentrations from none detected (ND) to 5,100 pans per million (ppm). toluene (the most abundantcontaminant) at 4,100 to 5,100 ppm; BNAs included phenol (ND to 280 ppm), 2-chlorophenol (NDto 960 ppm), 2,4-dichlorophenol (ND to 150,000 ppm), naphthalene (ND to 2,000 ppm), 2,4.6-trichlorophenol (ND to 1,600 ppm), and 2,4,5-trichlorophenol (ND to 5,500 ppm); herbicides included2,4-dichlorophenoxyacetic acid (0.25 to 140,000 ppm), 2,4,5-TP (0.034 to 640 ppm). and 2,4.5-trichlorophenoxy-acetic acid (0.23 to 2,300 ppm); and metals included antimony (ND to 14.4 ppm),arsenic (ND to 24 ppm), barium (3.8 to 92 ppm), calcium (190 to 3,490 ppm), lead (ND to 30 ppm),magnesium (74 to 819 ppm), potassium (ND to 537 ppm), sodium (15 to 1,970 ppm), and zinc (NDto 36 ppm).
Hazen Research, Inc.
4T-^
COi>0
The test durations varied depending on the attainment of specific test objectives. These included: 1) 0the specified bed temperature, 2) cessation of liquid condensate formation, and 3) a decrease in gas ^evolution to a level below 0.004 actual cubic feet per minute (acfm). Once these objectives weremet, the test was concluded by purging the reactor with nitrogen, removing the reactor lid, andrecovering the solid residue. This material was allowed to cool, then weighed and sampled forchemical analysis.
A ramp test was completed for each of the source samples. In the ramp test, the sample was heatedfrom a relatively low (near ambient) initial temperature to approximately 1,200°F. The rate of gasevolution and condensate production with respect to temperature was monitored throughout the test
Fixed-temperature retort runs were conducted on all three source samples. The purpose of the retorttests was to simulate direct injection of the contaminated material into the retort zone of the full-scaleATP unit. All three source samples were evaluated in two retort runs, with bed temperatures ofapproximately 1,000 and 1,100°F, respectively. In these tests roughly equal masses of sample andsilica sand were charged to the reactor. The treated solids recovered from these tests were sampledfor analysis and the remainder stored.
The solids produced by the ramp and retort runs are referred to as "coked solids" because therelatively high reactor-bed temperature, in combination with the absence of oxygen in the reactoratmosphere, results in the formation of coke (carbon), which coats the solid residue particles. Thecoked solids represent the product of the full-scale ATP unit's retort zone. The coked solids aresubmitted for organic analysis to determine the degree of decontamination achieved by thermaldesorpuon.
During all ramp and retort runs, aqueous and organic liquid condensates were collected in thecondensate reservoir. The condensates were recovered and their masses and volumes measured forthe material balances prior to sampling for laboratory analysis. The volume of the gases producedwas also measured and recorded for the material balances.
Hazen Research, Inc.
5C\£"0
Combustion Tests ^0
In the commercial ATP System, the coked solids move through the combustion zone after being fully ^decontaminated in the retort zone. Bench-scale combustion testing was performed to represent andconfirm this step. The combustion test product simulates the final product of the ATP process.
The batch combustion tests were conducted in the same reactor as the ramp and retort tests; thegeneral combustion test procedure resembles that of the retort tests in many respects. However, incombustion tests, air is continuously passed through the reactor to react with the carbon that coatsthe solids. A lifter is also installed in the retort to facilitate combustion by lifting and dropping thecoked solids through the air stream.
Two combustion tests were performed in this treatability study. The coked solids produced in the1,000 and 1,100 retort tests from each soil source sample (HRI No. 46427-1,46427-2) were blendedto produce the feedstock for each of the combustion tests. In these tests the reactor was preheatedto approximately 1,250°F and purged with nitrogen before the test charge was loaded. Once thereactor was charged and sealed, the nitrogen flow was discontinued and approximately 15 actualcubic feet per hour (acfh) of combustion air was injected through the same piping system employedin the retort tests. Likewise, the product gases passed through the gas metering system describedpreviously. The exhaust gases were monitored with an oxygen meter and Draeger tubes to determinewhen combustion was completed. The offgas volume was monitored throughout the test and the gaswas discharged through the laboratory ventilation and filtration system. At the conclusion of thecombustion test, the combusied solids were removed from the retort, weighed, and prepared forchemical analysis.
Hazen Research, Inc.
RESULTS AND OBSERVATIONS
CHARACTERISTICS OF FEED MATERIAL AND PROCESS RESIDUES
Observations regarding the physical appearance and qualities of the source samples and variousprocess residues (i.e. coked solids, liquid condensate, and noncondensable gases) are summarizedbelow.
Source Samples
The three source samples were received at Hazen on Thursday October 15, 1992. The samplesoriginated at the Vertac remediation site in Jacksonville. Arkansas. The source samples wereprepared by Albert Lefranc. The samples were in compliance with Hazen and SoilTech shippingprotocols.
Each of the three source samples was packed in two 2-gallon plastic pails fitted with a locking lid.The pails were clean, dry, intact, and sealed. The samples were logged into Hazen records, assignedHazen identification numbers, and weighed. This information is tabulated below:
Client Designation
HE-TS-152-SSX-01 (1 of 2)
HE-TS-152-SSX-01 (2 of 2)
HE-TS-419-SSX-01 (1 of 2)
HE-TS-419-SSX-01 (2 of 2)
HE-SC-DC4-OSO-01 (1 of 2)
HE-SC-DC4-OSO-01 (2 of 2)
HRI No.
46427-1
46427-2
46427-3
Gross Wt. Kilograms
7.74
6.83
7.67
7.57
4.17
4.30
Hazen Research, Inc.
'0r-»
The sample containers for 46427-1, 46427-2. and 46427-3 were initially opened for inspection on ^October 19. 20, and 22, 1992 respectively. The containers were scanned for beta/gamma radiation; ^no radiation above background levels was detected. Once the containers were opened, aphotoionization detector was used to measure the concentration of organic vapors in the freeboardabove each sample. No organic vapors were detected for the 46427-1 and 46427-2 samples. Abovethe 46427-3 (carbon) sample. 14 ppm was detected. The samples were mixed to ensure homogeneitybefore withdrawing samples for chemical analysis. Hazen observations regarding the color, matrix,and other characteristics of the source samples are detailed below. The Hazen sample identificationnumbers (HRI No.) as well as the client's designation will serve as the designators for each sourcesample throughout this report
• HRI No. 46427-1: HE-TS- 152-SSX-01 was a sandy soil. reddish in color with visible roots andpeat There were no particles greater than one inch. Sample appeared very uniform with lowmoisture (11.4%) content. A screwdriver was placed into the sample and it came out clean.The percent ash was measured at 85.5%.
HRI No. 46427-2: HE-TS-419-SSX-01 was a fine soil material with only a few particlesgreater than 12 mesh. It was reddish to light brown in color with low (5.52%) moisture andhumus content The sample will bind together with a firm grip but falls apart easilyafterwards. A screwdriver was placed into the sample and it came out clean. The ash contentof this sample was 89.5%.
HRI No. 46427-3: HE-SC-DC4-OSO-01 was a granular, black, and somewhat glossy carbonmaterial. The sample did not stick together when compressed by hand. A screwdriver wasplaced into the sample and it came out with 15 to 20 grains adhering to the blade. The percentmoisture and ash of this sample were determined to be 34.3% and 7.76%, respectively.
Products
One ramp test and two retort tests were conducted on each of the three source samples. Twoadditional retort tests were performed on the HE-TS-152-SSX-01 (HRI No. 46427-1) source sampleto generate adequate condensate mass for testing at Wright State University. One combustion testwas performed on a blend (50:50) of the coked solids from the 1,000°F and the 1,100°F retort runson the HE-TS-152-SSX-01 source sample (HRI No. 46427-1). In addition, one combustion test wasperformed on a blend (50:50) of the coked solids from the 1,000°F and the 1,100°F retort runs on
Hazen Research, Inc.
'•-0r^o
the HE-TS-419-SSX-01 source sample (HRI No. 46427-2). Hazen's observations of the physical °
characteristics of the coked solids and liquid condensates from the ramp and retort runs, as well as
the combusied solids, are described below. Photographs of the feed and product solids were made
available to SoilTech.
The approximate mass balances for the ramp, retort and the combustion tests are also tabulated in this
section.
Sample: HE-TS-152-SSX-01Test: Ramp
HRI No. 46427-1. Test 15.1: The ramp test with the HE-TS-152-SSX-01 source sample wasperformed on October 19. 1992. In the ramp test, approximately 2.0 kilograms (kg) of the sourcesample were charged to the reactor at ambient temperature (approximately 65°F). The test was
completed two hours and 6 minutes after the power was first applied to the reactor. The final bed
temperature was 1,200°F. Condensate continued to flow after gas evolution was below 0.004 acfm
for approximately 20 minutes. The overall balance closure for the run was 99.3%
The appearance of the liquid condensate changed throughout the course of the ramp test These
changes are summarized in Table 1 and are described below.
The liquid condensate first appeared when the bed temperature had reached 215°F; it was clear in
color. Within five minutes the color of the condensate had changed to a rusty brown. By the time
the bed temperature had reached 808°F, two phases were visible with the top layer being reddish incolor and the lower layer remaining a rusty brown. As bed temperature neared 909°F, the bottom
layer turned cloudy. After bed temperature reached 1,200°F, gas generation had dropped below 0.004acfm. but condensate production continued. The system was held in stasis for approximately 20minutes until condensate production had ended. The final volume for the condensate was 380milliliters (ml), with 50 ml in the upper layer and 330 ml in the bottom layer.
The coked product formed during the run was a dusty free-flowing material that was easily retrievedfrom the reactor. The color of the material was dark grey to black. Particle size appeared to remaincomparable to the original soil sample.
Hazen Research, Inc.
Time
0955
1015
1020
1025
1030
1040
1050
1100
1110
1120
1130
1140
1150
1201
• Acmal•• Millilil
HE
Bed
Temp.
("F)
Ambient
215
296
367
450
578
730
808
909
1011
1115
1184
1200
1200
Cubic Feetten
:-TS-152-SSX-C
Offgas
Temp.
