ONS8TE ENGINEERING REPORT
FOR SOLIDIFICATION/STABILIZATION
TREATMENT TESTING OF
CONTAMINATED SOILS
by
IT Environmental Programs, Inc.
(formerly PEL Associates, Inc.) i
Cincinnati, OH 45246 ;
Contract No. 68-C9-0036 i
Technical Project Monitor i
Richard P. Lauch
Water and Hazardous Waste Treatment Research Division
Risk Reduction Engineering Laboratory
Cincinnati, Ohio 45268
RISK REDUCTION ENGINEERING LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
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DISCLAIMER
This material has been funded wholly or jn part by the United States Environ-
mental Protection Agency under Contract 6&-C9-0036 to IT Environmental Programs,
Inc. It has been subject to the Agency's review and it has been approved for publica-
tion as an EPA document. Mention of trade names or commercial products does not
constitute endorsement or recommendation1 for use.
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FOREWORD
Today's rapidly developing and changing technologies and industrial products
and practices frequently carry with them the increased generation of materials that, if
improperly dealt with, can threaten both public health and the environment. The U.S.
Environmental Protection Agency (EPA) is charged by Congress with protecting the
Nation's land, air, and water resources. Under a mandate of national environmental
laws, the Agency strives to formulate and implement actions leading to a compatible
balance between human activities and the ability of natural systems to support and
nurture life. These laws direct the EPA to perform research to define our environ-
mental problems, measure the impacts, and search for solutions.
I
The Risk Reduction Engineering Laboratory is responsible for planning,
implementing, and managing research, development, and demonstration programs to
provide an authoritative, defensible engineering basis in support of the policies,
programs, and regulations of the EPA with respect to drinking water, wastewater, .
pesticides, toxic substances, solid and hazardous wastes, and Superfund-related
activities. This publication is one of the products of that research and provides a vital
communication link between the researcher and the user community. :
This report describes the results of a pilot-scale test of the solidification/
stabilization technology for treatment of a lead-contaminated soil. The data will be
used to develop best demonstrated available technology (BOAT) standards for con-
taminated soil in support of the land disposal restrictions under the 1984 RCRA
Hazardous and Solid Waste Amendments. '
E. Timothy Oppelt, Director '.
Risk Reduction Engineering Laboratory
in
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ABSTRACT
The EPA's Office of Solid Waste and Emergency Response (OSWER) is
currently developing land disposal restrictions (LDRs) for contaminated soil and debris
(CS&D). The Office of Research and Development, through its Risk Reduction
Engineering Laboratory (RREL), is providing' support to OSWER by supplying technical
data on the performance of selected types of technologies for CS&D treatment.
Based on the technical data supplied by RREL and other data obtained from inde-
pendent sources, OSWER will prepare a regulatory package that establishes BOAT
standards for the level of CS&D treatment required prior to land disposal.
IT Environmental Programs (ITEP) is providing RREL with technical data on the
solidification/stabilization (S/S) treatment technology. This treatment process is
designed to achieve one or more of the following objectives:
Improve handling and physical characteristics of the waste by producing
a solid from liquid or s.emi-liquid wastes.
Reduce contaminant solubility jn the treated waste.
i
Decrease the exposed surface area across which transfer or loss of
contaminants may occur. ;
A pilot-scale test of the S/S technology was conducted in Cincinnati, Ohio, in
coordination with IT Corporation and the University of Cincinnati. The test was
conducted in two phases. Phase I took place February 20 through April 10, 1991, and
Phase II, June 6 through July 5, 1991. Thre'e different binders (portland cement, a
cement kiln dust and fly ash mixture, and a fly ash and quicklime mixture) were used
in three binder-to-soil ratios each to determine the optimum mixtures for stabilizing
lead in soil from the Brown's Battery Breaking Site in Tilden Township, Pennsylvania.
The following binders were able to reduce the leachable lead content of the soil to less
than 5 mg/L: 45% portland cement, 139.5% kiln dust and fly ash, 77.5% fly ash and
quicklime, and 20% portland cement on soiljthat was heated prior to treatment to
remove organic carbon from the soil. This report presents detailed information
concerning the operation and sampling andianalysis of the solidification/stabilization
treatment process. I
This report was submitted in fulfillment of Contract No. 68-C9-0036 by IT Envi-
ronmental Programs, Inc., under the sponsorship of the U.S. Environmental Protection
Agency. This report covers a period from t October 1989 to 31 March 1992, and
work was completed as of 31 March 1992.
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CONTENTS
Volume I ,
Disclaimer .. ,. 1 jj
Foreword ,."..•; . . i jjj
Abstract '. jv
Figures ....;. vii
Tables . . ; viii
List of Acronyms : xi
Acknowledgment : xiii
1, Introduction '• 1-1
2,, Contaminated Soil Under Evaluation 2-1
3,, Treatment System Under Evaluation i 3-1
3.1 Description of Treatment I . 3-1
. 3.2 Experimental Design . : 3-3
4. Sampling and Analysis Activities : . ; 4-1
4.1 Sampling Methods .... j ....... 4-2
4.2 Analytical Procedures 4-16
4.3 Deviations From the Sampling and Analysis Plan , . . . . i 4-22
4.4 Health and Safety 4-22
!
5. Design and Operating Data Collection j 5-1
5.1 Binder/Water Addition .......;.. 5-1
5.2 Fractionation and Cold Acid Digestion 5-12
5.3 Set Testing 5-13
6. Analytical Results 6-1
6.1 Lead .; 6-1
6.2 CS&D Constituents .: 6-25
7. Quality Assurance/Quality Control Measures j.-....'.. 7-1
7.1 Method Detection Limit for TCLP Lead ' 7-1
7.2 Accuracy Data j 7-1
7.3 Precision Data 7-2
7.4 Blank Data for Soil Analysis | 7-4
7.5 Analytical Prbblems i 7-4
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CONTENTS (cont.)
7.6 Deviations from Established Analytical Methods 7-4
8. Correspondence and Activities ... L. 8-1
I
Appendices j
(The Appendices are contained in a separate volume and can be obtained,
for a limited time, from the Technical Project Monitor).
I. Sections of the S/S Sampling and Analysis Plan Pertinent to the
Pilot-Scale Study .. i 1-1
II. S/S Sampling and Analysis Plan for Additional Treatment Testing 11-1
III. Outline for Writing On-Site Engineering Report 111-1
IV. Field-Portable X-Ray Fluorescence Standard Operating Procedure ....... IV-1
V. Raw Operating Data ;. V-1
i . • ;
VI. GANG Procedure '. . VI-1
VII. Toxicity Characteristic Leaching Procedure VII-1
VIII. TCLP Raw Extraction Data ,;.......>..-. VIII-1
IX. FAD Procedure „ . . ix-1
X. Binder/Soil/Water Mix Sheets i •".. x-1
XI. Analytical Data for Soil Samples From S/S Pilot-Scale Test XI-1
XII. Matrix Spike/Matrix Spike Duplicate Recovery Results XI1-1
vi;
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FIGURES
Number ; Page
2-1 Treatment Sample Locations for the S/S Treatability Study 2-3
2-2 Grain-Size Distribution for Brown's Battery Site , 2-5
3-1 Treatment Soil Sampling Procedures \ 3-2
3-2 Homogenization and Subsampling Procedure for the Raw Soil ... 3-4
5-1 GANG Curve for Raw Soil ! 5-2
5-2 GANG Curve for Type I Portland Cement ,'.. 5-3
5-3 GANG Curve for Quicklime ....... 5-4
5-4 GANG Curve for Fly Ash i 5.5
5-5 GANG Curve for Cement Kiln Dust ; 5-6
5-6 Mix Design for Portland Cement 5-7
5-7 Mix Design for Quicklime/Fly Ash i....... 5-8
!
5-8 Mix Design for Cement Kiln Dust/Fly Ash j 5-9
VII
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TABLES
* !
Number • Page
1-1 Key Personnel Involved in the Solidification/Stabilization Pilot-
Scale Test 1-4
2-1 XRF Total Lead Concentrations in the Six Flagged Areas 2-4
2-2 XRF Total Lead Concentrations in the Containerized Samples 2-4
2-3 Sieve and Hydrometer Analysis ! 2-6
2-4 Summary of Analytical Results (detected Constituents) for the
Characterization Samples Collected at Brown's Battery Breaking
Site, Tilden Township, PA ...!.... 2-7
2-5 Key Personnel Involved in the Excavation of Treatment Soil ........ 2-9
[
4-1 CS&D List by Constituent Type j 4-4
. 4-2 Required Sample Containers, Preservation Methods, and
Holding Times 4-17
4-3 Preparation and Analytical Methods 4-19
5-1 Water Requirements and Flow Achieved Mixes 1 Through 6 5=10
5-2 Water Requirements and Flow Achieved Mixes 7 Through 10 5-12
5-3 Setting Measurements on Mixes 1 to 10 5-14
5-4 Physical Characteristics of Cast Samples 5-16
6-1 Sample Tracking Information 6-2
6-2 Perkin-Elmer Plasma II Emission Spectrometer Operating
Conditions for Analysis of TCLP Lead 6-12
6-3 Concentration of Total Lead by FAD Extraction in Raw Untreated
Soil [ 6-14
viii
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TABLES (cont)
Number
6-4 Concentration of Total Lead by FAD Extraction in Binder/Soil
Mixtures From Phase I ; 6-14
6-5 Concentration of Total Lead in Digested Solids by FAD
Extraction in Raw Untreated Soil 6-15
i
6-6 Concentration of Total Lead in Digested Solids by FAD
Extraction in Binder/Soil Mixtures from Phase I 6-15
6-7 Comparison of Predicted and Actual Lead Concentrations by
FAD Extraction in Binder/Soil Mixtures . . 6-17
6-8 TCLP pH Levels in Pretreatment Soil Samples From Phase I ........ 6-17
6-9 TCLP Lead Concentrations in Pretreatment Soil Samples from
Phase I 6-18
6-10 TCLP pH Levels in Posttreatment Soil Samples from Phase I ...... 6-18
6-11 TCLP Lead Concentrations in Posttreatment Soil Samples from
Phase I . f 6-19
6-12 TCLP pH Levels in Pretreatment Soil Samples From Phase II 6-21
6-13 TCLP Lead Concentrations in Pretreatment Soil Samples from Phase II 6-22
6-14 TCLP pH Levels in Posttreatment Soil Samples From Phase II 6-23
6-15 TCLP Lead Concentrations in Posttreatment Soil Samples from
Phase II 6-24
6-16 Percent Reduction of TCLP Lead by Treatment With S/S . . j 6-26
6-17 Comparison of TCLP Lead Concentrations in Ashed and Nonashed
Soil Treated With Portland Cement at a Binder-to-Soil
Ratio of 20 Percent 6-26
6-18 Analytical Results for CS&D Constituents Detected in the >
Treatment Soil Matrix '. 6-27
IX
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TABLES (cont.)
Number Page
7-1 Accuracy Data for TCLP Lead „ 7-3
7-2 Precision Data for TCLP Lead t . . . 7-3
7-3 Blank Data for TCLP Lead 7-5
7-4 Blank Data From the Analysis of Raw Soil Samples 7-6
8-1 Critical Activities and Correspondence 8-1
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ABBREVIATIONS, ACRONYMS, AND SYMBOLS
ASTM American Society for Testing and Materials
BOAT best demonstrated available technology
CERCLA Comprehensive Environmental Response, Compensation; and Liability
Act of 1980 (Superfund) |
CHF Center Hill Solid and Hazardous Waste Research Facility
cm2 square centimeters
CFR Code of Federal Regulations
CG&E Cincinnati Gas & Electric
ckd/fa cement kiln dust/fly ash !
