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Project 92-229-02 February 1993 CanonieEnvironmenlal S Draft Report Dechlorination Treatability Study SoilTech Anaerobic Thermal Process and Base Catalyzed Decomposition ••'ertac Site ^acKsonviile, .Arkansas ^reoared For: Hercules incorporated Wilmington, Delaware

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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

'y<%'SO

PAGE o0

1

2

3

4

4

5

9

9

10

10

12

12

14

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

PH/W:/82-228/TBEAT.RPT IFcbniwy 24. 18831

TABLE OF CONTENTS

(Continued)

0OS^0000

PAGE

5.0 CONCLUSIONS AND RECOMMENDATIONS

TABLES

FIGURES

APPENDICES

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37

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

2

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).

PRW:/92-229/TBEAT.HPT IFtbruwy 23. 1993]

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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.

PWW:/92-229/TBEAT.RPT IF«bru*ry 23, 10931

5

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

t.06 s00

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

PR/W:/92-22»n-f»EAT.RPT IFfbruTv 23. 18831

CanonieEnvironmental

"-?0 2>8 0

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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

CanonieEnvironmen-tal

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^T.

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.

PRAV:/92-22a<TREAT.RPT IFebruwy 23. 19831

CanonieEnvironmental

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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

1 3 SM-^5>

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.

PfUW^»2-22B/TREAT.RPT IFtbrufy 23. 1B931

CanonieEnvironmental

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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.

PWW:/92-229/TREAT.RPT IFfbruwy 23, 19031

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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.

PR/W-J92-229/TREAT.RPT lP«bruwy 24. 19831

CanonieEnvironmental

17 ^T»»

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.

PRJW:/82-228/TREAT.RPT [Fabrufy 24, 1fl831

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

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SCALE NONE

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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

OOOTSQ

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

APPENDIX A

ATP AND BCD TB&ATABILITY STUDYPHOTOGRAPHS

CanonieEnvironmental

SOILTECH ATP SYSTEM TREATABILITY TEST PHOTOGRAPHS

SoUTech ATPBench Scale Test Unit"nn^

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.

^er ramp -, paroon sa^P'® °

Spent car"^

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,

BCD TREATABILITY TEST PHOTOGRAPHS

BCD treatment apparatus

BCD round bottom reaction flask with recycling Dean & Stark-type receiver.

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

HAZEN RESEARCH, INC.SOILTECH ATP SYSTEM, VERTAC TREATABILITY STUDY

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^

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-'

APPENDIX

Hazen Research, Inc.

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.

HE-TS-419-SSX-01Composite Combustion

15.8-46427-2-S3

Hazen Research, Inc.

. •

,. ^•-1-0^-"'

^w v "',^^--\-

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reject No.——__ ^ ^ ;Book No._[4o^_ TITLE Lo^/tO^.^ ^CX^DU^

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( '• '•( 'S^i <?-r ^^L'-c/.-f-DaAzr ^(as^J -^[k^r-.. . - .- - -.. -...-.-.-. -

To Page No. l_

Witnessed & Understood by me.

Recorded by J J

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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)

ATP SYSTEMTREATABILITY STUDY ANALYTICAL RESULTS

TABLE 1

w

Concern

CAfiONIE ENV. ;5;5BSaioleNuioer

1AAA. l;.;-i642:-:-;l

4AAA. 15.4-46t27-:-:'l

2A. 15.2-46427-1-S2H

3A. 15.3-46427-1-52.

5A. 15.5-46427-2-S2H

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

LAB BLANK ( B )

•rigr.: 5;

suits 3t I

[rations i

Colu

heightg a.

0.012002.00998

20.55

20.02

20.19

20.20

20.67

20.40

20.29

20.21

0.00980

20.00

t2t* .r.i

;C;.1£ AT:WlS in

«•• - :.liaer

"7?

:mt.

.leas.

:?3

512

NO

NO

0.0870

0.053i

W

a.0256

0.0300

SO

SO

so

versity, 3a'

arses •;f £,

anograas cei

£5 sM '.;o-;;'i': api

i '«•'•

Found?PB

lOCc.

-

-

0.0014

0.0087

-

-

0.0010

-

-

3.0019

5.00

0.0006

f.y.. 3-.

f.racti

• vai o

Z.;5uii>Sii

instr.ID

ns-;5•1S-25

ns-25flS-25

ns-25ns-25ns-25ns-25ns-25ns-25HS-25

ns-25

.C 4Cbv:

•;r ::•

• iaDCie 1

;ate

.1/20/5:i * AA lyi.-.iivni.

11/13/92

11/13/92

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.

BCD PROCESSTREATABILITY STUDY ANALYTICAL RESULTS

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

QUALITY ASSURANCE ANALYTICAL SUMMARY

"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

QUALITY ASSURANCE

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