CF)
N/A
99
210
222
215
216
169
149
137
123
112
106
Table»1 Ramo Test I'.
Cumulative
Gas Vol.
(•CO-
N/A
0304
0.304
0.304
0.304
0.347
0.380
0.402
0.494
0.600
0.664
0.691
0.724
1
S.I. Ooerator's C
Condensiif
Volume
(ml)**
N/A
Visible
50
100
130
180
190
40
180
220
50
190
240
240
200
250
210
260
330
380
(bservations
Layer
N/A
Tod
Told
Tool
Told
Total
Total
Top
Bottom
Total
Top
Bottom
Total
Total
Bottom
Total
Bottom
Total
Bottom
Total
0"05>CO00
Color
N/A
dear
Rusty Brown
Rusty Brown
Rusty Brown
Rimy Brown
Rusty Brown
Reddish
Rusty Brown
Dark Red
Rusty Brown
Dark Tan
Hazen Research, Inc.
10
Sample: HE-TS-152-SSX-01Test: RetortTemperature: 1,100°F
HRI No. 46427-1. Test 15.2: The first retort test was conducted at the specified final bedtemperature of 1,100°F. Approximately one kilogram of silica was placed in the reactor andpreheated to 1,100° before the 1-kg sample was charged. After charging, the bed temperaturedropped to 984°; bed temperature returned to 1,100° after three minutes. The initial gas temperaturewas 496°F, After three minutes the cumulative gas volume was 0.314 actual cubic feet (acf), andthe gas temperature was 241°F. At twelve minutes the cumulative gas volume was 0.374 acf; thegas temperature was 181°F. The run was complete twelve minutes after the sample was charged.The overall balance closure for the run was 100.2%.
There was 190 ml of condensate formed during the run. The condensate had no distinct layers andwas a uniform brown-black color.
The coked product formed during the run was a dusty free-flowing material which was easilyretrieved from the reactor. The color of the material was dark grey/black. The balance of the materialother than the added sand was about 90% fine-grained particles and about 10% particles larger than12 mesh. The loss on ignition (LOI) for the coked product was 0.55%.
Sample: HE-TS-152-SSX-01Test: RetortTemperature: 1,000°F
HRI No. 46427-1. Test 15.3: The second retort test with this sample was conducted at 1,000°F.Approximately one kilogram of silica was placed in the reactor and preheated to 1,040°F before the1-kg sample was charged. After charging the feed material, the bed temperature dropped toapproximately 959°F. The initial gas temperature was 523°F. After five minutes the bed temperature
was 1.000°F, the gas temperature was 275°F. and the cumulative gas volume was 0.318 acf. Afterten minutes the bed temperature was 1,043°F and the gas temperature was 205°F; gas generation wasapproximately 0.020 acfm. The run was complete 13 minutes after the sample was charged to thereactor. The final bed temperature was 1,028°F, the gas temperature was 161°F, and the cumulativegas volume was 0.470 act. The overall balance closure for the run was 125.7%'''.
Hazen Research, Inc.
" CO'-02>
There was 190 ml of condensate formed during the run. The condensate had no distinct layers and r-^
was a uniform dark black/brown color. ^0
The coked product formed during the run was a dusty free-flowing material, and it was easilyretrieved from the reactor. The color of the material was dark grey/black. The balance of thematerial other than the added sand was about 90% fine-grained particles and about 10% particleslarger than 12 mesh. The LOI for the coked solids was 0.76%.
* It was observed that during the initial minute of the test that the gas flow had run backward for
approximately three seconds, representing 0.5 acf of gas. It is assumed that a blockage in the gas
scrubbing system allowed gas pressure to build in the scrubber until it equalized with the reactor
pressure. When the reverse gas flow occurred, a vacuum was created, pulling the scrubber liquids
from the scrubber back to the condensate collection reservoir. These additional liquids accounted for
approximately 550 milliliters of liquid or 550 grams of mass included with the condensate mass for
the test and the 125% balance closure. If the 550 grams were removed from the condensate mass,
the balance closure would be a calculated 98.8%. Both Tests 15.2 and 15.3 were repeated as Tests
15.12 and 15.13, respectively, to generate valid condensate samples for analysis.
Sample: HE-TS-152-SSX-01Test: Retort
Temperature: 1,100°F
HRI No. 46427-1. Test 15.12 frepeat of Test 15.2): This retort test was conducted at the specified
final bed temperature of 1,100°F. Approximately one kilogram of silica was placed in the reactor
and preheated to 1,130° before the 2-kg sample was charged. After charging, the bed temperature
dropped to 171°F; bed temperature returned to 1,100°F after eighteen minutes. The initial gas
temperature was 602°F. After five minutes the cumulative gas volume was 0.543 acf, and the gastemperature was 383°F. At ten minutes the cumulative gas volume was 0.803 acf, the gastemperature 218°F. The run was complete twenty minutes after the sample was charged. The overallbalance closure for the run was 98.58%.
There was 370 ml of condensate formed during the run. The condensate had no distinct layers and
was a uniform brown-black color.
Hazen Research, Inc.
12
The coked product formed during the mn was a dusty free-flowing material which was easily C"sretrieved from the reactor. The color of the material was dark grey/black. The balance of the material *&?other than the added sand was about 90% fine-grained panicles and about 10% panicles larger than12 mesh.
Sample: HE-TS-152-SSX-01
Test: RetortTemperature: 1,000°F
HRI No. 46427-1. Test 15.13 (repeat of Test 15.3): The second reton test with this sample wasconducted at 1,000°F. Approximately one kilogram of silica was placed in the reactor and preheatedto 1.040°F before the 2-kg sample was charged. After charging the feed material the bed temperaturedropped to approximately 209°F. The initial gas temperature was 363°F. After five minutes the bedtemperature was 900°F, the gas temperature was 246°F, and the cumulative gas volume was 0.444act. After ten minutes the bed temperature was 1,008°F and the gas temperature was 197°F. gasgeneration was approximately 0.012 acfm. The run was complete 20 minutes after the sample wascharged to the reactor. The final bed temperature was 1,002°F, the gas temperature was 165°F, andthe cumulative gas volume was 0.653 acf. The overall balance closure for the run was 99.33%.
There was 370 ml of condensate formed during the run. The condensate had no distinct layers andwas a uniform dark black/brown color.
The coked product formed dunng the run was a dusty free-flowing material and it was easilyretrieved from the reactor. The color of the material was dark grey/black. The balance of thematerial other than the added sand was about 90% fine-grained particles and about 10% panicleslarger than 12 mesh.
Sample: HE-TS-419.SSX-01
Test: Ramp
HRI No. 46427-1. Test 15.4: The ramp test with the HE-TS-419-SSX-01 source sample wasperformed on October 20, 1992. In the ramp test, approximately 2.0 kilograms (kg) of the sourcesample were charged to the reactor at ambient temperature (approximately 63°F). The test wascompleted one hour and 52 minutes after the power was first applied to the reactor. The final bedtemperature was 1,202°F. The overall balance closure for the run was 98.01%
Hazen Research, Inc.
13
0C5
The appearance of the liquid condensate changed throughout the course of the ramp test. These ^changes are summarized in Table 2 and are described below. ^
.0
The liquid condensate first appeared when the bed temperature had reached 215°F; it was a dirtyyellow color. Within five minutes the color of the condensale had changed to a clear yellow-gold,similar to thin motor oil. By the time the bed temperature had reached 631°F, two phases werevisible with the top layer being a dark brown color and the lower layer remaining a yellow-gold.These colors and characteristics remained throughout the duration of the test The final volume forthe condensate was 200 ml, with 60 ml in the upper layer and 140 ml in the bottom layer.
The coked product formed during the run was a dusty free-flowing material, and it was easilyretrieved from the reactor. The color of the material was dark grey to black. Particle size appearedto remain comparable to the original soil sample.
Sample: HE-TS-419.SSX-01Test: RetortTemperature: 1,100°F
HRI No. 46299-3. Test 15.5: Test 15.5 was the 1,100°F retort test for the second Vertac soilsample. Approximately one kilogram of silica was placed in the reactor and preheated to U30°Fbefore the 1-kg sample was charged. After charging the feed material, the bed temperature fell toapproximately 1,002°F. The initial gas temperature was 558°F. After three minutes the bedtemperature had returned to 1.100°F. Gas temperature at this point was 387°F, and the cumulativegas volume was 0.746 act. The run was complete 13 minutes after the sample was charged to thereactor. The final cumulative gas volume was 0.860 acf. The overall balance closure for the run was97.6%.
There was 100 ml of condensate formed during the run. The condensate had no distinct layers or
phases and was a uniform black/dark brown color.
The coked product formed during the run was a dusty free-flowing material, easily retrieved from thereactor. The color of the material was dark grey/black. The balance of the material other than theadded sand was about 90% fine-grained particles, and about 10% particles larger than 20 mesh. TheLOI of the coked product was 1.64%.
Hazen Research, Inc.
14
HE-TS^19-SSX-01
Bed Offgu
Texup> Temp*
Time (°F) (°F)
0845 Ambient N/A
0900 215 145
0915 466 201
0925 631 186
0935 747 157
0945 851 142
0955 950 131
1000 994 125
1010 1107 112
1020 1209 100
1030 1218 95
1036 1202 92
• Actual Cubic Feet
•• Milliliten
Table 2Ramo Test 15.4,
Cumilttive
Gas Vol.
(arf)*
N/A
0.419
0.419
0.419
0.553
0.658
0.843
0.925
1.124
1.277
1.296
1.356
Ooerator's
Coadeuaic
Volume
(ml)—
N/A
Visible
110
Visible
130
130
20
140
160
50
140
190
60
140
200
60
140
200
60
140
200
60
140
200
60
140
200
60
140
200
Observations
Layer
N/A
Total
Total
Top
Bottom
Total
Top
Bottom
Total
Top
Bottom
Total
Top
Booom
Total
Top
Bottom
Total
Top
Bottom
Total
Top
Bottom
Total
Top
Bottom
Total
Top
Bottom
Total
•r-402>C^0
———— -^
Color
N/A
Yellow-Cloudy
Yellow/Gold
DarkBrowo
Yellow/Gold
Dark Brown
Yellow/Gold
Dark Brown
Yellow/Gold
Dark Brown
Yellow/Gold
Dark Brown
Yellow/Gold
Dark Brown
Yellow/Gold
Dark Browo
Yellow/Gold
Dark Brown
Yellow/Gold
Dark Brown
Yellow/Gold
Hazen Research, Inc.