CS&D contaminated soil and debris
DD dry density ;
EPA U.S. Environmental Protection Agency i
eq/kg equivalents per kilogram
FAD Fractionation Cold-Acid Digestion.
GANG Generalized Acid Neutralization Capacity
GFAA graphite furnace atomic absorption !
HSWA Hazardous and Solid Waste Amendments of 1984
ICAP inductively coupled argon plasma spectrometry '
ITAS IT Analytical Services i
ITEP IT Environmental Programs
kg kilograms '•
kg/m3 kilograms per cubic meter ;
kPa kilo Pascals
1 LDRs land disposal restrictions i
L/min liters per minute
MANC Metal Acid Neutralization Capacity \
1MDL | method detection limit
mg/L l milligrams per liter j
mg/kg milligrams per kilogram i
MS/MSD matrix spike/matrix spike duplicate
OER On-Site Engineering Report
ORD Office of Research and Development •
OSW Office of Solid Waste .!
OSWER Office of Solid Waste and Emergency Response
% M percent moisture content ' ;
PADER Pennsylvania Department of Environmental Resources '
pc portland cement >
XI
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ppm parts per million
QA/QC quality assurance/quality control
ql/fa quicklime/fly ash
RCRA Resource Conservation and Recovery Act
RI remedial investigation
RPD relative percent difference
RREL Risk Reduction Engineering Laboratory
SAP Sampling and Analysis Plan
S/S solidification/stabilization
TCL Target Compound List
TCLP Toxicity Characteristic Leaching Procedure
TOC total organic carbon !
TOX total organic halogen :
XRF X-ray fluorescence spectrophbtometry
UCS • unconfined compressive strength
WD wet density
XII
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ACKNOWLEDGMENT
This report was prepared for the U.S. Environmental Protection Agency, Office
of Research and Development, Risk Reduction Engineering Laboratory, Cincinnati,
Ohio, by IT Environmental Programs (ITEP) under Contract No. 68-C9-0036. Mr.
Richsird P. Lauch was the EPA Technical Project Monitor. The principal ^authors of this
report were Mr. Majid Dosani of ITEP and Dr. Alan Jones of ECOVA Corporation.
Other personnel contributing to the project were Ms. Judy Hessling (ITEP), Mr.
Michael Smith (ITEP), Mr. Ernie Grossman (U.S. EPA), Dr. William Mahaffey (ECOVA),
Ms. Madonna Brinkman (ECOVA), and Mr. Christopher Krauskopf (ECOVA).
XIII
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SECTION 1
INTRODUCTION
The 1984 Hazardous and Solid Waste Amendments (HSWA) to the Resource
Conservation and Recovery Act (RCRA) prohibit the continued land disposal of
untreated hazardous wastes beyond specified dates. The statute requires the U.S.
Environmental Protection Agency (EPA) to set "levels or methods of treatment, if any,
which substantially diminish the toxicity of the waste or substantially reduce the likeli-
hood of migration of hazardous constituents from the waste so that short-term and
long-term threats to human health and the environment are minimized."; The legislation
sets forth a series of deadlines beyond which further disposal of untreated wastes is
prohibited. Land disposal restrictions (LDRs) have been established for solvents and
dioxins; the California List; and first-, second-, and third-third hazardous wastes.
These LDRs establish concentration- or technology-based treatment standards that
must be met prior to land disposal of RCRA-regulated hazardous wastes. These treat-
ment standards also apply to soil and debris contaminated with these wastes at
uncontrolled hazardous waste sites under the Comprehensive Environmental
Response, Compensation and Liability Act (CERCLA or Superfund) and at RCRA
corrective-action and closure sites. ,
Contaminated soil and debris (CS&D) pose a special problem because of their
complexity and high degree of variability. As a result of these adverse waste charac-
teristics, the EPA has determined the need for a detailed evaluation of treatment tech-
nologies to develop separate LDR standards applicable to CS&D waste' disposal.
These standards are being developed through the evaluation of best demonstrated
available technologies (BDATs). Once these LDRs are promulgated, only CS&D
1-1
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wastes that meet the LDR standards will be permitted to be disposed of in land
P
disposal units unless a treatability variance lis issued.
The EPA's Office of Solid Waste and Emergency Response (OSWER) is in the
process of developing LDRs for CS&D. The Office of Research and Development
(ORD), through its Risk Reduction Engineering Laboratory (RREL), is supporting
OSWER by providing technical data on the performance of various technologies used
to treat CS&D. Based on the technical data provided by RREL, along with other data
obtained from independent sources, OSWER will prepare a regulatory package that
establishes BOAT standards for the level of CS&D treatment required prior to land
disposal. ;
i
In support of this activity, RREL is developing performance data on solidifica-
tion/stabilization (S/S) of contaminated soil. Solidification/stabilization refers to treat-
ment processes that are designed to achieve one or more of the following objectives:
i '
Improve handling and physical characteristics of the waste by producing
a solid from liquid or semi-liquid wastes.
i
0 . Reduce contaminant solubility in the treated waste.
Decrease the exposed surface area across which transfer or loss of
contaminants may occur. ! ,
i
The elimination of free liquid in the wastes increases the bearing strength of the
solidified material and assists in the formation of a monolithic solid product with high
structural integrity. Solidification techniques do not necessarily involve chemical
interactions between the waste and the solidifying agents; instead, the waste is me-
chanically bound within the solidified media. Stabilization techniques reduce the
hazardous potential of a waste material by Converting the contaminants into their least
soluble, mobile, or toxic form. Stabilization [processes may change the physical char-
acteristics of the wastes. I
i
This on-site engineering report (OER) describes the treatment of lead-
contaminated soil from the Brown's. Battery {Breaking Site in Tilden County, Pennsyl-
vania, by use of various S/S techniques. The University of Cincinnati, in coordination
1-2 - •' : ' ' , '
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with IT Corporation and under contract to EPA, performed pilot-scale tests at EPA's
Center Hill Solid and Hazardous Waste Research Facility (CHF) in Cincinnati, Ohio.
The purpose of the tests was to collect data that would be representative of data
obtained from a full-scale S/S demonstration. Specifically, the objective of the S/S
test was to obtain six sets of pre- and posttreatment sample data on the teachability of
lead as well as design and operating data that could be used to evaluate the perfor-
mance of the S/S treatment system. Three binders were evaluated in this study,
including portland cement, a cement kiln dust and fly ash mixture, and a quicklime and
fly asih mixture at two binder-to-soil ratios each (Phase I). Additional studies (Phase II)
were performed on the soil due to the failure of the six original binder mixes to
effectively stabilize lead. Phase II studies utilized three new binder mixtures to deter-
mine if lead in the Brown's Battery Breaking soil could be effectively treated by the
stabilization process. In addition, one portion of soil was heated to reduce the organic
content of the soil then treated with a binder to stabilize lead. This test ;was performed
to determine if the high organic carbon content of the soil (17 percent) had an adverse
effect on the original binder mixtures' ability to stabilize the lead present in the soil.
This report details the results of the S/S treatment study. The procedures fol-
lowed during the S/S test are outlined in the Sampling and Analysis Plan (SAP) for the
S/S process, which is included as Appendix I, and the SAP for the additional treatment
studies, included as Appendix II. Any deviations from the SAP are noted in the OER.
Operating data collected during the tests and the analytical results of the bench-scale
tests are presented herein to assist the CS&D group in evaluating the S/S technology.
The OER was prepared in accordance with guidelines established by the Office
of Solid Waste (OSW) in their "Quality Assurance Project Plan for Characterization
Sampling and Treatment Tests Conducted for the Contaminated Soil and Debris
(CS&D) Program" (Appendix III). Section 1 presents an overview of the CS&D pro-
gram and describes the objectives of the study. Section 2 describes the contaminated
soil, and Section 3 describes the treatment technology under evaluation. Section 4
addresses the sampling and analysis activities, and Section 5 addresses the collection
of design and operating data. Section 6 presents data on all analyses performed on
1-3
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the treatment test samples. Section 7 discusses the quality assurance/quality control
I
measures associated with the analytical data. Any correspondence critical to the per-
formance or evaluation of the treatment test is presented in Section 8.
i
The bench-scale S/S tests were conducted at the CHF in two phases: Phase I
was initiated on February 20, 1991, and Phase II was initiated on June 6, 1991.
i
Samples collected from the tests were sent to the IT Analytical Services (ITAS)
i
Laboratory in Cincinnati. The names of key personnel involved in the activities
throughout this study are presented in Table 1-1.
TABLE 1-1. KEY PERSONNEL INVOLVED IN THE
SOLIDIFICATION/STABILIZATION PILOT-SCALE TEST
Treatment Test Facility:
Test Facility Coordinator:
Dates of Treatment Test:
EPA Personnel:
Contract Personnel:
OER Preparation:
Laboratory Manager:
U.S. EPA|Center Hill Solid and Hazardous
Waste Research Facility
5995 Center Hill Road
Cincinnati, OH 45224
Jerry Iseriburg
University^ of Cincinnati
.5995 Center Hill Road „
Cincinnati, OH 45224
(513) 569*7885
February 20 through April 10, 1991 (Phase I)
June 6 through July 5, 1991 (Phase II)
Richard P. Lauch, Technical Project Monitor
Judy L Hessling, ITEP, CS&D Project Manager
John Miller, ITEP, Project Engineer
Michael Smith, ITEP, Sampling and Analysis
Coordinator
Michael Li Smith, ITEP
John Miller, ITEP
Jerry Isenberg, UC
i
Richard Gurley
IT Analytical Services
11499 Chester Road
Cincinnati, OH 45246
1-4
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SECTION 2
CONTAMINATED SOIL UNDER EVALUATION
Brown's Battery Breaking is an abandoned lead-acid battery processing/
recycling facility in Tilden Township, Pennsylvania, approximately 20 miles northwest of
Reading. The 10-acre site lies south of Fisher Dam Road on the peninsula formed by
the S>chuylkill River and Mill Creek. The initial process at the site involved placing
batteries on a conveyor belt, which carried them to a hydraulic guillotine that sliced the
top off each battery. The batteries were then turned upside down, and:the acid and
battery grids (i.e., perforated or ridged lead plates used as conductors in batteries)
were dumped on the ground. The grids were subsequently transported for sale, and
the casings were dumped into pits along Mill Creek. Eventually, the entire site was
covered with casings. Later processes involved washing the casings with water to
remove the lead oxides. Typical operations included the processing of more than
5000 batteries per day. The casings were used locally as a lightweight aggregate and
fill.
During the remedial investigation (Rl) for the site, samples of soil, ground water,
surface water, and sediments were collected and analyzed, primarily for total lead.
Low concentrations of other metals and Target Compound List (TCL) organic con-
taminants were also detected, but they were determined to be of minor significance
and not to pose significant environmental hazards. Low concentrations: of PCBs were
detected in two samples in the parts-per-billion range. Field x-ray fluorescence spec-
trophotometry (XRF) and inductively coupled argon plasma spectrometry (ICAP) were
used to determine lead concentrations in the site soils and laboratory soil samples,
respectively. |
2-1
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Soil samples taken by the Pennsylvania Department of Environmental
Resources (PADER) in 1980 showed high concentrations of lead on a nearby dairy
farm. Subsequent blood tests of children living on the Brown's Battery site showed
elevated lead levels. Sampling of the Brown's Battery Breaking Site in 1983 revealed
lead levels ranging from 3,130 to 84,200 ppm around the residences and levels of
20,100 ppm and 378,000 ppm at depths of 2.5 ft and 1.5 ft, respectively. From Oc-
tober 1983 through July 1984, 72,000 yd3 of contaminated solids (soil and battery
casings) were encapsulated on site. The contaminated soils arid battery casings were
graded into a mound covering an area 100 ft by 230 ft and measuring 6 to 7 ft high.
S'ix thousand cubic yards of clay and a 6-inch veneer of topsoil were used to cover
this soil/debris pile. Despite this action, lead contamination on the site remained
widespread, and concentrations range fromiless than 100 to 24,000 mg/kg.
i
In October 1990, ITEP sent a sampling team to characterize the soil that was
not encapsulated in 1983-1984. Field XRF was used to select samples, and six loca-
tions in the wooded areas in the southwest borner of the site were flagged as having
lead concentrations in the range of 10,000 to 30,000 ppm. The methodology followed
for XRF analysis of the soil is presented in Appendix IV. The lead concentrations
detected by XRF in the six flagged areas are presented in Table 2-1. Two flagged
locations (5 and 6 in Table 2-1) were deleted from consideration because the field XRF
determined a wide range of variation in the lead concentrations in one of the areas,
and low concentrations of lead in the other area. Shovels, rakes, a 3/8-inch sieve, and
stainless steel spoons were used to collect samples of surface soil only. Sampling
locations and depths were based on data and observations from previous site
activities as well as the sampling personnel's best engineering and field judgment.
The four sampling locations are shown in Figure 2-1. The collected soil samples were
placed in 5-gallon plastic containers. Field XRF was also used to scan the soil after it
had been sieved and collected in the four 5-gallon plastic containers. Table 2-2
presents the total lead concentrations found; in the containerized samples based on
the XRF analysis. The soil under investigation is a dark brown, sandy, silty clay with a
2-2
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high organic content (17% TOC). Figure 2-2 shows the grain-size distribution graphi-
cally. Table 2-3 presents the sieve and hydrometer analysis for the Brown's Battery
soil.
TABLE 2-1. XRF TOTAL LEAD CONCENTRATIONS
IN THE SIX FLAGGED AREAS
i
Flag No. Concentration, ppm
1 : 30,000
2 13,000 to 16,000
3 ; 17,000
4 ; 25,000
5 3,000 to 19,000
6 12,000
TABLE 2-2. XRF TOTAL LEAD CONCENTRATIONS IN THE
CONTAINERIZED SAMPLES
Container No.
1
2
3
4
Flag No.
1 and 4
1 and 4
2
3
Concentration
23,120 to 25
19,940 to 22
10,580 to 11
9,230 to 9,
, ppm
,010
,520
,880
500
The soil sample had a moisture content of 27.4 percent, and a specific gravity
of 2.26. A falling-head permeameter was used to determine the permeability of the
raw soil; the average permeability was 1.57 x 10"6 cm/s at 95 percent of the standard
Procter compaction density. Raw data sheets for the physical tests conducted on the
I
soil are included in Appendix V. !
Table 2-4 presents analytical results for the initial Brown's Battery characteriza-
tion. Table 2-5 lists key personnel present at the site during the excavation and collec-
tion of the soil samples.
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2-5
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TABLE 2-3. SIEVE AND
HYDROMETER ANALYSIS
Sieve size or
diameter, mm
Percent passing
10
20
40
60
100
200
0.02973
0.02083
0.01261
0.00903
0.00646
0.00326
0.00137
99.2
98.6
97.0
89.5
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34.8
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22.8
18.9
12.4
9.6
-6
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TABLE 2-4. SUMMARY OF ANALYTICAL RESULTS (DETECTED CONSTITUENTS)
FOR THE CHARACTERIZATION SAMPLES COLLECTED AT BROWN'S BATTERY
BREAKING SITE, TILDEN TOWNSHIP, PA !
Analytical constituents
Total Basis
Aroclor 1254, /xg/kg
pH, SU
Moisture, %
TOC, jug/g
Oil and grease, %
Dioxins/Furans, ng/g
1,2,3,4,6,7,8-HpCDD
Total HpCDD
OCDD
Metals (total), mg/kg
Aluminum
Antimony
Arsenic
Barium
Beryl 1 i urn
Cadmium
Calcium
Chromium
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Mercury
No. la
1100
4.79
29.0
143,000
0.13
No. 1
2.2
3.7
15,0
5210
43.2
12.0
65.9
0.938
2.02
506
7.56
13.3
35.8
17,000
25,800
662
713
0.289
Concentration
Samples
No. 2
NDb
4.36
25.7
j
!
:
No. 3
530
4.70
27.5
325,000 200,000
0.045
Samel es
No. 2
NAC
NA
NA
4980
34.8
11.8
65.4
0.854
1.91
576
7.27
14.0
34.0
-
No. 3
ND i
ND ;
ND ;
2770
ND
5.35
37.8
0.486
1.47
776
4.21
8.0
23.0
16,300 11,800
23,100
639
719
0.299
5460
397
388
0.71;4
0.036
No. 4
ND
ND
1.9
4810
8.06
6.55
62.9
0.828
1.92
946
6.52
11.1
30.1
15,500
6950
672
539
0.222
(continued)
2-7
-------
TABLE 2-4 (continued)
Analytical constituents
Concentration
Samples
•
Metals (total) (cont.)
Nickel
Potassium
Selenium
Silver
Sodium
Vanadium
Zinc
Metals (EP-Toxic), mg/L
Barium
Cadmium
Chromium VI
Lead
Mercury
Nickel
Selenium
Zinc
Metals (TCLP), mg/L
Barium
Cadmi urn
Copper
Lead
Mercury
Nickel
Silver
Zinc
a Composite of Containers
ND « Not detected above
0 NA « Not analyzed.
No • 1
i
11.2
251
4.3
0.464
68.9
8.82
95.8
0.300
0.003
ND '
1.90 '
ND j
0.026
ND
0.377
0.19 i
0.008
0.012
130
No. 2
11.5
256
1.0
0.443
69.5
8.42
87.2
0.324
0.002
ND
1.95
ND
ND
0.005
0.382
0.211
0.009
0.012
123
0.0002 0.0001
0.049 0.036
ND '
0.654
1 and 2.
the reported detection
.
0.1
0.721
limit.
No. 3
6.89
286
1.2
ND
65.6
4.65
50.3
0.402
ND
0.008
1.28
0.0001
ND
ND
0.511
0.255
0,004
ND
24.8
0.0002
0.029
0.011
0.552
No. 4
10.5
305
0.65
ND
64.1
8.12
70.9
0.371
ND
0.007
0.532
ND
ND
ND
0.281
0.341
0.005
0.018
44.4
0.0001
0.032
ND
0.486"
2T8
-------
TABLE 2-5. KEY PERSONNEL INVOLVED IN THE EXCAVATION! OF
TREATMENT SOIL
Excavation Site Facility:
Excavation Location:
Site Remediation Coordinator:
Date of Excavation:
Contact Personnel:
Brown's Battery Breaking ;
Superfund Site
Tilden Township, Pennsylvania
Southwest Corner of Brown's ;
Battery Breaking Site (as shown
in Figure 2-1)
Chris Corbett
Remedial Project Manager :
U.S. Environmental Protection Agency
Remedial Enforcement Response Branch
841 Chestnut Street
Philadelphia, Pennsylvania 19107
(215) 597-6906
October 31, 1990
Dick Lauch, EPA/RREL, Observer
Chris Corbett, EPA/Region 3, Observer
George Prince, EPA/Edison, Observer
Doug Janick, Weston/REAC, Field XRF
Mark Berncik, Weston/REAC, Field XRF
John Miller, ITEP, Sampling Team Leader
Dave El stun, ITEP, Sampling Team Member
2-9
-------
-------
SECTION 3
TREATMENT SYSTEM UNDER EVALUATION
3.1 Description of Treatment System
The bench-scale S/S treatment system evaluated under this project was con-
ducted at the U.S. EPA's Center Hill Solid and Hazardous Waste Research Facility
(CHF).
In this study, attempts were made to determine the ability of selected binder
materials (e.g., portland cement, kiln dust/fly ash, and quicklime/fly asr)) used in
connection with S/S to reduce the leaching of lead in soils. Soil samples collected
from the Brown's Battery Breaking site were used as test materials. Rgure 3-1
presents a process diagram showing all treatment operations and the points at which
operating data and samples were collected.
3.1.1 Mixing/Homogenization of the Raw Soil •
The four buckets of raw soil were emptied into a 55-gallon steel drum lined with
a standard polyethylene drum liner. A lid liner was placed on top, and the lid was then
secured with a screw drum clamp ring. The drum was placed horizontally on a drum
roller (Morse Manufacturing Model 201/5-1) and rolled at 30 rpm for 12 hours.
After blending was completed, the sample appeared to be a mass of smooth
spheres 2- to 3-cm in diameter. When the drum was emptied in a pile on the floor for
homogenization, the contents consisted entirely of such lumps except for one lump
about 15-cm in diameter. This one larger lump was broken by hand into 2-cm pieces
and sprinkled onto the pile of spheres. |
3-1
-------
CO
LU
U.X
is!
O
co
§
CO
o
PROPORTIONING a
MIXING
soil/binder mix
co :=
«s
CD
I 52
!«••§
09
D.
«
^
coS. |
S2 l
IO...O
c
2'ocO-l^>vO>j-3if = -SSw
I 1
'1
E3 \
ETERS
each mi
TEST PARAM
Total Pb (FAD) for
pH of each mix
co
|
O)
O
^it
§£l
LU^
£
W
o>
*S
2°S
'
- -
lti
OD
< s'
a« «8
a JrS* to 03 CL a*
u. a, |
3-2
8-803811.28-1-091.1
-------
So that representative subsamples could be obtained, the Quartering Method
(Method B) of ASTM Method C702-87 was used to divide the pile of spheres. No
subsample contained less than 20 of the 2- to 3-cm spheres, and most samples
contained more than 40 such spheres. Figure 3-2 presents a breakdown of the sub-
samples collected and their disposition. ;
3.1.2 Preparation of the Stabilization Mixes ]
The soil/binder mixes were prepared in a planetary rotary mixer in accordance
with the protocols in ASTM Method C305. The order of addition was:
1. Raw soil was sieved to less than 3/8-in. mesh size to crush the 2- to
3-cm spheres formed by the soil mixing/homogenization step and to
make the soil more amenable to the treatment process.
2. Soil and binder were dry-blended. i
3. Water was added until the mixture passed the flow table test (ASTM
Methods C230 and C109 - Section 103).
For each binder/soil mix, six 2-in. by 4-in. (long) cylinders and one 4-in. by 1-in.
(long) cylinder (used to determine set time) were prepared (i.e., the binder/soil/ water
mixture was poured into molds). All molded samples were covered with a thin plastic
sheet and placed in a concrete test cure box for a 28-day curing period. The cure
box was maintained at 75 °F and water was kept standing in the bottom of the box to
maintain moist storage.
During the curing of the cast samples, the set was checked by using a Vicat
needle to test for setting qualities (ASTM C191-82). In addition, after 28 days, an
unconfined compressive strength (UCS) test (ASTM Method G109-90) was conducted
on all remaining molds. Vicat and UCS data are presented in Section 5.