15
Sample: HE-TS-419-SSX-01Test: RetortTemperature: 1,000°F
HRI No. 46427-2. Test 15.6: The second retort test with this sample was conducted at 1,000°F.Approximately one kilogram of silica was placed in the reactor and preheated to 1.040°F before the1-kg sample was charged. After charging the feed material, the bed temperature fell to approximately876°F. The initial gas temperature was 571 °F. After eight minutes the bed temperature had returnedto 1,000°F. At this point the gas temperature was 417°F, and the cumulative gas volume was 0.379acf. The run was complete 16 minutes after the sample was charged to the reactor. The final bedtemperature was 1016°F, the gas temperature was 164°F, and the cumulative gas volume was 0.542act. The overall balance closure for the run was 98.3%.
There was 100 ml of condensate formed during the run. The condensate, which appeared to haveonly one layer, was a uniform black/brown color.
The coked product formed during the run was a dusty free-flowing material; it was easily retrievedfrom the reactor. The color of the material was dark grey/black. The balance of the material otherthan the added sand was mostly fine-grained particles. The LOI of the coked product was 2.12%.
Sample: HE-SC-DC4-OSO-01Test: Ramp
HRI No. 46427-3. Test 15.9: The ramp test with the HE-SC-DC4-OSO-01 source sample wasperformed on October 22, 1992. In the ramp test, approximately 2 kg of the source sample and 1kg of silica sand were charged to the reactor at ambient temperature (approximately 65°F). The testwas completed two hours and four minutes after the power was first applied to the reactor. The finalbed temperature was 1,227°F. The overall balance closure for the run was 99.75%.
The appearance of the liquid condensate changed throughout the course of the ramp test. Thesechanges are summarized in Table 3 and are described below.
Hazen Research, Inc.
16
Table3HE-SC-DC4-OSO-01-Ramo Test 15.9
Bed Offgai CumulativeTemp- Temp. Gu Vol.
Time (°F) (°F) (act)*
0809 Ambiem N/A N/A
0823 204 203 0.365
0830 204 214 0.427
0835 204 239 0.427
0845 255 276 0.522
0855 480 190 0.746
0905 641 194 1.135
0915 783 175 1.432
0925 900 156 2.005
0945 1077 117 2.515
0955 1145 106 2.626
1013 1277 92 2.831
* Actual Cubic Fool*• MilUliter
. Operator's
CondeasieVolume(ml)"
N/A
Visible
240
5
415
420
5
635
640
5
675
680
5
695
20
720
5
695
50
750
5
695
70
770
5
695
70
770
5
695
70
770
5
695
70
770
Observations
Layer
N/A
Toul
Total
Top
Booom
Total
Top
Bottom
Total
Top
Bottom
Total
Top
Middle
Bottom
Total
Top
Middle
Bottom
Total
Top
Middle
Bottom
Total
Top
Middle
Bottom
Total
Top
Middle
Bottom
Total
Top
Middle
Bottom
Total
C'5^
C^
0®
Color
N/A
Light Brown
Light Brown
Dark Brown
Light Brown
Dark Brown
Light Brown
Dark Brown
Light Brown
Dark Brown
Light Brown
Black
Dark Brown
Light Brown
Black
Dark Brown
Light Brown
Black
Dark Brown
Light Brown
Black
Dark Brown
LJghl Brown
Black
Dark Brown
Light Brown
Black
Hazen Research, Inc.
17
The liquid condensate, which first appeared when the bed temperature had reached 204°F. was a clear
light brown color. Approximately thirteen minutes later, two phases were visible with the top layer
being a dark brown color and the lower layer remaining a light brown. When the bed temperaturereached 641 °F a thick black condensate formed. This phase appeared thick and oily; it dropped tothe bottom of the reservoir. After approximately 20 minutes condensate production stopped; bed
temperature was at 900°F, gas temperature at 150°F. Testing continued for an additional 53 minutesuntil gas evolution had dropped to 0.004 acfm. Final bed temperature was 1,227°F, gas temperature
92°F. The final condensate volume was 770 ml, with 5 ml as the top layer, 695 ml in the middle,
and 70 ml as the bottom layer.
The coked product formed during the run was a free-flowing material, easily retrieved from the
reactor. The material appeared like unused carbon: granular, slightly dusty, and dark black in color.
Particle size appeared to remain comparable to the original sample.
Sample: HE.SC-DC4-OSO-01
Test: RetortTemperature: 1,100°F
HR1 No. 46299-3. Test 15.10: Test 15.5 was the 1,100°F retort test for the Venae spent carbon
sample. Approximately one kilogram of silica was placed in the reactor and preheated to 1,130°F
before the 1-kg sample was charged. After charging the feed material, the bed temperature fell to
approximately 229°F. The initial gas temperature was 647°F. After 16 minutes the bed temperature
had returned to 1,100°F. Gas temperature at this point was 199°F, and the cumulative gas volume
was 1.306 acf. The run was complete 20 minutes after the sample was charged to the reactor. Thefinal cumulative gas volume was 1.338 acf. The overall balance closure for the run was 95.3%.
There was 300 ml of condensate formed during the run. The condensate had no distinct layers orphases and was a uniform black/dark brown color.
The coked product formed during the run, a slightly dusty free-flowing material, was easily retrievedfrom the reactor. The color of the material was a typical carbon: granular and black.
Hazen Research, Inc.
18
Sample: HE-SC-DC4-OSO-01Test: RetortTemperature: 1,000°F
HRI No. 46427-2, Test 15.11: The second retort test with this sample was conducted at 1,000°F.
Approximately one kilogram of silica was placed in the reactor and preheated to 1,040°F before the1-kg sample was charged. After charging the feed material, the bed temperature fell to approximately
229°F. The initial gas temperature was 572°F. After 14 minutes the bed temperature had returned
to 1,000°F. At this point the gas temperature was 197°F, and the cumulative gas volume was 1.214
acf. The run was complete 25 minutes after the sample was charged to the reactor. The final bedtemperature was 1.060°F, the gas temperature was 169°F, and the cumulative gas volume was 1.295act. The overall balance closure for the run was 94.8%.
There was 300 ml of condensate formed during the run; it appeared to have only one layer and wasa uniform black/brown color.
The coked product formed during the run was a slightly dusty free-flowing material, and was easily
retrieved from the reactor. The color of the material was a typical carbon: granular and black.
Sample: HE-TS-152.SSX-01Test: Combustion
HRI No. 46427-1, Test 15.7: One kilogram of the coked solids from Test 15.2 and 15.3 was used
as the feed for this combustion test. The run was complete 53 minutes* after the coked solids were
charged to the reactor. The total gas volume measured was 11.65 acf; this is only 88% of the purgegas that theoretically should have gone through the reactor at 15 acf/h. This low result wouldindicate that the air compressor was cycling low during the run. and it also means that the volumeof any offgas generated during the run cannot be measured.
The combusted solids were tan in color. The balance of the material other than the added sandappeared to be 90% fines and the remaining material of approximately 12 mesh.
* This run time is not exact, due to the lack of gas monitoring equipment. As the gas detector was
available, the offgas was checked and the test ended at that point
Hazen Research, Inc.
19
Sample: HE-TS-419-SSX-01Test: Combustion
HRI No. 46427-2. Test 15.8: One kilogram of the coked solids from Test 15.4 and 15.5 was usedas the feed for this combustion test. The run was complete 19 minutes after the coked solids were
charged to the reactor. The total gas volume measured was 6.745 acf; this represents 4.75 act of
purge air and 1.995 acf produced gas.
The combusted solids were tan in color. The balance of the material other than the added sand
appeared to be 90% fines and the remaining material of approximately 12 mesh.
PROCESS RESULTS AND PERFORMANCE DATA
The operating and mass balance data recorded during the ramp run and each of the retort runs are
summarized in Table 4. Operating data from the combustion test is presented in Table 5. Particlesize distribution data for the feed material and the combusted solids are included in Table 6 and Table
7. These data are also presented in graphic form as Figure 1 in the Appendix.
Hazen Research, Inc.
20
R
Test Number
Date
Test Type
HRI Sample No.
Input
Virgin feed. g
Silica, g
Mineral Oil
Total, g
Output
Total gas volume, acf
Purge gas. acf
Produced gas, act
Produced gas, g
Coked solids, g
Liquid condensale, g
Total, g
Balance Closures
Total input basis. %
Virgin feed basis, %
r
amo and Ri
15.1
10/19/92
Ramp
46427-1
2000.7
0.0
70.3
2071.0
1.804
1.08
0.724
23.9
1654.0
377.9
2055.8
99.26
99.26
Fable 4etort Test Sum
15.2
10/19/92
1.100° Retort
46427-1
1006.7
999.0
35.6
2041.3
1.396
1.022
0.374
12.3
1897.4
147.7
2057.4
100.7
101.5
marv
15.3
10/19/92
1,000° Retort
46427-1
1006.6
1000.2
34.1
2040.9
1.634
1.164
0.470
15.5
1883.0
667.9
2566.4
125.7
150.5
!>0i>000
15.4
10/20/92
Ramp
46427-2
2005.3
66.7
2072.0
2.428
1.072
1.356
44.75
1781.8
204.3
2030.8
98.01
98.01
acf = Actual cubic feet
Hazen Research, Inc.
21
Test Number
Date
Test Type
HRI Sample No.
Input
Virgin feed. g
Silica, g
Mineral Oil
Total, g
Output
Total gas volume, acf
Purge gas, acf
Produced gas, acf
Produced gas, g
Coked solids, g
Liquid condensale, g
Total, g
Balance Closures
Total input basis. %
Virgin feed basis. %
TabRamo and R<
15.5
10/20/92
1.100° Retort
46427-2
1004.8
1005.8
33.9
2044.5
2.027
1.167
0.860
28.4
1873.9
93.8
1996.1
97.6
98.6
Ie 4 Cont.itort Test Sumrnai
15.6
10/20/92
1.000° Retort
46427-2
1001.3
1008.3
33.2
2042.7
1.624
1.074
0.550
18.2
1909.9
79.1
2007.2
98.3
96.6
•V
15.9
10/22/92
Ramp
46427-3
2014.1
1007.2
66.8
3088.1
3.911
1.080
2.831
93.4
2191.6
795.6
3080.6
99.75
99.6
COC75£'*00
———————— 015.10
10/22/92
1,100° Retort
46427-3
1012.0
1004.9
35.1
2052.0
2.504
1.166
1.338
44.1
1600.5
310.4
1955.0
95.3
90.7
act = Actual cubic feet
Hazen Research, Inc.