3.2 Experimental Design
The three binder systems used during the bench-scale S/S testing (Phase I)
were:
i
1. 100% Type I portland cement
3-3 ! '
-------
52kg
(raw soil)
6 FAD samples
taken (grab)
's////Ar//&y///S/r/^^^
\ f
J
9.5 kg tor
Permeability
Study
Reserve
Sieve GANG
Hydrometer
* Soil held in reserve and eventually used in mixes 7-10.
•* Soil used in mixes 1-6.
Figure 3:2. Homogenization and subsampling procedure for the raw soil.
3-4
S-M0611-28-1 -Ml -2
-------
2. 67 percent cement kiln dust and 33 percent fly ash !
3. 60 percent fly ash and 40 percent quicklime.
For the design of the recipes for the test mixes (i.e., the ratio of binder to soil),
the acid and alkaline response of the binders and the waste (soil) had to be
determined. ;
The Generalized Acid Neutralization Capacity (GANG [CHFE-09-90]) test has
been developed by CHF to standardize data collection and interpretation in S/S
testing. Because the GANG data had already been developed by CHF for the binders
to be evaluated in this study, only the raw waste required a GANG test; These tests
!
generate graphs that indicate pH versus equivalents of acid/alkali. These graphs are
then used to predict the acid and alkaline response that will occur with various ratios
of waste-to-binder. These data can then be used to select binder/waste ratios that fall
in the pH range that has been shown to immobilize lead (pH 8.5 to 10.0 for the
cement kiln dust and fly ash, pH 8.5 to 10 for the quicklime and fly ash, and pH 8.0 to
11.0 for the portland cement) at the,number of acid equivalents used in the TCLP (i.e.,
2 eq/kg), The pH ranges for immobilizing lead are based on MANC (Metal Acid
Neutralizing Capacity) analyses. These are analyses of metals that leabh into solutions
produced during the GANG tests. The analyses of the solutions for lead content
allowed for determination 'of the ranges in pH which reduced the leaching of lead to
less than 5 mg/L The GANG curves for Type I portland cement, dolomitic quicklime,
fly ash, and cement kiln dust are presented in Section 5. The GANG, as well as the
CHF procedure for calculating S/S binder recipes for trial mixes on thej basis of GANG
results, are presented in Appendix VI. ;
3-5
-------
-------
SECTION 4
SAMPLING AND ANALYSIS ACTIVITIES
Sampling of the Brown's Battery soil during the S/S treatment test was con-
ducted in accordance with the Sampling and Analysis Plan (SAP) for Treatment Tes-
ting of Solidification/Stabilization of Contaminated Soils (Appendix I), with one
modification. As a result of the failure of the six original binder mixtures: to stabilize the
lead present in the soil, additional studies were conducted on three new binder mix-
!
tures (one each for portland cement, the mixture of cement kiln dust and fly ash, and
the mixture of quicklime and fly ash). In addition, another portion of the soil was
heated to reduce the organic content of the soil and then treated with a portland
cement binder-to-soil ratio of 20 percent. The modification to the SAP covering these
additional studies is included in Appendix 11. j
The following three types of samples were.collected during the treatment test:
Sampling Point Description
1 Raw homogenized soil
2 Binder/soil pretreatment sample
3 Binder/soil monoliths
Sampling and analysis activities performed during the pilot-scale tests are pre-
sented in Subsections 4.1 and 4.2, respectively, and deviations from the Sampling and
Analysis Plan are presented in Subsection 4.3. Subsection 4.4 contains;information
about safety considerations observed during the sampling activities.
4-1
-------
4.1 Sampling Methods
Six replicate samples were collected from each portion of test soil both prior to
and after treatment to evaluate the performance of the different binder mixes in stabi-
lizing the lead content of the soil. One exqeption to this was the portion of soil heated
before treatment from which three replicate samples were collected to determine the
effect the organic carbon content of the soil had on the performance of the binders in
stabilizing the lead content of the soil. In addition, samples were collected of the raw
homogenized soil to characterize the soil being investigated. The following
subsections explain the purpose of collecting each sample, the sampling location, the
method and frequency of sampling, and thb constituents to be analyzed. Additionally,
details regarding sample containers and sample preservation techniques are pre-
sented.
4.1.1 Sampling Point 1-Raw Homogenized Soil
Pwrpose-The raw homogenized soil was sampled to characterize the soil under
investigation. As part of the CS&D prograrri, one sample of soil was analyzed for the
complete CS&D constituent list to verify no further type of contamination was present
in the soil. \
Description of Sampling Point-Samples of the raw homogenized soil were
collected after the soil was quartered, as illustrated in Figure 3-2.
Sample Collection Method-After being subjected to the mixing and quartering
process, the soil was in the form of spheres approximately 2- to 3-cm in diameter.
The soil was crushed, sieved, and mixed by hand to achieve a homogeneous sample
amenable to analysis. Grab samples of soil were collected from the homogenized
mixture and placed in the appropriate sample containers for the analyses to be
performed.
Frequency of Sampling-One grab sample was collected from the raw homog-
enized soil, and portions of the sample were placed into the appropriate containers for
the analyses to be performed. !.
4-2
-------
Constituents Analyzed-Jne sample collected was analyzed for the CS&D con-
stituents listed in Table 4-1. j •
4.1.2 Sampling Point 2 - Binder/Soil Pretreatment Sample
Purpose-Jhe soil was sampled prior to treatment to determine contamination
levels; of lead leaching from the soil. :
Description of Sampling Po//tf--During quartering of the test soil, aliquots of the
soil v/ere set aside for treatment tests. Samples were collected from the aliquots of
soil prior to the addition of the binder mixes. :
Sample Collection Method-Each portion of soil was mixed by hand to crush the
spheres and to homogenize the soil. Grab samples were then obtained from each
aliquot of soil. \
Frequency of Sampling-Six replicate grab samples were collected from each
portion of soil prior to the addition of the binder mix, except for the soil that had been
heated before treatment. Because of the small volume of soil available, ionly three
replicate grab samples were collected from the soil heated before treatment.
Constituents analyzed-The samples collected from the pretreatment soil were
analyzed for the critical constituent TCLP lead.
4.1.3 Sampling Point 3-Binder/Soil Monoliths
Purpose-Tne monoliths were sampled to determine the effectiveness of the
binder mixes in stabilizing the lead content of the soil.
Description of Sampling Point-Binder/soil mixes were allowed to
cure for 28
days. Upon completion of curing, the monoliths were crushed and sampled.
Sample Collection Method-Tr\e cured monoliths were crushed prior to sam-
pling. Grab samples were then collected from each binder/soil mixture.
Frequency of Sampling-Six replicate samples were collected from the monoliths
for eaich binder mixture,-except for the soil that had been heated before treatment.
Because of the small volume of soil available, only three replicate samples were
collected from the monoliths for the soil heated before treatment. !
4-3
-------
TABLE 4-1. CS&D LIST BY CONSTITUENT TYPE
Constituent
Volatile organ ics
Acetone '•
Acetonitrile
Acrolein
Acryl amide
Acrylonitrile
Benzene
Bromodi chl oromethane
Bromomethane !
Carbon tetrachloride ;
Carbon disulfide
Chlorobenzene
2-Chloro-l,3-butadiene
Chlorodibromomethane ;
Chloroethane
2-Chloroethyl vinyl ether ;
Chloroform
Chl oromethane <
3-Chloropropene
l,2-Dibromo-3-chloropropane ,
1,2-Dibromoethane
Di bromomethane
cis-l,4-Dichloro-2-butene
trans-1 , 4-Di chl oro-2-butene
Di chl orodi f 1 uoromethane
1,1 -Di chloroethane
1,2-Dichloroethane
1 , 1 -Di chl oroethyl ene
(continued) 4-4
CAS No.a
67-64-1
75-05-8
107-02-8
79-06-1
107-13-1
71-43-2
75-27-4
74-83-9
56-23-5
75-15-0
108-90-7
126-99-8
124-48-1
.75-00-3
110-75-8
67-66-3
74-87-3
107-05-1
96-12-8
106-93-4
74-95-3
1476-11-5
110-57-6
75-71-8
75-34-3
107-06-2
75-35-4
BOAT
Reference
No.
222
1
2
233
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
234
20
21
22
23
24
-------
TABLE 4-1 (continued)
Constituent
Volatile orqanics (continued)
• trans-l-2-Dichloroethene
1 , 2-Di chl oropropane
trans - 1 , 3 -Di chl oropropene
cis-l,3-Dich!oropropene
1,4-Dioxane
Ethyl acetate
Ethyl benzene
Ethyl cyanide
Ethyl ether
Ethyl methacryl ate
Ethyl ene oxide
2-Hexanone
lodomethane
Methyl ethyl ketone
4-Methyl -2-pentanone
Methyl methacryl ate
Mettiacrylonitrile
Methyl ene chloride
Styrene
1 , 1 , 1 , 2-Tetrachl oroethane
1,1,2 , 2-Tetrachl oroethane
Tetrachl oroethene
Toluene
Tribromomethane
1 , 1,, 1 -Tri chl oroethane
1,1., 2-Tri chl oroethane
Tri chl oroethene
CAS No.a
156-60-5
78-87-5
10061-02-6
10061-01-5
123-91-1
141-78-6
100-41-4
107-12-0
60-29-7
97-63-2
75-21-8
591-78-6
74-88-4
78-93-3
108-10-1
80-62-6
126-98-7
75-09-2
100-42-5
630-20-6
79-34-6
127-18-4
108-88-3
75-25-2
71-55-6
79-00-5
79-01-6
BOAT
Reference
No.11
i
i 25
; 26
27
! 28
j 29
1 225
226
!. 30
227
31
i
214
! - •
; 32
; 34
i ' -
, 35
37
! 38
•
i 40
! 41
42
43
i 44
i 45
I 46
i 47
(continued)
4-5
-------
TABLE 4-1 (continued)
Constituent
Volatile organics (continued) ,
Tri chl oromonof 1 uoromethane
1,2,3-Trichloropropane
l,l,2-Trichloro-l,2,2-trifluoroethane
Vinyl acetate
Vinyl chloride
1,2-Xylene
1,3-Xylene
1,4-Xylene
Alcohols
Butanol
2-Ethoxy ethanol
Isobutanol
Methanol
Volatile organics (TCLP)
Benzene
Carbon tetrachloride
Chlorobenzne
Chloroform
1,1-Dichloroethane
1 , 1 -Di chl oroethyl ene
Methyl ethyl ketone
Tetrachl oroethene
Trichlorpethene
Vinyl chloride
Seniivolatile organics
Acenaphthylene • . !
Acenaphthene
(continued) 4-rS
1
f
CAS No.a
75-69-4
96-18-4
76-13-1
108-05-4
75-01-4
97-47-6
108-38-3
106-44-5
71-36-3
110-80-5
78-83-1
67-56-1
71-43-2
56-23-5
108-90-7
67-66-3
75-34-3
75-35-4
78-93-3
127-18-4
79-01-6
75-01-4
208-96-8
83-32-9
BOAT
Reference
No.