Ramp
Test Number
Date
Test Type
HRI Sample No.
Input
Virgin feed. g
Silica, g
Mineral Oil
Total, g
Output
Total gas volume, acf
Purge gas, acf
Produced gas, act
Produced gas, g
Coked solids, g
Liquid condensate, g
Total, g
Balance Closures
Total input basis. %
Virgin feed basis, %
Table 4and Retort
15.11
10/22/92
1.000° Reton 1,100° Retort
46427-3
10119
1006.8
33.4
2053.1
2.320
1.025
1.295
42.7
1604.1
298.9
1945.7
94.8
89.7
Cont.Test Summarv
15.12
10/23/92
46427-1
2007.6
1001.1
66.6
3074.3
1.920
1.028
0.892
29.4
2705.1
296.2
3030.7
98.58
97.9
C^^I>00®
15.13
10/23/92
1.000° Reton
46427-1
2019.3
1020.4
66.1
3105.8
1.704
1.051
0.653
21.5
2749.6
313.9
3085.0
99.33
99.0
acf = Actual cubic feet
Hazen Research, Inc.
TablesCombustion Test Data
Test Number 15.7 15.8
Test Date
Feed Material
Retort Charge, g
Run Length, minutes
Theoretical Gas Input, acf
Combusted Solids
Offgas Volume, acf
Balance Closure. %
10/21/92
15.1 & 15.2Coked Product
1000.6
46
11.5
1008.6
11.65
100.7
10/21/92
15.4 & 15.5Coked Product
1011.1
19
4.75
999.8
6.745
98.9
Hazen Research, Inc.
24
Raw Fee
U.S. Sieve Size
Mesh Micron
5 4000
12 1700
20 850
45 355
70 212
100 150
200 75
Pan <75
TOTAL
Partici
d-HRI#4<
Direct
Wt%
13
0.8
1.2
IS
15.9
8.5
37.6
62.4
100.0
e Size IVer
»427-1
Cum
Ret
13
2.1
33
5.8
21.7
30.2
62.4
100.0
Tab
distributiontac/Herculei
. W t %
Pass.
98.7
975
96.7
94.2
783
69.8
0.0
Ie 6
of ATP Treas Chemical Si
U.S. Sie
Mesb
5
12
20
45
70
100
200
Pan
TOTAL
unent Solite
Combi
ve Size
Microo
4000
1700
850
355
212
150
75
<75
ids
Jslion Prodi
Direct
Wt.%
0.7
13
5.4
47.1
12.0
4.5
3.9
25.1
100.0
ICt
Cum.
Ret.
0.7
2.0
7.4
54.5
66.5
71.0
74.9
100.0
1000C309
Wt.%
Pass.
993
98.0
92.6
45.5
33.5
29.0
25.1
0.0
Hazen Research, Inc.
25
Particle Size DistributionVertac/Hercules Chemical Site
Sieve Size
100
Cumu
a 80
t
ve
60Percen 40
t
Re1 20a
ned
n
400ri
m 200"l
A^
i"? ii
^<
"\
B"?
^
^
\
^
^
V
\\
. ^
\\
2
\
01
4
<
-E
t
m 12m 5m
^- 46427-1-81
3- Combustion Product
3- Silica Sand
-
1
^1@h -^>
M
10 100 1000
Size. microns10000
M = Mean Particle SizeFIGURE 1
009803Hazen Research, Inc
26
Raw Fee
U.S. Sieve Size
Mesh Micron
5 4000
12 1700
20 850
45 355
70 212
100 150
200 75
Pan <75
TOTAL
Partici
d - HRI #4<
Direct
Wt.%
0.0
8.9
8.7
10.3
9.1
5.0
8.5
49.6
100.0
e Size EVert
•427-2
Cum.
Ret.
0.0
85
17.6
27.8
36S
42.0
50.4
100.0
Tab
(istributionac/Hercules
Wt.%
Pas*.
100.0
91.1
82.4
72.2
63.1
58.0
49.6
0.0
Ie 7
of ATP Treai Chemical Si
U.S. Sie
Mesh
5
12
20
45
70
100
200
Pan
TOTAL
tmentSolite
Comb'
ve Size
Micron
4000
1700
850
355
212
150
75
<75
lids
usuon Prodi
Direct
Wt.%
0.0
4.6
9.2
54.3
6.1
2.9
4.5
18.3.
100.0
ICt
Cum.
Ret
0.0
4.6
13.8
68.2
74.3
77.1
81.7
100.0
C^s^CO000
Wl.%
Pan.
100.0
95.4
86.2
31.8
25.7
22.9
18.3
0.0
Hazen Research, Inc.
Particle Size DistributionVertac/Hercules Chemical Site
Sieve Size
10000
Size, microns
M
M = Mean Particle SizeFIGURE 2
000804
) it-rn.-i n/t.-i-i'irr'h t'-ii-'
HE-SC-DC4-OSO-01HOOF Retort
15.10-46427-3-S2H
HE-SC-DC4-OSO-011000 F Retort
15.11-46427-3-S2L
Hazen Research, Inc.
HE-TS-152-SSX-011200 F Ramp
15.1-46427-1-S2
HE-TS-152.SSX-011100 F Retort
15.2-46427-1-S2H
Hazen Research, Inc.
HE-TS-152-SSX-011000 F Retort
15.3-46427-1-S2L
HE-TS-419-SSX-011200 F Ramp
15.4-46427-2-S2
Hazen Research, Inc.
HE-TS-419-SSX-011100 F Retort
15.5-46427-2-S2H
HE-TS-419-SSX-011000 F Retort
15.6-46427-2-S2L
Hazen Research, Inc.
reject No.——__ ^ ^ ;Book No._[4o^_ TITLE Lo^/tO^.^ ^CX^DU^
From Page No. L?
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Witnessed & Understood by me.
Recorded by J J
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corn Page NO.-L^
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APPENDIX C \.. '•'''''
ATP SYSTEM AND BCD PROCESSTREATABILITY STUDY ANALYTICAL RESULTS
J -1 . SAMPLE TRACKING DIAGRAM
f^2. ATP SYSTEM TREAf ABILITY STUDY ANALYTICAL RESULTS
3. BCD .PROCESS TREATABILITY STUDY ANALYTICAL RESULTS
4. QUALITY ASSURANCE ANALYTICAL SUMMARY
TREATABILITY STUDY
SAMPLE TRACKING DIAGRAM
VERTAC SITE, JACKSONVILLE, ARKANSAS
46427-1-81
HE-TS-152-SSX-01
(Grid 152 Soil)
-»— 15.1-46427-1
(Ramp Test, Coked Solids)
»- 15346427-1-S2L
(Low Temp., Retort Solids)
-»-15.2-46427-1-S2H
(High Temp., Retort Solids)
NOTES:
15 7-46427-1-S3
-^- 925496-001
(Combusted Solids)
HE-XX-XXX-XXX-01 Hercules Sample #
XXX-46427-X-XXX SollTech Sample •>
925496-OOX Vista Sample #
SOI12C-12XX Wright State University Sample #
---.-^- 46427-1-L1 i
(Ramp/Retort Condensate)
46427-2-S1
HE-TS-419-SSX-01
(Grid 419 Soil)
-^- 15.4-46427-2
(Ramp Test, Coked Solids)
^-»-15.6-46427-2-S2L ——
(Low Temp., Retort Solids)
- »- 15.5-46427-2-S2H
(High Temp., Retort Solids)
15.8-46427-2-S3
»- 925496-002
(Combusted Solid;.)
SOI2C-12GA
r^ S012C-12B
(Solid Phase)
Extracted
Contaminants
-^- S012C-12GB(Intermed. BCD Product)
(Feed to BCD Test G)
SOI2C-12GC
(Final BCD Product)
-^- SOI2C-12HB
(Intermed. BCD Product)
46427-3-S1
HE-SC-DC4-OS&01
(Spent Carbon)
4642?<2-L|i
(Ramp/Retort Bondensate)
-»- 15.9-46427-3
(Ramp Test, Coked Solids)
- »-15.11-46427-3-S2L
(Low Temp., Retort Solids)
-»-15.10-46427-3-S2H
(High Temp., Retort Solids)
-—-- - -_ . -_ -_ .——^-46427-3-L1 I
(Ramp/Retort Condensate)
Condensate
Composite
S012C-12
Organic Phase
S012C-12C
^ SOI2C-12D
(Aqueous Phase)
Extracted
Contaminants
SOI2C-12HA
(Feed to BCD Test H)
S012C-12HC
'(Final BCD Product)
SOI2C-12IA
-»^ SOI2C-12IB
(Intermed. BCD Product)
SOI2C-12IC
(Feed to BCD Test I) (Final BCD Product)
CanonieEt i\ i<IWM-.191 229/1 RACKOIA XIS I2I24J33)
TABLE 1
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CAfiONIE ENV. ;5;5BSaioleNuioer
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2A. 15.2-46427-1-S2H
3A. 15.3-46427-1-52.
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6A. 15.6-46427-2-S2L
7A. 15.7-46427-1-53
3PK 15.7-46427-1-S3
SPK 15.7-46247-1-S3
8A. 15.8-46427-2-S3
11AAA. 15.9-46427-1-51
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11/09/92
11/09/92
11/20/92
11/20/92
11/20/92
11/09/92
11/20/92
11/09/92
-9 "">rl b • ^k'^
3r Dar;
T
TiM 1
13:204 ^ , ^
t-;...'
16:25
17:51
15:50
17:15
14:53
15:51
16:55
18:40
17:33
13:12
3-Mr-£:...:in;2.
on Int. Ratios320/322 332'354
0.i2 3.34
3.80 3.77
0.88
0,83
0.79 0.83
0.81 0.87
0.79
0.39 0.81
0.79 0.78
0.83
0.73
0.86
^ 3.Sec.