48
49
231
-
50
215
216
217
223
224
33
.228
4
7
9
14
22
24
34
42
47
50
51
52
-------
TABLE 4-1 (continued)
Constituent
Semi volatile oraanics (continued)
Acetophenone
2-Acetyl ami nof 1 uorene
4-Aminobi phenyl
Aniline
Anthracene
Aramite
Benzo (a) anthracene
Benzal chloride
Benzo(a)pyrene
Benzo (b)fluoranthene
Benzo (g,h,i)perylene
Benzo ( k) f 1 uoranthene
Benzoic acid
Benzyl alcohol
Bi s (2-chl oroethoxy)methane
Bi s (2-chl oroethyl )ether
Bis (2-chl oroisopropyl) ether
Bi s(2-ethyl hexyl )phthal ate
4-Bromophenyl phenyl ether
Butyl benzyl phthalate
2-sec-Butyl -4,6-dinitrophenol
p-Chloroaniline
Chi orobenzi late
p-Chloro-m-cresol
2-Chl oronaphthal ene
2-Chlorophenol
4-Chlorophenyl phenyl ether
CAS No.a
96-86-2
53-96-3
92-67-1
62-53-3
120-12-7
140-57-8
56-55-3
98-87-3
50-32-8
205-99-2
191-24-2
207-08-9
. 65-85-0
100-51-6
111-91-1
111-44-4
39638-32-9
117-81-7.
101-55-3
85-68-7
88-85-7
106-47-8
510-15-6
59-50-7
91-58-7
95-57-8
7005-72-3
BOAT
Reference
i No.
• 53
54
• 55
56
57
58
! 59
218
62
i 63
1 64
• 65
1
!
1 6? '
'! 68
69
; 70
71
i 72
73
74
75
76
77
78
_
(continued)
4-7
-------
TABLE 4-1 (continued)
Constituent .;
i
Semi volatile organ ics (continued)
Chrysene
Cycl ohexanone '.
Dibenzo(a,h)anthracene
Dibenzofuran
Dibenzo(a,e)pyrene
1 ,3-Di chl orobenzene
• 1,2-Dichlorobenzene
1 , 4-Di chl orobenzene
3,3'-Dich1orobenzidine
2 , 4-Di chl orophenol
2,6-Dichlorophenol i
Di ethyl phthalate
3,3'-Dimethdxybenzidine
p-Dimethylaminoazobenzene
3, 3' -Dimethyl benzidine
2, 4-Dimethyl phenol
Dimethyl phthalate
Di-n-butyl phthalate i
1, 4-Di nitrobenzene
4,6-Dinitro-o-cresol
2,4-Dinitrophenol
2,4-Dinitrotoluene
2,6-Dinitrotoluene
Di-n-octyl phthalate
Di-n-propylnitrosamine
Diphenylamine
Diphenylnitrosamine
CAS No.a
218-01-9
108-94-1
53-70-3
132-64-9
192-65-4
541-73-1
95-50-1
106-46-7
91-94-1
120-83-2
87-65-0
84-66-2
119-90-4
60-11-7
119-93-7
105-67-9
131-11-3
84-74-2
100-25-4
534-52-1
51-28-5
121-14-2
606-20-2
117-84-0
621-64-7
122-39-4
86-30-6
BOAT
Reference
No.
SO
232
- 83
-
84
86
87
88
89
90
91
92
93
94
95
96
97
98.
99
100
101
102
103
.104
105
106
219
(continued) 4-8
-------
TABLE 4-1 (continued)
Constituent
Semi volatile organ ics (continued)
1 , 2-Di phenyl hydrazi ne
Fl uoranthene
Fluorene
Hexachl orobenzene
Hexachl orobutadi ene
Hexachl orocyclopentadiene
Hexachl oroethane
Hexachl oropropene
Indeno(l,2,3-cd)pyrene
Isophorone
Isosafrole
Methapyrilene
3-Methyl chol anthrene
4,4' -Methyl enebi s (2-chl oroani 1 i ne)
Methyl methanesulfonate
2-Methyl naphtha! ene
2-Methyl phenol
4-Methyl phenol
Naphthalene
1,4-Naphthoquinone
1-Naphthylamine
2-Naphthylamine
m-Nitroaniline
o-Nitroaniline
p-Nitroaniline
Nitrobenzene
2-Nitrophenol
CAS No.a
122-66-7
206-44-0
86-73-7
118-74-1
87-68-3
77-47-4
67-72-1
1888-71-7
193-39-5
78-59-1
120-58-1
. 91-80-5
56-49-5
101-14-4
66-27-3
91-57-6
95-48-7
106-44-5
91-20-3
130-15-4
134-32-7
91-59-8
99-09-2
88-74-4
100-01-6
98-95-3
88-75-5
: BOAT
Reference
No.
!
107
108
109
! no
in
1 112
113
115
1 116
;
• 117
1 118
: 119
120
36
i
: 81
!' 82
i 121
; 122
123
124
I
':
125
I 126
i _ =
(continued)
4-9
-------
TABLE 4-1 (continued)
Constituent
Semi volatile orqanics (continued)
4-Nitrophenol
N-Nitrosodi-n-butylamine
N-Nitrosodiethylamine
N-Nitrosodimethylamine
N-Nitrosomethyl ethyl ami ne
N-Nitrosomorphol ine
N-Nitrosopi peri dine
N-Nitrosopyrrol idine
5-Nitro-o-toluidine
Pentachl orobenzene
Pentachl oroethane
Pentachl oroni trobenzene
Pentachl orophenol
Phenacetin
Phenanthrene
Phenol
Phthalic anhydride
Pronamide
Pyrene
Pyridine
Resorcinol \
Saf rol e
1,2, 4, 5-Tetrachl orobenzene
2,3,4,6-Tetrachlorophenol
1 , 2 , 4-Tri chl orobenzene
2, 4, 5-Trichl orophenol
2 , 4 , 6-Tri chl orophenol
CAS No.a
100-02-7
924-16-3
55-18-5
62-75-9
10595-95-6
59-89-2
100-75-4
930-55-2
99-65-8
608-93-5
76-01-7
82-68-8
. 87-86-5
62-44-2
85-01-8
108-95-2
85-44-9
23950-58-5
129-00-0
110-86-1
108-46-3
94-59-7
95-94-3
58-90-2
120-82-1
95-95-4
88-06-2
BOAT
Reference
No.
127
128
129
130
131
132
133
134
135
136
137
138
139
140
141
142
220
!144
145
39
146
147
148
149
150
151
152
(continued)
4-10
-------
TABLE 4-1 (continued)
Constituent
Semi volatile oraanics (TCLP)
1 , 4 -Di chl orobenzene
2,4-Dinitrotoluene
Hexachl orobenzene
Hexachl orobutadi ene
Hexachl oroethane
2-Methyl phenol
4-Methyl phenol
Nitrobenzene
Pentachlorophenol
Pyriidine
2,4,, 5-Tri chl orophenol
2 , 4 j, 6-Tri chl orophenol
Metals (total)
Aluminum
Antimony
Arsenic
Barium
Beryl 1 i urn
Cadmium
Chromium (total)
Cobal t
Copper
Iron
Lead
Magnesium
Manganese
Mercury
CAS No.a
106-46-7
121-14-2
118-74-1
87-68-3
67-72-1
95-48-7
106-44-5
98-95-3
87-86-5
110-86-1
95-95-4
88-06-2
7429-90-5
7440-36-0
7440-38-2
7440-39-3
7440-41-7
7440-43-9
7440-47-3
7440-48-4
7440-50-8
7439-89-6
7439-92-1
7439-95-4
7439-96-5
7439-97-6
BOAT
efere^pce
No.
88
102
110
111
113
81
82
126
139
39
151
152
-
154
155
156
157
158
159
-
160
-
161
-
-
162
(continued)
4-11
-------
TABLE 4-1 (continued)
Constituent
Metals (total) (continued)
Nickel '
Potassium
Silver ;
Sodium
Thallium
Vanadium ;
Zinc
Metals fTCLP) ;
i
Arsenic
Barium
Cadmi urn \
Chromium (total) i
Chromium (hexavalent) '.
Lead
Mercury
Selenium ;
t
Silver i
Inorqanics other than metals
Cyanide ;
Fluoride
Sulfide I
Orqanochlorine Pesticides
Aldrin
Alpha-BHC
Beta-BHC
Delta-BHC
Gamma- BHC
CAS No.a
7440-02-0
7440-09-7
7440-22-4
7440-23-5
7440-28-0
7440-62-2
7440-66-6
7440-38-2
7440-39-3
7440-43-9
7440-47-3
-
7439-92-1
7439-97-6
7782-49-2
7440-22-4
57-12-5
16964-48-8
8496-25-8
309-00-2
319-84-6
319-85-7
319-86-8
58-89-9
BOAT
Reference
No.
163
-
165
-
166
167
168
155
156
158
159
221
161
162
164
165
169
170
171
172
173 .
174
175
176
(continued) 4-12
-------
TABLE 4-1 (continued)
Constituent
Orqanochlorine Pesticides (continued)
ChTordane
p,p'-DDD
p,p'-DDE
p,p'-DDT
Dieldrin
Endosulfan I
Endosulfan II
Endosulfan sulfate
Endrin
Endrin aldehyde
Endrin ketone
Heptachlor
Heptachlor epoxide
Isodrin
Kepone
Metihoxychlor
Toxaphene
Phenoxvacetic acid herbicides
2,4-Dichlorophenoxyacetic acid (2,4,-D)
Silvex (2,4,5-TP)
2,4,5-Trichlorphenoxyacetic acid (2,4,5-T)
Oraanophosphorus insecticides
Di siul f oton
Famphur
Methyl parathion
Parathion
Phorate
»
CAS No.a
57-74-9
72-54-8
72-55-9
50-29-3
60-57-1
939-98-8
33213-6-5
1031-07-8
72-20-8
7421-93-4
53494-70-5
76-44-8
1024-57-3
465-73-6
143-50-0
72-43-5
8001-35-2
94-75-7
93-72-1
93-76-5
298-04-4
52-85-7
298-00-0
56-38-2
298-02-2
BOAT
Reference
No.
177
178
179
180
181
182
183
238
184
185
-
186
187
188
189
190
191
192
193
194
195
196
197
198
199
(continued)
4-13
-------
TABLE 4-1 (continued)
Constituent • I ,,.,. .. a
CAS No.
Orqanophosphorus Insecticides (continu
Sul f otep
ed)
3689-24-5
Thiorazin 297-97-2
0,0, 0-Tri ethyl phosphorothi oate
Pesticides, herbicides (TCLP)
Aldrin
Alpha-BHC
Beta-BHC
Delta-BHC
Gamma -BHC
Chlordane
p,p'-DDD
p,p'-DDE
p,p'-DDT
Dieldrin
Endosulfan I
Endosulfan II
309-00-2
319-84-6
319-85-7
319-86-8
58-89-9
57-74-9
72-54-8
72-55-9
50-29-3
60-57-1
939-98-8
33213-6-5
Endrin 72-20-8
Endrin aldehyde 7421-93-4
Heptachlor 76-44-8
Heptachlor epoxide ; 1024-57-3
Isodrin . 465-73-6
Kepone • 143-50-0
Methoxychlor 72-43-5
Toxaphene 8001-35-2
2,4-D 94-75-7
BOAT
Reference
No.
-
172
173
174
175
176
177
178
179
180
181
182
183
184
185
186
187
188
189
190
191
192
(continued)
4-14
-------
TABLE 4-1 (continued)
BOAT
CAS NO.*
Pesticides, herbicides (TCLP)
2,4-TP _ . _ _ _ 93-72-1 : 193
a Reference numbers taken from Table 3-2 from "Quality Assurance Project
Plan for Characterization Sampling and Treatment Tests Conducted for
the Contaminated Soil and Debris (CS&D) Program" prepared by 'the U.S.
EPA Office of Solid Waste.
4-15
-------
Constituents Analyzed-Jhe samples bollected from the monoliths were analyzed
for the critical constituent TCLP lead.