4k
35
60
61
63
68
75
66
59
48
27
37
Ion320
37002
190201
-1250
6605
6258
53056
-1500
27044
40920
-1600
-1420
914
IniensitK3^
105950
237153
-1250
7058
7398
65565
-1500
30528
51662
-1600
-529
-374
•S V.257
-1
.17:17
-716
5088
7925
32832
-3246
15661
28103
-849
-1289
-1
332
33S99
23198
39991
37814
51118
57399
66009
55398
75052
37165
24343
26713
<^—1CO000
334
43229
29984
44615
43095
61676
66199
;3036
68574
95784
44859
33344
31131
a. "he designation NO indicates "None Detectea' in eicess of :ns •iniBUB aetectaoieconcentration unien is Listefl directly oelov the NO aesignation.
c. ^cr water samoies the weignt if tne saBoie aliouot was calculates oy inuitiolying tne voiune of vater snaiyzeo oy l.BMC.
:. "X = "iniinua Oetectaoic Concentration
:. t Rec. = Percent recovery ^or ;ne TCSD internal stanaara
e. Tne notation useo here to cesignate ion intensities is exoonentiai notation.A negative sign preceding ;r.e oeaK intensity value citea inaicates tnac no response was ooserveo at tnat ii/z.
TABLE 2-right State University. Dayton, inia 45*35
."sulES of aC/flS Analyses of Extracts for 2378 7CCD
Concentrations found ipiccsraas oer graB or wait or oarcs-Der-tril..ior.ia.
Colar. - 3E5 B0fl , a.25uIsowr soeciTi; analysis
i>-CiCOC"-)00
;ANC,1IE E.W. 2559CSuoli UeigntNuber g b.
11A6. 15.C-4627-3-S1 8.9889
^A. l5.13-4b427-3-32K 20.65
1BA. 15.11-46A27-3-S2L 20.37
LAB BLANK (C) 20.00
2"S •:XCone. Founc
PPT"teas. HDC c.
Instr. Ion Int. Ratios » d.:3 Date Tine 320/322 332/334 Rec.
.46 - iTS-25 12/11/92 12:36 3.88 0.86 39
N0 29.6 f1S-25 11/10/92 13:40 - 3.89 55
80.5 - (B-25 11/10/92 17:09 0.67 3.87 49
N0 1.53 US-25 11/10/92 14:12 - 0.83 33
Ion Intensities e.320 322 257
4612
2.167
33313
5265 2956
61636 -I
49571 103337
-1758 -1750 444229
332 334
11730 13682
.8053 54166
26490 30388
51574 62222
a. The designation NC indicates 'None detected' in excess of the •iniBr oetectafileconcentration wnicn is misted directly beiow the NO designation.
:. Fsr vatsr saaoies tne weignt of tne sanoic aliauot uas calculated or nultiDmns rne voiuae of water anaiyzeo by Li
:. "DC = '"inl.T'Jiii Oerctisie Concentration
:. ^ Sec. •- Percent recovery for tne TCDD internal standard
e. The notation usea nere to designate ion intensities is eicionential notation.A negative sis". Dreceaing tne PCBK intensity value citea inaicates triat no resoonse uas ooserveo at that ni/z.
TABLE 3-frignt state University, Day:on, Crio *5.35
C.iiuan - u35 ?3M , 3..5u
Native SciKCi
Conci".;r2:;;r.s 'wx; inaricigraits oir y3B of aaiait y i'arts-oer-si.-iarJS.
sfk Is.^-iOt.T-l-^
::737-;;:i
Conctncraion fiund - rig/a. Native Anaiytss26.1
Concentraisr. founa in 'JnsciKed sa«Die - '13/0.NC.
Concentraion found (Soiked sa»>ie - Unspiked saaoie> - ng/iL26.:
Soike Concentration • ng/nL50.9
\ recovery of SDike52 »
SPK 15.7-46247-1-53
2378TC30
Concentraion foimd - ng/iL Native Analytes3B.5
Concentraion found in unspiked saiiole - ng/'BLNO
Concentraion round ; Soiked saitolt - UnsDikeo safflDiei - ng/'BL33.5
Soike Concentration - ng/aL53.0
\ ,-ecovery o'' soike61 ',
SampleNu.-b=r
TABLE 1
Wright State University
Herbicide Analyses
Column - DBS 5 0 M , 0 . 2 5 , 0 . 2 5
Samples, levels - micrograns/g
Native Values ( p p r . )
2 , 4 D 2 , 4 , 5 T SILVEX
Rec ( % ;C13
2 , 4 D
1CA. 15.1-46427-1-S1 0.1 ND ND( 0 . 0 3 ) ( 0 . 0 3 )
95
4CA. 15.4-46427-2-S1 21 28 23 85
2C. 15 .2 -46427-1 -S2H ND ND ND( 0 . 0 1 ) ( 0 . 0 2 ) ( 0 . 0 2 )
3C. 15.3-46427-1-S2L ND ND ND( 0 . 0 0 5 ) ( 0 . 0 1 ) ( 0 . 0 1 ;
70
5C. 15.5-46427-1-S2H
6 C . 15.6-46427-2-S2L
73. 15.7-46427-2-S3
NATIVE SPIKE7H. 15.7-46427-1-S3
NATIVE SPIKE RECOVERY
NATIVE SPIKE71. 15.7-46427-1-S3
NATIVE SPIKE RECOVERY
8C. 15.8-46427-2-S3
ND ND ND( 0 . 0 0 5 ) ( 0 . 0 1 ) ( 0 . 0 1
ND ND ND( 0 . 0 0 5 ) ( 0 . 0 1 ) ( 0 . 0 1
ND ND ND( 0 . 0 0 5 ) ( 0 . 0 1 ) ( 0 . 0 1
1 . 1 1 . 0 0 . 7
107% 101% 72%
1 . 1 0 . 9 0 . 6
116% 95% 62%
ND ND ND( 0 . 0 0 5 ) ( 0 . 0 1 ) ( 0 . 0 1
65
45
95
63
43
49
SampleNumber
TABLE 2
Wright State University
Herbicide Analyses
Colur-.n - DB5 r:Ot-I, 3 . .I 5 , C . 25
Samples, levels - ."'icrograrp.s/g
Native Va1u e s ippm,'
2 , 4 D 2 , 4 , 5 T SILVEX
Rec ( % )C13
2 , 4 D
9 C . 15.10-46427-3-S2H ND ND ND( 0 . 0 1 ) ( 0 . 0 1 ) ( 0 . 0 1 ;
10C. 15.11-46427-3-S2L ND ND ND( 0 . 0 1 ) ( 0 . 0 1 ) ( 0 . 0 1 ;
11CAA. 15.9-46427-3-S1 721 45 9
ND ND ND( 0 . 0 0 5 ) ( 0 . 0 1 ) ( 0 . 0 1 )
LAB BLANK LB11122-2
ND ND ND( 0 . 0 0 5 ) ' ; 3 . 0 1 ) ( 0 . 0 1 )
LAB BLANK LB11172-1
62
72
81
85
90
Column - DBS
S anp1es, 1 •= ve1s
Native Values (pp.^.)Sa.-pleNunber
1BA. 1( 0 . 5 )
4BA. 15.4-46427-2-S1
2B. 15( 0 . 1 )
3B. 15
5B. 15( 0 . 1 )
6B. 15( 0 . 1 )
-n - =
( 0 . 2 )
NATIVE7E. 15
NATIVE
NATIVE7F. 15
NATIVE
SB. 15( 0 . 1 )
5 .1 -46427-1-S1
.2-46427-1-S2H
•3-46427-1-S2L
•5-46427-1-S2H
.5 -46427-2 -S2L
. 7 - 4 6 4 2 7 - 2 - S 3
SPIKE.7 -46427 -1 -S3
SPIKE RECOVERY
SPIKE. 7 - 4 6 4 2 7 - 1 - S 3
SPIKE RECOVERY
.8 -46427-2 -S3
TA
Wright State
PolyChlorinatedP
MonoCP
ND
9.5
ND
ND( 0 . 1 )
ND
ND
ND
1 . 4
1 4 8 %
1 . 3
140%
ND
.BLE 1
Uni
heno
60M.
- T.icrograr.s,
6.7
( 0 . 0 2
( 0 . 0 2 )
ND *
( 0 . 0 2 )
2 .7
2 .4
•/ersic
is Ana
0 . 2 5 . 0
DiCP
ND( 0 . 3 )
ND
ND
ND( 0 . 0 2 )
( 0 . 0 2 )
ND
1 4 6 %
125%
ND( 0 . 0 2 )
y
J.
.
Tri C13
ND 35
)
ys»:
25
( 1 . 0 )
( 0 . 0 8 )
( 0 . 0 8 )
v*>s u?
COCT0
g o
Rec ( % )
CP CP
96 52
ND 38( 0 . 0 8 )
ND 36( 0 . 0 8 )
ND 39( 0 . 0 8 )
ND 40
ND 19
2 .7 37
143%
2.1 37
1 1 1 %
ND 28( 0 . 0 8 )
TABLE 2
Wright State University
PolyChlorinatedPhenols Analyses
Column - DBS 6 0 M , 0 . 2 5 , 0 . 2 5
Samples, levels - rr.icrograms/g
Native Values (pp.-n)SampleNumber Mono
CPDi
CPTri
CP
NATIVE SPIKE7X. 15.7-46427-1-S3
NATIVE SPIKE RECOVERY
1.2
118%
2.3
116%
2.1
108%
NATIVE SPIKE9X. 15.10-46427-3-S2H
NATIVE SPIKE RECOVERY
9B. 15 .10-46427-3 -S2H
10B. 1 5 . 1 1 - 4 6 4 2 7 - 3 - S 2 L
1.
150%
ND(0.
ND(0 .