4.1.4 Sample Containers and Sample Preservation
Raw homogenized soil samples from the S/S treatment test were collected as
grab samples in 8-oz precleaned glass jarsJ Pretreatment soil and posttreatment
monolith samples were collected as grab samples and extracted by the TCLP method
at the Center Hill Facility. The resulting leachate samples were preserved with nitric
acid to pH <2 prior to their shipment to the ITAS-Cincinnati laboratory.
Besides the aforementioned samples, trip blanks were prepared and analyzed
for volatile organics, and TCLP extraction blanks were prepared and analyzed for lead.
The extraction blanks were preserved with nitric acid to pH <2.
All samples were packed in coolers with ice before being shipped to the labora-
tory for analysis. Proper shipping papers, chain-of-custody forms, and request-for-
analysis forms also accompanied the samples. Table 4-2 presents a summary of the
analytical parameters and their proper sample containers, preservation methods, and
holding times.
4.2 Analytical Procedures
Table 4-3 lists the analytical parameters and the appropriate preparation and
analytical methods. A brief description of the analytical methods used to analyze for
the critical parameter TCLP lead and FAD lead in the soil matrix are presented in
Subsections 4.2.1 and 4.2.2, respectively. ;
4.2.1 TCLP Lead Analysis
The contaminant of most critical concern for this study was lead. In particular,
the leachability of lead in the soil was the primary concern because of the interest In
trying to stabilize the lead in the soil. Pretreatment soil samples and posttreatment
monolith samples were extracted in accordance with the Toxicity Characteristic
Leaching Procedure (TCLP) detailed in Method 1311 in SW-846 (Appendix VII in this
report). University of Cincinnati personnel performed the TCLP extraction at the
4-16
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4-18
-------
TABLE 4-3. PREPARATION AND ANALYTICAL METHODS
Parameter class
Preparation method
Analytic|1
method
Raw homogenized soil
Volatile organics
TCLP volatile organics
Alcohols
Semi volatile organics
TCLP semi volatile organics
Organochlorine pesticides
TCLP organochlorine pesticides
Phenoxyacetic acid herbicides
TCLP phenoxyacetic acid herbicides
Organophosphorus pesticides
Hetals (total)
Alumi num
Antimony
Arsenic
Barium
Beryl1i urn
Cadmi urn
Chromium (total)
Cobalt
Copper
Iron
Lead
Magnesium
Manganese
Mercury !
Nickel
Potassium
Sodi urn
Thallium
Vanadi urn
Zinc
Metals (TCLP)
Arsenic
NA
1311°
NA
3550
1311/3520
3550
1311/3520
3550
1311/3520
3550
3050
3050
3050
3050
3050
3050
3050
3050
3050
3050
3050
3050
3050
7471
3050
3050
3050
3050
3050
3050
1311
3010
8240
8240
J3015
8270
8270
8080
8080
8150
8150
8140
6010
6010
7060
6010
6010
6010
6010
6010
6010
6010
6010.
6010
6010
7471
6010
6010
6010
6010
6010
6010
7060
(continued)
4-19
-------
TABLE 4-3 (continued)
Parameter class
Barium
Cadmium
Chromium (total)
• Chromium (hexavalent)
Lead
Mercury
Selenium
Silver
FAD lead
Other parameters '
Moisture content
Oil and grease
Total organic carbon
Total organic halides
pH
Chloride
Cyanide
Fluoride
Sul.fate
Sulfide
6ANC
Binder/soil pretreatment soil and monolith
samples >
TCLP lead .
FAD lead
6ANC :
Flow table test
Vicat needle test ' [
Unconfined compressive strength
Cone penetrometer
a
Preparation method
3010
3010
3010
7196
3010
7470
7740
3010
Appendix IX
NA
NA
NA
NA
NA
Water extraction
NA
13 B
NA
Water extraction
Appendix VI
1311/3010
Appendix IX
Appendix VI
NA
NA
. NA
NA
Analytical
method
6010
6010
6010
7196
6010
7470
7740
6010
6010
ASTM 3713d
9071
9060
9020
9045
9252
9012
340. 26
9038
9030
Appendix VI
6010
6010
Appendix VI
ASTM C230 + C109
ASTM C191-82
ASTM C190-90
ASTM D3441-79
(continued)
4-20
-------
TABLE 4-3 (continued) ,
3 SW-846 Methods for Evaluating Solid Wastes. ;
Not applicable. ;
c ' ;
Method 1311 TCLP extraction followed by individual preparation methods for each
class of parameters.
d • . '
American Society for Testing and Materials. l
Methods for Chemical Analysis of Water and Wastes. !
4-21
-------
Center Hill Facility. Raw data obtained during the TCLP extraction process is
presented in Appendix VIII.
The resulting extract was preserved ito a pH <2 with nitric acid and cooled to
4"C prior to being shipped to ITAS-Cincinhati. The extract was then digested in
accordance with Method 3010 of SW-846.
A 100-mL aliquot was placed in a beaker with 3-mL of concentrated nitric acid,
and the resulting mixture was heated to evaporate excess solution to 5-mL. After the
beaker was allowed to cool, 3-mL of concentrated nitric acid was added, and the
beaker was again heated so that a gentle reflux occurred. This procedure was
i
continued until no change in the appearance of the sample was observed. At this
point, the beaker was heated to evaporate;excess sample to 3-mL The sample was
then allowed to cool, a small quantity of 1:;1 HCI was added, and the sample was
refluxed for 15 minutes to dissolve any precipitate resulting from the evaporation
procedure. The sample was then filtered to remove particles that may have clogged
i
the nebulizer, and reagent water was addeb to adjust the volume of the sample to
100-mL
An aliquot of the digestate was'then injected into an inductively coupled argon
plasma spectrometer. The sample was nebulized, and the resulting aerosol was
transported to the plasma torch. Element-specific atomic-line emissions are produced
by a radio-frequency, inductively coupled plasma. For lead, the wavelength used is
220 nm. The resulting spectra are dispersed by a grating spectrometer, and the inten-
sities of the lines are monitored by photomultiplier tubes.
4.2.2 Fractionafion and Cold Acid Digestion Method
In addition to the TCLP testing, a Fractionation and Cold Acid Digestion (FAD)
analysis was conducted to determine the total teachable lead content of the treatment
soil. Six grab samples were collected from: the pile of mixed raw soil, prior to quarter-
i
ing, and three grab samples were collected from each of the six original binder mixes.
The FAD testing is based on the use of a more representative sample size of 100
grams rather than the 1 to 5 grams of sample used in the standard method (i.e.
4-22
-------
SW-846, Method 3050). The CHF has used this type of comparison in previous
studies. The FAD used in the mixing steps is CHF's quality control measure for the
mixing process (i.e., the dilution effect of binder and water), and is in essence a criti-
que of the design/mix process. The FAD test is outlined in Appendix IX.
The primary purpose of the FAD test is to check the uniformity of the division of
the samples into mix subsamples with regard to the metal (Le., lead) contaminants.
The FAD data are also used to check the dilution factor of the waste by the binder and
water addition. ;
The FAD extraction procedure was performed at the Center Hill Facility. The
extracts were then analyzed according to Method 6010 by ICP at ITAS-Cincinnati.
4.3 Deviations From the Sampling and Analysis Plan • !
One deviation to the original SAP was implemented during the treatment evalua-
tion study. Because of the inability of the six original binder mixes to stabilize lead in
the soil, additional studies were performed on the soil. Three new binder mixes were
set up for evaluation of their effectiveness in stabilizing lead. In addition, it was
theorized that the heavy organic carbon content of the soil was the reason the six
original mixtures failed to stabilize the lead. Therefore, a portion of the treatment soil
was heated for 24 hours at 310° C to remove the organic carbon from, the soil. The
soil was then treated with portland cement at a binder/soil ratio of 20 percent because
of this binder mixture's ability to stabilize lead in the soil more effectively than the other
five original binder mixtures. This allowed the effect of the organic carbon content of
the soil on the stabilization treatment process to be evaluated.
4,4 Health and Safety
The major concern with lead contamination was exposure through inhalation or
ingestion. The CHF workers wore modified Level D protective equipment. This
included a half-face respirator to protect against inhalation of dust particles, lab coats,
and polyvinyl gloves to protect against unnecessary skin exposure.
4-23
-------
-------
SECTION 5
DESIGN AND OPERATING DATA COLLECTION
Before and during the S/S bench-scale testing, samples were collected and
analyzed to obtain design and operating data to confirm whether the desired process
conditions (e.g., mix design and set) were being met. The parameters monitored
included binder/water addition, total lead determined by Fractionation and Cold Acid
Digestion (FAD), and set. The raw operating data collected during the test (which are
included in Appendix V) are summarized here. !
5.1 Binder/Water Addition
Binder and water addition were monitored to ensure that the nefcessary binder
mix and water were added to the raw soil to achieve the desired stabilization. The
amount of binder to be mixed with the soil was determined by the GANG procedure
(Section 3). |.
5,1.1 Original Mix Design I
The GANG results for the raw waste were combined with the GANG values for
the proposed binders to predict the expected GANG curves for several possible
blends of waste and binder. The GANG curves for the raw soil, Type I portland
cement, dolomitic quicklime, CG&E fly ash, and cement kiln dust are shown in Figures
5-1 to 5-5. The graphs of the mix design possibilities using portland cement, quicklime
with fly ash, and kiln dust with fly ash are shown in Figures 5-6 to 5-8. Optimum pH
ranges to immobilize lead were based on analyses of solutions produced during
GANG tests for lead content. Minimum and maximum values were determined by the
ability of the binder to reduce lead content in leachate to less than 5 mg/L The
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TABLE 6-2. PERKIN-ELMER PLASMA II EMISSION SPECTROMETER
OPERATING CONDITIONS FOR ANALYSIS OF TCLP LEAD
i
Technique: Inductively Coupled Argon Plasma Spectroscopy
Wavelength: 200 nm
Measurement type: Peak height
Carrier gas: Argon i ' •
Nebulizer flow rate: 1 L/min
Auxiliary line flow rate: 1 L/min
Plasma feed flow rate: 15 L/min
Pump rate: 1 mL/min
RF generator: 1006 watts
6-12
-------
duplicate (MS/MSD) samples were spiked with lead to determine accuracy and
precision data. Section 7 presents a detailed description of all QA/QC procedures
performed during the study.
Tables 6-3, 6-4, 6-5, and 6-6 summarize the data collected from the FAD extrac-
tions on the soil used in the original binder mixes. Appendix XI contains the complete
data package for the analysis of lead in the treatment soil matrix. Tables 6-3 and 6-4
list the FAD lead data obtained from the pretreatment samples collected from the raw
soil before binder mixes were added and from the six binder/soil mixtures, respec-
tively. The FAD data were reported from the laboratory in mg/L and had to be con-
verted to the concentration of teachable metal based on dry solids (mg/kg). Tables
6-5 and 6-6 present the converted FAD data for the raw soil before birtder mixes were
added and from the six binder/soil mixtures, respectively. :
As stated previously, FAD extract analyses were performed to check the unifor-
mity of the splitting of the soil samples into mix subsamples. In addition, the FAD data
were used to check the dilution factor of the waste resulting from the addition of the
binder and water. Comparison between the samples in Tables 6-3 and 6-5 indicate
the quartering method was very effective in mixing and dividing the soil into homo-
geneous subsamples. Comparison of data presented in Tables 6-3 and 6-5 with data
presented in Tables 6-4 and 6-6 indicate a dilution of metal concentration with the ad-
dition of the binder and water. Because of the high levels of lead still detected in the
soil matrix after binder addition, the dilution resulting from the binder addition should
i
not adversely affect the study. The actual concentration of lead in the FAD extracts of
the soil and binder mixes compared well with the predicted concentrations for the
mixes using calculated dilution factors. The dilution factors were calculated using the
following calculation: i.