5
1 )
2)
2.1
100%
ND( 0 . 0 2 )
ND' 0 . 0 4 )
1 . 3
65%
ND(0 .08
ND( 0 . 1 )
113AA. -5.9-46427-3-S1 160 3250 1300
LAB BLANK LB11122-1 ND( 0 . 7 )
ND( 0 . 1 )
ND( 0 . 3
LAB BLANK LB11052-1 ND ND ND( 0 . 0 5 ) ( 0 . 0 1 ) ( 0 . 0 8 )
LAB BLANK LB11032-1 ND( 0 . 0 5 ;
ND( 0 . 0 1 )
ND( 0 . 0 8
LAB BLANK LB11112-1 ND( 0 . 0 5 )
ND( 0 . 0 1 )
ND( 0 . 0 3 :
SampleNumber
TABLE 3
Wright Stace University
TetraChloroBanzene Analyses
Column - DBS 6 0 M , 0 . 2 5 , 0 . 2 5
Samples, levels - r.i^rogra.-rs •'g
Native Values(ppm)
TCB
Rec ' % )C:3TCB
1BA. 15.1-46427-1-S1 41ND( 0 . 1 5 )
4BA. 15.4-46427-2-S1 55
2B. 15.2-46427-1-S2H ND(0 .01 )
39
52
3B. 15.3-46427-1-S2L 52ND( 0 . 0 1 )
5B. 15 .5-46427-1-S2H 48ND[ 0 . 0 1 )
6B. 15 .6 -46427 -2 -S2L 58ND( 0 . 0 1 )
-'3. 1 5 . 7 - 4 6 4 2 7 - 2 - S 3 26ND( 0 . 0 1 )
NATIVE SPIKE7E. 15.7-46427-1-S3
NATIVE SPIKE RECOVERY
1. 3
98^
57
NATIVE SPIKE7F. 15.7-46427-1-S3
NATIVE SPIKE RECOVERY
1 . 9
1 0 1 %
53
8B. 15 .8 -46427 -2 -S3 51ND( 0 . 0 1 :
TABLE 4
SampleNumber
Wrigh^ Scace University
TetraChlcrcB-inzene Analyses
Column - DBS cOI-:, C . 25 , 0 . 25
Samples, levels - .-icrcgrams/g
Native Values(ppm)
TCB
Rec ( % ]C13TCB
NATIVE SPIKE7X. 15.7-46427-1-S3
NATIVE SPIKE RECOVERY
1.7
84^
44
NATIVE SPIKE9X . 15.10-46427-3-S2H
NATIVE SPIKE RECOVERY
2.1
107%
39
9 B . 15.10-46427-3-S2H 0.04 39
10B. 15.11-46427-3-S2L 0.12 48
11BA. 15.9-46427-2-S1 50
LAB BLANK LB11122-1 ND( 0 . 1 5 :
51
61
LAB BLANK LB11052-1 73ND; 0 . 0 1 ;
LAB BLANK LB11032-1 57ND( 0 . 0 1 )
LAB BLANK LB11112-1 53ND( 0 . 0 1 )
TCLP Metals f3•'^CO
Client: Soiltech ^Client Sample ID: 15.7-46427-1-S3 ^VISTA Sample ID: 925496-001 Sample Type: TCLP Leachate ^Date Sampled : 10/22/92 Date Received: 10/22/92TCLP Preparation: 10/26/92
Reporting DateAnalvte Result Limit Units Method Analyzed
Arsenic < 0.5 mg/L 6010 11/03/92Barium < 5 mg/L 6010 11/03/92Cadmium < 0.1 mg/L 6010 11/03/92Chromium < 0.1 mg/L 6010 11/03/92Lead < 0.5 mg/L 6010 11/03/92Mercury < 0.02 mg/L 7470 11/11/92Selenium < 0.5 mg/L 6010 11/03/92Silver < O.I mg/L 6010 11/03/92
< = Analyte not detected at or above the listed reporting limit.
1
TCLP ListChlorinated Herbicides ^
E?A Method 8150 ^-0C~>
Client: Soiltech §Client Sample ID: 15.7-46427-1-S3VISTA Sample ID: 925496-001 Sample Type: TCLP LeachateDate Sampled : 10/22/92 Date Received: 10/22/92TCLP Preparation: 10/26/92Date Extracted: 10/28/92 Date Analyzed: 11/05/92
Analvte
2,4-D2,4,5-TP (Silvex)
Surrogate Recoveries
2,4-DCPAA
ReportingResult Limit Units
< 120 ug/L< 17 ug/L
PC Limits
69 % 37-132
< = Compound not detected at or above the listed reporting limit.
2
TCLP ListSemivolatile organic compounds EPA Method 8270
Client: SoiltechClient Sample ID: 15.7-46427-1-S3VISTA Sample ID: 925496-001Date Sampled : 10/22/92TCLP Preparation: 10/26/92Date Extracted: 10/29/92
Sample Type: TCLP LeachateDate Received: 10/22/92
Date Analyzed: 11/04/92
Analvte
m & p-Cresolso-Cresol1,4-Dichlorobenzene2,4-DinitrotolueneHexachlorobenzeneHexachlorobutadieneHexachloroethaneNitrobenzenePentachlorophenolPyridine2.4.5-Trichlorophenol2.4.6-Trichlorophenol
Surrogate Recoveries
Nitrobenzene-dg2-FluorobiphenylTerphenyl-d.,4Phenol-dg2-Fluorophenoi2,4,6-Tribromophenol
ReportingResult Limi
2020202020202020100202020
567274211773
%
Units
ug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/L
PC Limits
10-14210-10936-11510-12110-12610-140
< = Compound not detected at or above the listed reporting limit.
TCLP Metals C3?i'5CO
Client: Soiltech C5Client Sample ID: 15.8-46427-2-S3 0VISTA Sample ID: 925496-002 Sample Type: TCLP Leachate ^Date Sampled : 10/22/92 . Date Received: 10/22/92TCLP Preparation: 10/26/92
Reporting DateAnalvte Result Limjt Units Method Analyzed
Arsenic < 0.5 mg/L 6010 11/03/92Barium < 5 mg/L 6010 11/03/92Cadmium < 0.1 mg/L 6010 11/03/92Chromium < 0.1 mg/L 6010 11/03/92Lead < 0.5 mg/L 6010 11/03/92Mercury < 0.02 mg/L 7470 10/29/92Selenium < 0.5 mg/L 6010 11/03/92Silver < O . I mg/L 6010 11/03/92
< = Analyte not detected at or above the listed reporting limit.
4
TCLP ListChlorinated Herbicides 02
ERA Method 8150 ;/5COC-3
Client: Soiltech 0Client Sample ID: 15.8-46427-2-S3 0VISTA Sample ID: 925496-002 Sample Type: TCLP LeachateDate Sampled : 10/22/92 Date Received: 10/22/92TCLP Preparation: 10/26/92Date Extracted: 10/28/92 Date Analyzed: 11/05/92
Analvte
2,4-D2,4,5-TP (Silvex)
Surrogate Recoveries
2,4-DCPAA
ReportingResult UB±£ 9nAtS
< 120 ug/L< 17 ug/L
PC Limits
66 % 37-132
< = Compound not detected at or above the listed reporting limit.
TCLP ListSmivolatile Organic Compounds EPA Method 8270
Client: SoiltechClient Sample ID: 15.8-46427-2-S3VISTA Sample ID: 925496-002Date Sampled : 10/22/92TCLP Preparation: 10/26/92Date Extracted: 10/29/92
Sample Type: TCLP LeachateDate Received: 10/22/92
Date Analyzed: 11/04/92
Analvte
m & p-Cresolso-Cresol1,4-Dichlorobenzene2,4-DinitrotolueneHexachlorobenzeneHexachlorobutadieneHexachloroethaneNitrobenzenePentachioropheno1Pyridine2.4.5-Trichlorophenol2.4.6-Trichlorophenol
Surrogate Recoveries
Nitrobenzene-dg2-FluorobiphenylTerphenyl-d^Phenol-dg2-Fluorophenol2,4,6-Tribromophenol
ReportingP^sult LiffiJA
2020202020202020
100202020
628176242075
Units
ug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/L
PC Limits
10-14210-10936-11510-12110-12610-140
< = Compound not detected at or above the listed reporting limit.
Uright State University
BCD Treatment of SoilTech ATP Systems, Inc. Condensates
Target Chemical Concentrations
2Sample
Vertac Site Samples Prior to SoilTechSOI2-1 SoilS012-4 SoilS012-11 Carbon
Condensate Phases Following SoilTech 1SOI2C-12B Solid PhaseSOI2C-12D Water Phase
Cootxned SoilTech Oil Condensates andS012C-12GAS012C-12HAS012C-12IA
Combined SoilTech Oil Condensates andSOI2C-12GBSOI2C-12HBSOI2C-12IB
Combined SoilTech Oil Condensates andS012C-12GCSOI2C-12HCS012C-121C
'378-TCOO(ng/g)
Treatment293912
0.45
'reatment of48905.6
Hater-Solid352040603810
Mater-SolidN0(0.534)N0(0.223)N0(0.152)
Uater-SolidN0(0.184)N0(0.258)N0(0.188)
24-0 HE(M9/9)
0.121721
Vertac Samples210027
Fraction Extracts10501150940
Fraction ExtractsN0(0.04)N0(0.03)N0(0.03)
Fraction ExtractsN0(0.08)N0(0.03)N0(0.30)
245-T ME(M9/9)
N0(0.03)2845
4455.7
Prior to BCD194198209
Following SCON0(0.07)N0(0.02)N0(0.07)
Following BCDN0(0.04)N0(0.04)N0(0.70)
Silvex ME(W/g)
ND(0.03)239
310.8
Treatment (Split irIS1616
Treatment - InternND(0.04)N0(0.02)N0(0.04)
Treatment - FinalN0(0.04)N0(0.03)N0(0.10)
Mono-CP
(w/g)
N0(0.5)9.5160
122002120
no Three Aliquot!450003000037400
nediate TreatmentN0(200)N0(100)N0(150)
Treated ProductsN0(120)N0(250)N0(100)
Di-CP(M/8)
N0(0.3)6.73250
40800680
»460003050046700
StageN0(45)N0(15)N0(30)
N0(20)N0(80)N0(15)
Tri-CP(M/g)
N0(1.0)96
1300
860044
667083007400
N0(75)N0(25)N0(35)
N0(25)N0(80)N0(20)
N0(0.15)55SO
510680(50
N0(0.5)N0(0.2)N0(0.4)
N0(0.2)N0(0.8)N0(0.2)
Tetra-CT(w/g)
1660.8
Uright State University
BCD Treatment of SoitTech ATP Systems, Inc. Condensates
Total Quantities of Analytes and Calculated Percent Destruction of Target Chemicals Achieved by BCD Treatment
Sample
SoUTech Condensate Added to BCD
S012C-12G
SOI2C-12H
SOI2C-12I
BCD-Treated SoilTech Condensate
S012C-12G
SOI2C-12H
SOI2C-12I
BCD-Treated SoilTeck Condensate
S012C-12G
SOI2C-12H
SOI2C-12I
Percent Destruction Achieved in
S012C-12G
SOI2C-12H
SOI2C-12I
Percent Destruction Achieved in
S012C-12G
SOI2C-12H
SOI2C-12I
2378-TCDD
(ng)
Reactor
156886
179939
170917
- IntermediateND(71.2)ND(29.6)
ND(20.3)
• Final Treated
N0(26.4)
N0(36.8)
N0(27.0)
Intermediate Stage Products froro BCD
> 99.955
> 99.984
> 99.988
Final Products
> 99.983
> 99.980
> 99.984
24-D ME
(rg)
46799
50968
42168
Treatment Stage
N0(5.33)
N0(3.99)
N0(4.02)
Products
N0(11.5)
N0(4.28)
N0(43.1)
> 99.989
> 99.992
> 99.990
from BCD Treatment of
> 99.975
> 99.992
> 99.898
245-T HE
(M)
8647
8775
9376
N0(9.34)
N0(2.66)
N0(9.37)
N0(5.74)
N0(5.71)
N0(100)
Treatment of
> 99.892
> 99.970
> 99.900
SoilTech Condensate
> 99.934
> 99.935
> 98.929
Sitvex HE
(H>
669
709
718
N0(5.33)
N0(2.66)
N0(5.35)
N0(5.74)
N0(4.28)
N0(14.4)
SoilTech Condensate
> 99.202
> 99.625
> 99.254
> 99.141
> 99.396
> 98.001
Hono-CP
(M)
2005650
1329600
1677764
N0(26700)
N0(13300)
N0(20100)
N0(17200)
N0(35700)
N0(14400)
> 98.670
> 99.000
> 98.803
> 99.141
> 97.316
> 99.145
Di-CP
(•0)
2050220
1351760
2094962
N0(6000)N0(1990)
N0(4020)
N0(2870)
N0(11400)
N0(2150)
> 99.707
> 99.853
> 99.808
> 99.860
> 99.155
> 99.897
Tri-CP
(M)
297282
367856
331964
N0(10000)N0(3320)
N0(4690)
N0(3590)
N0(11400)
N0(2870)
> 96.635
> 99.097
> 98.589
> 98.793
> 96.896
> 99.135
Tetra-CB
(••)
22731
30138
20187
N0(66.7)N0(26.6)
N0(53.5)
N0(28.7)
N0(114)
N0(28.7)
> 99.707
> 99.912
> 99.735
> 99.874
> 99.621
> 99.858
000863
"3CO
OA/OC C"30
QA/QC measures incorporated in the analytical procedures S3applied in this study included the preparation and analyses ofMatrix Spike (MS) and Matrix Spike Duplicate (MSD) samples. Actualsamples of the SoilTech-treated soils and of the BCD-treatedproduct residues were spiked with known quantities of the targetanalyte compounds prior to analyses. The percent recoveries of thespiked native compounds achieved in these analyses are a measure ofthe accuracy of the analyses* The agreement obtained between theanalytical results for the MS and MSD samples (Relative PercentDifference or RPD) is a measure of the precision of the analyses*
Table 1 and 2 attached herewith show comparisons of theanalytical data obtained in this study for the MS and MSD samples,and the calculated RPD's. As can be seen, the agreement isexcellent, the RPD's ranging from 0% to 25%, most of these beingless than 151. This is well within the range typically achievedusing the analytical methods applied here. A direct comparison ofthese results with representative data cited in the U . S . EPAmethods is not possible, since in the published methods, precisiondata are generally cited in terms of Relative Standard Deviation orRSD, based on several analyses. In the present study, the projectplan specified only two QA/QC eamplac.
Tables 3 and 4 attached herewith show the percent recoveriesof spiked target compounds achieved in the analyses of the MS andMSD samples. Tables 5, 6 and 7 compare these results with recoverydata cited in the analytical methods, although no data is reportedfor actual samples of the type analyzed here. Generally, thecomparisons indicated in Tables 5, 6 and 7 show reasonableagreement between the recovery data obtained in the presentanalyses and the typical data cited in the published analyticalmethods. The results obtained for 2,3,7,8-TCDD in the spiked BCD-treated products are well outside the expected range, but as notedin the table, this is due to the fact that the lev<sl of the addedspike was too low considering the magnitude of interferences fromextraneous compounds in the sample matrix. Of course, there is noway to forecast such interferences prior to spiking and analyses.
TABLE 1
WRIGHT STATE UNIVERSITY
Precision of Duplicate Matrix Spike Sanple Analysesfor Samples Treated by SoilTech ATP Systems, Inc.
Measured Target Chemical Concentrations
M—rix Spike Sample
SPK 15.7-46427-1-S3
SPK 15.7-46427-1-S3
TH 15.7-46427-1.53
71 l5.7-4M27.l-S3
7B 15.7-46427-1 S3
7F 15.7-46427-1-53
RPD"
2,3.7,8-TCDD•tft
0.0256
0.0000
15.8%
2,4 D MEre^e.
1.1
I.I
0.0ft
2,4,5-T MEwts
1.0
09
10.5ft
Silvcx MErsfs
0.7
0.6
15.4X
Mon»<Twis
1.4
1.3
7.4»
Di-CPMfK
Z7
2.4
11.8ft
TC-CPM/B
2.7
2.1
2S.O«
Tctra-CBfSf6
1.8
1.9
5.4«
a. Precision calculated as the Relative Percent Difference (RPD)
RPD =- (D, - Di)/((Di + D^/2] X 100
TABLE 2
WRIGHT STATE UNIVERSITY
Precision of Duplicate Matrix Spike Saxple Analysesfor Combined SoilTech Oil Concentrates and Water-Solid Fraction Extracts
Following BCD Treatment
Measured Target Chemical Concentrations
Mirix Spike Sampk
Spike 1 - Sample 3
Spike 2 - S—nple 3
S012C - 12ICD
SOEC - 121CE
S012C - 12ICFA
SOI2 - 121CGA
BPD"
2,3,7.8-TCDD"S/B
1.91
2.10
9.5%
2,4-D ME(*B^
1-21
1.24
2.4%
2,4,5-T ME
ItlS/S
1.46
1.82
22.0%
Sit'-ex ME
nis
1.10
1.37
21.8ft
Mono-CP?e/e
20t
247
19.1
Di-CP»»fi/S
168
111
^A%
Tri-CP
"6/S
172
\T9
4.0ft
TclnhCBrite.
2.13
13S
53ft
a. Preci»ion calcutetod u the Relative Percent Diffcrcnoc (HPD)
RPD = (D, - D^l(Di + D,)/21 X 100
009867
TABLE 3
WRIGHT STATE UNIVERSITY
Percent Recovery of Target Chemicals from Duplicate Matrix Spike Saaple Analysesfor Samples Treated by SoilTech ATP, Inc
____________________ ____ Percent Recovery___________________MNrix Spite Simple
SPK 15.7-46427-1-S3;
SPK 15.7-46427-lnS3
7H15.7-46427-1-S3
'»! 15.7-46427-1-S3
7E 15.7-46427-1-S3
7F 15.7-46427-1-S3
2,3.7,8-TCDD
52%
61%
2.4-DME
107%
116%
2,4>-T MB
101%
95%
SilvexME
72%
62%
MOM-CP
148ft
140ft
Di-CP
146ft
125ft
IW-CP
143ft
lllft
Tetra-CB
9Kft
101ft
TABLE 4
WRIGHT STATE UNIVERSITY
Percent Recovery of Target Chemicals from Duplicate Matrix Spike Sawple Analysesfor Combined SoilTech Oil Condensates and Water-Solid Fraction Extracts
Following BCD Treatment
Percent RecoveryMitrix Spftc Sunpk*
Spike 1 - final TrcM. Sam. A
Spike 2 - Final Treat. Sara. <B
SOI2C - 12ICD
SOQC - 121CE
SOI2C - 12ICFA
SOG - 121CGA
2.3,7,8-TCDD
212<*
243%-
2.4-D ME
69%
71 %
2,4.5-T ME
83%
104%
SilvcxME
63ft
TS%
Mono-CP
\9W
2301.*
DfrCP
78ft
84ft
Tri-CP
80ft
83ft
Tkm-CB
99ft
105ft
a. Cniiocatntlion of Mthre ipflcc was loo low to give reliable recovery inrnnralion for Ibis nrmtrix.
b. Chcnaical interfcicaceii enbmccd recovery for this sample.
000869
TABLE 5
WRIGHT STATE UNIVERSITY
Percent Recoveries of Herbicides Achieved in Analysesof Spiked SoilTech-Treated and BCD-Treated Samples
As Compared to Representative Recoveries Cited in U.S. EPA SW846, Method 8270A
_________________ Average Percent Recoveries ___ _____________
Target Chemical
2,4-D ME
2,4,5-T ME
Silvex ME
Representative DataCited in
SW846. Method 8150A"
72%
82%
83%
SoilTech TreatedSanples
112%
98%
67%
BCD Treated Samples
70%
94%
71%
a. Average recovery of target chemicals from organic-free reagent water and effluents from publiclyowned treatment works.
000870
TABLE 6
WRIGHT STATE UNIVERSITY
Percent. Recoveries of Chlorophenols Achieved in Analysesof Spiked SollTech-Treated and BCD-Treated Samples
As Compared to Representative Recoveries Cited in U.S. EPA SW846, Method 8270A
Target Chemical
Mono-CP
Di-CP
Tri-CP
Ropres^p.tative DataCited in
SW846, Method 8270A"
78S
87%
91%
SoilTech TreatedSamples
.1.44%
136%
127%
BCD Trs&ted Sanples
210t
81%
82%
a. Based on a spike of 5000ng/0.047g and using the correction factor listed in SW846, Method 8270A,Table 2, to adjust the sample size.