DF = 2. :
wt
6-13
-------
TABLE 6-3. CONCENTRATION OF TOTAL LEAD BY
FAD EXTRACTION IN RAW UNTREATED SOIL
(mg/L)
Contaminant
Lead
BBS-RAW-
FAD- 1
1300
BBS-RAW-
FAD-2
1320
1
BBS-iRAW-
FAD-3
J330
BBS-RAW-
FAD-4
1280
BBS-RAW-
FAD-5
1340
BBS-RAW-
FAD-6
1350
TABLE 6-4. CONCENTRATION OF TOTAL LEAD BY FAD EXTRACTION
IN BINDER/SOIL MIXTURES FROM PHASE I
(mg/L)
Portland cement (100%)
Sample
ID
A
B
C
Average
Binder/soil
16%
1090-
1170
1090
1117
Binder/soil
20%
1180
1100
1080
1120
Kiln dust and
Binder/soil
36%
987
950
974
970
fly ash (2:1)
Binder/soil
42%
943
942
976
954
Fly ash and quicklime (3:2)
Binder/soil
21.25%
1090
1010
1100
1067
Binder/soil
26.25%
1090
1010
1060
1053
Blnder-to-soU ratio calculated on a dry weight basis.
6-14
-------
TABLE 6-5. CONCENTRATION OF TOTAL LEAD IN DIGESTED SOLIDS
BY FAD EXTRACTION IN RAW UNTREATED SOIL ON A DRY WEIGHT BASIS
(mg/kg)
Contaminant
Lead
BBW-RAW BBS-RAW
FAD-1 FAD-2
25,800 26,400
BBS-RAW BBS-RAW
FAD-3 FAD-4
26,600 25,600
BBS -RAW BBS -RAW
FAD-5 FAD-6
26,500 26,900
i
TABLE 6-6. CONCENTRATION OF TOTAL LEAD IN DIGESTED SOLIDS
BY FAD EXTRACTION IN BINDER/SOIL MIXTURES FROM PHASE I ON A DRY WEIGHT BASIS
(mg/kg) ;
Samp] e
ID
A
B
c
Average
Portland cement
(100%)
Binder/ Binder/
soil soil
16% 20%
21,700 23,500
23,400 22,000
21,800 21,600
22,300 22.400
Kiln dust and fly
ash (2:1)
Bi nder/ Bi nder/
soil soil
36% 42%
19,700 18,800
18,900 18,800
19,500 19,500
19,400 19,000
Fly ash and quicklime
. i (3:2)
Binder/ Binder/
soi 1 soi 1
21.25% 26.25%
21,800 21,800
20,200 20,200
22,000 21,200
21,300 21,100
Binder-to-soil ratio calculated on a dry weight basis.
6-15
-------
where
DF = dilution factor |
i
W = mass of raw waste
Wm = mass of binder mix and water
Table 6-7 presents the dilution factors calculated for the six original binder mixes and
the expected lead concentrations in the soil and binder mixes based on the dilution
factor. Expected lead concentrations were calculated from the average FAD con-
centration of 26,300 mg/kg detected in the raw soil due to the inability to obtain an
accurate comparison between individual samples. The actual lead concentrations
!
were also based on the average value determined in each binder mixture. In addition,
since the FAD extracts data are based on dry weight basis, the actual lead con-
centrations had to be corrected for moisture (37.5 percent) to account for the dilution
effect of water in the binder/soil mixture.
Tables 6-8, 6-9, 6-10, and 6-11 summarize the data from the TCLP extractions
for the treatment samples collected from the six initial S/S binder mixes. Appendix XI
contains the complete data package for the analysis of lead in the treatment soil
matrix. Tables 6-8 and 6-9 present pH and TCLP lead data, respectively, obtained
from the pretreatment samples collected from the raw soil before binder mixes were
added. Tables 6-10 and 6-11 present pH and TCLP lead data, respectively, obtained
from the posttreatment samples collected from the binder monoliths that had been
allowed to cure for 28 days.
Comparison of the data presented in Tables 6-9 and 6-11 indicates the binder
mixes used in the study were unsuccessful in stabilizing the lead present in the soil.
TCLP extracts of two of the binder mixes ("16 percent portland cement and 21.25 per-
cent quicklime and fly ash) had higher concentrations of lead in the extracts of treated
soil than those of the raw, soil. In addition, none of the binder mixes were effective in
reducing the TCLP lead content to below the regulatory limit of 5 mg/L established to
categorize soil as being characteristically toxic for lead.
6-16
-------
TABLE 6-7. COMPARISON OF PREDICTED AND ACTUAL LEAD CONCENTRATIONS
BY FAD EXTRACTION IN BINDER/SOIL MIXTURES FROM PHASE I
Hinder mix
16% Portland cement'
20% Portland cement
36% Kiln dust and fly
aish
42% Kiln dust and fly
ash
21.25% Fly ash and
quicklime
26.25% Fly ash and
quicklime
Weight of
dry raw
waste (g)
3000
2000
2000
2000
2000
2000
Weight of
binder and
water (g)
2673.9
1857.3
2300
2401.2
2002.2
2065.6
Dilution
factor
1.9
1.9
2.2
2.2
2.0
2.0
Predicted lead
concentrations
(mg/kg)
13,800
13,800
12,000
12,000
13,200
. 13,, 200
!
Actual lead con-
icentration mois-
ture corrected
(mg/kg)
i 13,900
'' 14,000
I 12,100
11,900
!
' 13,300
13.200
TABLE 6-8. TCLP pH LEVELS IN PRETREATMENT
SOIL SAMPLES FROM PHASE I
Portland cement
(100%)
Sample ID
A
B
C
D
E
F
Average
Standard
deviation
Bi nder/
soi 1 16%
4.82
4.83
4.82
4.81
4.83
4.84
4.82
0.01
Binder/
soil
20%
4.89
4.90
4.91
4.91
4.89
4.92
'4.90
0.01
Kiln dust and
(2:1)
Binder/
soil
36%
4.87
4.86
4.86
4.86
4.87
4.88
4.87
0.01
fly ash
Bi nder/
soil
42%
4.86
4.86
4.85
4.84
4.87
4.88
4.86
0.01
Fly ash
Binder/
soil
21.25%
4.87
4.82
4.82
4.84
4.83
4.84
4.84
0.02
and quicklime
(3:2)
Bi nder/
soil
26.25%
4.86
4.86
4.85
4.86
4.88
4.88
4.86
0.01
Binder-to-soil ratio calculated on a dry weight basis.
6-17
-------
TABLE 6-9. TCLP LEAD CONCENTRATIONS IN PRETREATMENT
SOIL SAMPLES FROM PHASE I
(mg/L)
Portland cement (100%)
Sample
ID
A
B
C
D
E
F
Average
Standard
deviation
Binder/soil*
16%
86
90
85
73
82
84
83
5.7
Binder/soil
20%
84
96
112 '
87
89
89
. 93
10.2
a
Binder-to-soil ratio calculated on a dry
TABLE
Kiln dust and fly ash (2:1)
Binder/soil
36*
9C
88
88
89
95
91
90
1
Z.6
weight basis.
6-10. TCLP pH LEVELS
SAMPLES FROM
(S.U.)
Portland cement (100%)
Sample
ID
A
B
C
0
E
F
Average
Standard
deviation
Binder/soil"
16%
5.24
5.26
5.27
5.27
5.25
5.28
5.26
0.01
Binder/soil
20%
6.23
6.34
6.22
6.37
6.24
6:48
6.31
0.10
Binder/soil
42%
95
96
84
82
82
81
87
6.9
Fly ash and
Binder/soil
21.25%
84
88
86
88
87
86
86
1.6
quicklime (3:2)
Binder/soil
26.25%
87
87
88
88
89
91
88
1.5
IN POSTTREATMENT SOIL
PHASE I
Kiln dust and fly ash (2:1)
Binder/soil
36%
5.45
5.43
5.39
5.47
5.45
5.43
5.44
,0.03|
Binder/soil
42%
5.69
5.74
5.71
5.72
5.76
5.74
5.73
0.03
Fly ash and
Bi nder/soi 1
21.25%
5.25
5.34
5.27
5.28
5.30
5.35
5.30
0.04
quicklime (3:2)
Bi nder/soi 1
26.25%
6.10
6.10 .
6.03
6.29
6.29
5.90
6.12
0.15
a
Binder-to-son ratio calculated on a dry weight basis
6-18
-------
TABLE 6-11.
TCLP LEAD CONCENTRATIONS IN POSTTREATMENT SOIL
SAMPLES FROM PHASE I I
(mg/L) :
Portland cement (100%)
Sample ID Binder/soil
16%
A
B
C
D
E
F
Average
Standard
devi ati on
91
83
83-
85
82
se-
es
3.3
Binder/soil
20%
16
13.
16
12"
16
11
14
2.3
Kiln dust and
Binder/soil
36%
68
62
67
61
61
64
64
3.1
fly ash (2:1)
Bi nder/soi 1
42%
56
56
•53
52
54
55
54
1.7
i
Fly ash and quicklime (3:2)
Binder/soil
21.25% :
120
110 !
140 |
no' ;
120 ;
120 ;
120 1
11 •
Binder/soil
26.25%
49
46
49
32 '
36
63
46
11
Binder-to-soil ratio calcualted on a dry weight basis.
6-19
-------
The target pH for the TCLP leachate of the design mixes was 9.75. The actual
pH values observed for the mixtures, as presented in Table 6-10, indicate something in
the matrix is excessively acidic. An acidic matrix is also indicated by the pH results of
the raw soil presented in Table 6-8. One theory was that cellulose molecules present
in the organic material were undergoing oxidative reactions in the presence of thealkali
present in the binder mixes. The products! of these reactions are acid groups that
neutralized the alkali and, as a result, inhibited the ability of the binder mixes to
stabilize the lead content of the soil. To determine the binder-to-soil ratios necessary
for effective stabilization of lead and to determine the effect the organic carbon content
of the soil had on the binders' ability to stabilize the lead, a new study was initiated.
For determination of whether the soil could be effectively treated by S/S, the
three binders (portland cement, kiln dust plus fly ash, and fly ash plus quicklime) were
used in one new binder-to-soil ratio each. The new binder-to-soil ratios were based
on the results of the GANG data obtained from the first set of binder mixes.