Recovery as a Function of ConcentrationMono-CP 0.78C + 0 . 2 9Di-CP 0.87C - 0.13Tri-CP 0.91C - 0.18
SW846, Metliod 8270A average recoveries of target, chemicals fron organic-free reagent water,drinking water, surface water and industrial vastevaters using Method 8250.
000871
TABLE 7
WRIGHT STATE UNIVERSITY
Percent Recoveries of 2,3,7,8-TCDD Achieved in Analysesof Spiked SoilTech-Treated and BCD-Treated Sanples
As Compared to Representative Recoveries Cited in U.S. EPA SN846, Method 8280
Average Percent Recove'-iss
Target Che»ica.l
2,3,7.8-TCDD
Hepresentative DataCited in
SW846, Method 8280
„ *
SoilTech TreatedSanples
57%
BCD Treated Sanples
2281
a. SW846, Method 8280 does not include recovery data for the still bottom »atrix. Tills is the matrixin SN846, Method 8280, Table 6 that most closely matches the SoilTech treated samples and the BCDtreated samples•
000872
TCLP Metals
Client: SoiltechClient Sample ID: NAVISTA Sample ID: 925496-Blank Sample Type: WaterDate Sampled : NA Date Received: NA
Reporting DateAnalvte Result Limit Units Method Analysed
Arsenic < 0.5 mg/L 6010 11/03/92Barium < 5 mg/L 6010 11/03/92Cadmium < 0.1 mg/L 6010 11/03/92Chromium < 0.1 mg/L 6010 11/03/92Lead < 0.5 mg/L 6010 11/03/92Mercury < 0.02 mg/L 7470 10/29/92Selenium < 0.5 mg/L 6010 11/03/92Silver < O . I mg/L 6010 11/03/92
NA = Not Applicable< = Analyte not detected at or above the listed reporting limit.
TCLP Mfttala IT:!>•CO
Client: Soiltech C">Client Sample ID: HA 0VISTA Sample ID: 925496-Blank Sample Type: TCLP Leachate ®Date Sampled : NA Date Received: NATCLP Preparation: 10/26/92
Reporting DateAnalvte Result Limit Units Method Analyzed
Arsenic < 0.5 mg/L 6010 11/03/92Barium < 5 ng/L 6010 11/03/92Cadmium < 0.1 mg/L 6010 11/03/92Chromium < 0.1 mg/L 6010 11/03/92Lead < 0.5 mg/L 6010 11/03/92Mercury < 0.02 mg/L 7470 10/29/92Selenium < 0.5 mg/L 6010 11/03/92Silver < O.I mg/L 6010 11/03/92
< = Analyte not detected at or above the listed reporting limit.
9
Quality Assurance cTCLP Metals T>
Duplicate Analyses COC-50
Client: Soiltech ®Client Sample ID: NAVISTA Sample ID: NA Sample Type: TCLP LeachateDate Sampled : NA Date Received: 10/22/92
Analvte
ArsenicBariumCadmiumChromiumLeadMercurySeleniumSilver
Sample DuplicateResult Resultfma/L^ fmq/L) BED
NANA
NDNDNDNDNDNDNDND
NDNDNDNDNDNDNDND
NANANANANANA
Method
60106010601060106010747060106010
RPD = Relative Percent DifferenceND == Not detected at or above the reporting limit.NA = Not Applicable
10
£>•Quality Assurance r-.
TCLP M«f.lS c0Spike Sample ifoovry c~)
c.'0
Client: SoiltechClient Sample ID: NAVISTA Sample ID: NA Sample Type: TCLP LeachateDate Sampled : NA Date Received: NA
Analvte
ArsenicBariumCadmiumChromiumLeadMercurySeleniumSilver
Spike Sample Spike QCAdded Cone. Cone. Limitsfma/L^ fma/L) fma/Ll % Rec ^ Reg
ND 5.45 109 75-1255.0100
1.05.05.00.201.05 . 0
ND 103 103 75-125ND 1.06 106 75-125ND 5.47 109 75-125ND 5.30 106 75-125ND 0.177 89 75-125ND 1.05 105 75-125ND 3.13 63 50-150
NA = Not ApplicableND = Not detected at or above the reporting limit.
11
Quality AssuranceTCLP Htttals
Laboratory Control sample Results
Client: SoiltechVISTA Sample ID: 925496-LCS
Analvte
ArsenicBariumCadmiumChromiumLeadMercurySeleniumSilver
True Sample QCValue Result Limitsfmq/L) fmq/L) ^ Rec % Pec
5.0 5.60 112 75-125100 118 118 75-125
1.0 1.12 112 75-1255.0 5.85 117 75-1255.0 5.80 116 75-1250.20 0.208 104 75-1251.0 1.14 114 75-1255.0 3.07 61 50-150
12
TCLP ListChlorinated Herbicides °
EPA Method 8150 i>
COCT
Client: Soiltech °Client Saaple ID: NA —3VISTA Sample ID: 925496-Blank Sample Type: TCLP LeachateDate Sampled : NA Date Received: NATCLP Preparation: 10/26/92Date Extracted: 10/28/92 Date Analyzed: 11/05/92
Analyt?
2,4-D2,4,5-TP (Silvex)
Surrogate Recoveries
2,4-DCPAA
ReportingRe?m LiffiJA Units
< 120 ug/L< 17 ug/L
<?c Limit?
68 % 37-132
NA = Not Applicable< = Compound not detected at or above the listed reporting limit.
14
Quality AssuranceChlorinated Herbicides - Method 8150Matrix Spike Recovery and Precision
Client: SoiltechClient Sample ID: NAVISTA Sample ID: 925496-BLSPDate Sampled : NATCLP Preparation: 10/26/92Date Extracted: 10/28/92
Sample Type: TCLP LeachateDate Received: NA
Date Analyzed: 11/05/92
Comoound
2,4-D2,4,5-TP (Silvex)
SpikeAddedfuq/Ll
202.0
SampleCone.fua/Ll
NDND
MSCone.fuq/Ll
1 9 . 61.95
MS^ R<?c
9898
QCLimits% Rec
10-13021-136
Compound
2,4-D2,4,5-TP (Silvex)
Spike MSOAdded Cone. MSDfuq/L) ^uq/I^ % Rec RPD
QCLimitsRPD % Rec
202.0
19.11.85
9693
6141
10-13021-136
NA = Not ApplicableND = Not DetectedMS = Matrix SpikeMSD = Matrix Spike DuplicateRPD = Relative Percent Difference
15
TCLP ListSeaivolatile Organic Compounds ERA Method 8270
Client: SoiltechClient Sample ID: NAVISTA Sample ID: 925496-BlankDate Sampled : NADate Extracted: 10/29/92
Sample Type: WaterDate Received: NADate Analyzed: 11/04/92
Analvte
m & p-Cresolso-Cresol1,4-Dichlorobenzene2,4-DinitrotolueneHexachlorobenzeneHexachlorobutadieneHexachloroethaneNitrobenzenePentachlorophenolPyridine2.4.5-Trichlorophenol2.4.6-Trichlorophenol
Surrogate Recoveries
Nitrobenzene-dg2-FluorobiphenylTerphenyl-d,4Phenol-d,2-Fluorophenol2,4,6-Tribromophenol
ReportingResult LifflJJc
2020202020202020
100202020
787876496593
vnitsug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/L
PC Limits
37-9534-9548-10010-5310-7910-149
NA = Not Applicable< = Compound not detected at or above the listed reporting limit.
16
TCLP ListSemivolatilft organic Compounds EPA Method 8270
Client: SoiltechClient Sample ID: NAVISTA Sample ID: 925496-BlankDate Sampled : NATCLP Preparation: 10/26/92Date Extracted: 10/29/92
Sample Type: TCLP LeachateDate Received: NA
Date Analyzed: 11/04/92
Analvte
n & p-Cresolso-Cresol1,4-Dichlorobenzene2,4-DinitrotolueneHexachlorobenzeneHexachlorobutadieneHexachloroethaneNitrobenzenePentachlorophenolPyridine2.4.5-Trichlorophenol2.4.6-Trichlorophenol
Surrogate Recoveries
Nitrobenzene-dg2-FluorobiphenylTerphenyl-d.,4Phenol-d,2 -Fluoropheno12,4,6-Tribromophenol
ReportingResult LiffiJA
2020202020202020
100202020
7082806361
110
Units
ug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/Lug/L
W Limits
10-14210-10936-11510-12110-12610-140
NA = Not Applicable< = Compound not detected at or above the listed reporting limit.
17
Quality AssuranceSeaivolatir orgaaics - E?A Method 8270Matrix Spika Recovery and Precision
Client: SoiltechClient Sample ID: NAVISTA Sample ID: 925496-BLSPDate Sampled : NADate Extracted: 10/29/92
Sample Type: WaterDate Received: NADate Analyzed: 11/04/92
• AddedCompound
Phenol2-Chlorophenol1,4-DichlorobenzeneDi-n-propylnitrosamine1,2,4-Trichlorobenzene4-Chloro-3-methylphenolAcenaphthene4-Nitrophenol2,4-DinitrotoluenePentachlorophenolPyrene
Comoound
Phenol2-Chlorophenol1,4-DichlorobenzeneDi-n-propylnitrosamine1,2,4-Trichlorobenzene4-Chloro-3-methylphenolAcenaphthene4-Nitrophenol2,4-DinitrotoluenePentachlorophenolPyrene
Spike
fucr/Ll
400400200200200400200400200400200
SpikeAddedfuo/L)
400400200200200400200400200400200
SampleCone.
ruc/Ll
NDNDNDNDNDNDNDNDNDNDND
MSDCone.
fua/L)
260290112176132261147224163320128
MSCone.
(W/L1
275307127167144278173238173320132
MSD% Rec
6573568866657456828064
MS% Rec
6977648472708760878066
RPD
65
13597
167603
QCLimits
% Rec
10-7724-9825-8932-10129-9821-11035-12810-7815-11334-11840-114
QCLimits
RPD % Rec
20 10-7714 24-9815 25-8920 32-10117 29-9828 21-11018 35-12850 10-7824 15-11322 34-11823 40-114
NA = Not ApplicableND = Not DetectedMS = Matrix SpikeMSD = Matrix Spike DuplicateRPD = Relative Percent Difference
18