For determination of the effect the organic carbon content of the soil had on the
binders' ability to stabilize the lead, a portion of the untreated soil was heated to
remove the organic carbon from the soil. The process of organic carbon removal was
carried out by placing the sample in a muffle furnace and heating it to 310° C for a 24-
hour residence time. After the 24 hours, the sample was removed from the furnace
and mixed with a stainless steel spoon to check for complete and uniform heating of
the soil. Upon completion of heating, the soil was treated with portland cement at a
binder-to-soil ratio of 20 percent. This mixture was chosen because of its ability to
stabilize lead more effectively than the other five original binder mixes, An indication of
the effect the organic carbon content of tha soil had on the solidification process was
determined by comparing the data on the heated soil with data on soil that had not
i
been heated. It is possible that heating the soil could change the physical properties
of the soil as well as change the form of lead. These changes could have an effect on
the binders' ability to stabilize lead in the soil. However, based on the information
available, the only reasonable explanation for the failure of the six original binder
mixtures was the high organic content of the soil. Therefore, the data collected were
6-20
-------
only used to evaluate the effect the organic carbon content on the soil had on the
binders'ability to stabilize lead. i
Due to the limited amount of soil available for testing, FAD extracts were not
performed on the second phase study samples. Using the raw soil FAD data from
Phase I and using dilution factors based on the addition of the new binder mixes,
predicted lead concentrations can be calculated for each binder mixture. These
values are presented in Table 6-12. i
TABLE 6-12. PREDICTED LEAD CONCENTRATIONS BY
FAD EXTRACTION IN BINDER/SOIL MIXTURES FROM PHASE II
Binder mix
45% portland cement
139.5% kiln dust and
fly ash
77.5% fly ash and
quicklime
a
20% portland cement
Weight of
dry raw
waste (g)
2000
2000
. 2000
1660
Weight of
. binder and
water (g)
2552.4
3516.9
5252.7
1327.3
Dilution
factor
2.3
2.8
3.6
1.8
Average lead
concentration,
from raw soil
(mg/kg)
26,300
26,300
26,300
26,300
Predicted lead
iconcentration
i (mg/kg)
11,400
i 9,390
' 7,310
; 14,600
Soil heated prior to treatment to remove organic carbon.
Thought the predicted values indicate a major dilution effect as a result of the
addition of the new binder mixes, the concentration of lead predicted would still be at
levels which would require treatment. Therefore, the dilution resulting from the binder
addition should not adversely affect the study.
Table 6-13, 6-14, 6-15, and 6-16 present a summary of the data collected from
the TCLP extractions from the four additional S/S binder mixes. Appendix XI contains
the complete data package for the analysis of lead in the treatment sojl matrix. Tables
I
6-13 and 6-14 present pH and TCLP lead data, respectively, obtained for the pretreat-
ment samples collected from the raw soil before the addition of the binder mixes.
Tables 6-15 and 6-16 present pH and TCLP lead data, respectively, obtained for the
posttreatment samples collected from the binder monoliths that had been allowed to
i
cure for 28 days. Comparison of data from Tables 6-14 and 6-16 indicates a dramatic
decrease in teachable lead due to the three modified binder mixes. Table 6-17
6-21
-------
TABLE 6-13. TCLP pH LEVELS IN PRETREATMENT
SOIL SAMPLES FROM PHASE II
(S.U.)
Sample
No.
A
B
C
D
E
F
Average
Standard
deviation
Portl and
cement (100%)
Binder/soil,8
45%
4.87
4.87
4.87
4.85
4.88
4.89
4.87
0.01
Kiln dust and
fly ash i(2:l)
Binder/ioH,
139.5%
4.82
4.84
4.84
4.85
4.85
4.85
4.84
0.01
Fly ash and
quick lime
(3:2)
Binder/soil,
77.5%
4.90
4.89
4.90
4.90
4.91
4.93
4.90
0.01
Portl and
cement (100%)
Binder/soil",
20%
4.96
4.95
4.95
NAC
NA
NA
4.95
0.01
a Binder-to-son ratio calculated on a dry weight basis.
Soil heated prior to treatment to remove organic carbon.
c NA « Not applicable; only three samples collected due to small sample
volume available.
6-22
-------
TABLE 6-14.
TCLP LEAD CONCENTRATIONS IN PRETREATMENT SOIL SAMPLES
FROM PHASE II
(mg/L)
Portland
cement (100%)
Sample Binder/soil,8
No. 45%
A
B
C
D
E
F
Average
Standard
deviation
81
83
85
87
84
85
84
2.0
Kiln dust and
fly ash (2:1)
Binder/soil,
139.5%
85
84
84
83
84
83
84
0.8
Fly ash and
quick lime
(3:2)
Binder/soil,
77.5%
81
85
91
88
88
88
87
3.4
.! Portland
cement (100%)
Binder/soil",
: 20%
110
120
120
NAC
• NA
; NA
1 117
! 5.8
a Binder-to-soil ratio calculated on a dry weight basis. j
Soil heated prior to treatment to remove organic carbon.
c NA = Not applicable; only three samples collected due to small sample
volume available.
6-23
-------
TABLE 6-15. TCLP pH LEVELS IN POSTTREATMENT SOIL SAMPLES
FROM PHASE II
Sample
No.
A
B
C
D
E
F
Average
Standard
deviation
Port! and
cement (100%)
Binder/soil,*
45%
11.09
11.12
11.13
11.14
11.08
•11.08
11.11
0.03
Kiln dust and
fly ash (2:1)
Binder/soil,
139.5%
11.64
11.64
11.58
11.66
11.69
11.67
11.65
0.04
Fly ash and
quicklime (3:2)
Binder/soil,
77.5%
10.47
10.57
10.47
10.57
10.52
10.50
10.52
0.05
Portl and
cement (100%)
Binder/soil,15
20%
8.87
9.05
8.78
NAC
NA
NA
8.90
0.14
Binder-to-soil ratio calculated on a dry weight basis.
Soil heated prior to treatment to remove organic carbon.
c NA « Not applicable; only three samples collected due to small sample
volume available.
6-24
-------
TABLE 6-16. TCLP LEAD CONCENTRATIONS IN POSTTREATMENT SOIL SAMPLES
FROM PHASE II
Sample No.
A
B
C
D
E
F
Average
Standard
deviation
Port! and
cement (100%)
Binder/soil,3
45%
<0.2
<0.2
<0.2
<0.2
<0.2
<0.2
<0,2
0.0
Kiln dust
and fly ash
(2:1)
Binder/soil,
139.5%
1.3
1.5
1.3
1.6
1.6
1.5
1.5
0.1
Fly ash and
quicklime
(3:2)
Binder/soil,
77.5%
0.45
0.58
0.44
0.46
0.53
0.62
0.51
0.08.
Portland cement
: (100%)
Binder/soil, b
, 20%
<0.2
= <0.2
<0.2
i NAC
NA
i NA
;
-------
TABLE 6-17. PERCENT REDUCTION OF TCLP LEAD
BY TREATMENT WITH S/S
Portland cement Kiln dust and fly Fly ash and quick
(100%) ash (2;1) lime (3;2)
Binder/soil", Binder/soil, Binder/soil,
45% 139.5% 77.5%
TCLP Lead > 99.76 98.21 99.41
presents the percentage reduction of teachable lead in the soil matrix upon curing with
the three modified binder mixes. Calculations were based on average levels of TCLP
lead in the binder/soil mixtures because of the inability to obtain an accurate com-
parison of individual pre- and posttreatment samples.
Though the three modified binder mixes showed the ability to stabilize lead after
a 28-day curing period, the long-term ability to maintain lead stabilization is not known.
As discussed previously, cellulose molecules present in the organic mass will undergo
oxidative reactions, in the presence of alkali, to form acid groups. However, the
duration or extent to which these reactions take place in the binders is not known. It
is possible for oxidative reactions to continue occurring after the 28-day curing period.
i
If this is the case, then it is possible that alkali present in the binders may still be used
to neutralize acid groups formed during the oxidative reactions. This in turn would
result in lead being freed up and eventually leaching out of the binder mixture.
A comparison of ashed soil and nonashed soil treated by portland cement at a
binder-to-soil ratio of 20 percent indicates the organic content of the soil has a direct
impact on the effectiveness of the S/S treatment process. The S/S treatment showed
the ability to stabilize lead more effectively in ashed soil, as indicated, by the lower
teachable lead levels in the soil. Table 6-17 presents a comparison of the results
obtained for the ashed and nonashed soil treated with portland cement at a binder-to-
soil ratio of 20 percent
6-26
-------
TABLE 6-18. COMPARISON OF TCLP LEAD CONCENTRATIONS IN
ASHED AND NONASHED SOIL TREATED WITH PORTLAND CEMENT
AT A BINDER-TO-SOIL RATIO OF 20 PERCENT
Nonashed
soil
Ashed soil
Pretreatment soil, mg/1
Posttreatment monoliths, mg/L
Percent reduction
93
14
84.95
117
<0.2
99.83
6.2 CS&D Constituents
Prior to treatment, samples were collected to characterize the soil by analyzing
for volatile organics, semivolatile organics, organochlorine pesticides, brgano-
phosphorus insecticides, phenoxyacetic acid herbicides, alcohols, total metals, TCLP
metals, oil and grease, total organic carbon, total organic halogens, chloride, cyanide,
fluoride, sulfate, sulfide, and pH. Table 4-3 lists the methods used to analyze for these
parameters. Table 6-19 presents the analytical results for the CS&D constituents
detected in the treatment soil matrix. Of special note are the results for total organic
carbon and pH. The pH was measured at 4.3 standard units, which indicates a soil
acidic in nature. The total organic carbon was measured at 170,000 rrjg/kg. The
organic carbon content consisted primarily of naturally occurring humic material. The
complete data package for all analyses performed on the treatment soil during the
study is presented in Appendix XL ;
6-27
-------
TABLE 6-19. ANALYTICAL RESULTS FOR CS&D CONSTITUENTS
DETECTED IN THE TREATMENT SOIL MATRIX
(rag/kg)
Volatile orqanics
Methylene chloride 0.053
Acetone 0.071
Toluene . 0.01
Tn'chlorofluoromethane ; 0.004 Ja
Metals (total)
Aluminum 6700
Arsenic 13
Barium 86
Cadmium 0.65
Chromium 10
Cobalt 8.5
Copper 46
Iron i 21,000
Lead 21,000
Magnesium \ 940
Manganese 890
Mercury 0.3
Nickel 10
Potassium 540
Sodium 100
Vanadium 8.2
Zinc b 110
Metals (TCLP1
Barium 0.41
Cadmium 0.007
Chromium 0.033
Lead 91
Mercury ' 0.0002
(continued)
6-28
-------
TABLE 6-19 (contr)
Inorganics and other parameters
Fluoride 140
Cyanide 3
Sulfate 1,000
Sulfide 930
Chloride 1.5 mg/L
TOX 90
TOC • 170,000
pH 4.3 S.U.
Oil and grease 0.23 %
i
Percent moisture ; 27.7:%
a Estimated value of compound detected below specified
detection limit.
TCLP data reported in mg/L.
6-29
-------
-------
SECTION?
QUALITY ASSURANCE/QUALITY CONTROL MEASURES
This section describes the quality assurance/quality control (QA/QC) measures
associated with the sampling and analysis activities. Sample tracking information is
provided in Table 6-1. Analytical methods are listed in Table 4-3 and references for
these methods are footnoted at the bottom of this table. This section describes the
process for determining the detection limits used in the study. Also included are the
accuracy and precision data, results of analyses of blanks associated with the
tresttment samples, problems encountered during the analysis of the treatment
samples, and a discussion of the modifications made to established analytical
methods. ' i •
7.1 Method Detection Limit for TCLP Lead !
The method detection limit (MDL) for lead was determined in accordance with
40 CFR 136. A low-level standard estimated to be 3 to 5 times the detection level was
analyzed in seven replicate samples over three nonconsecutive days. This resulted in
21 replicate samples from which the standard deviation for lead was calculated. This
standard deviation was multiplied by 3 to determine the detection limit.; The MDL for
TCLP lead by ICP is 0.2 mg/L. i
7.2 Accuracy Data
Accuracy data were calculated from the analysis of matrix spike/matrix spike
duplicate samples. Accuracy is expressed as the percent recovery for the constituents
spiked into the sample in known quantities. The following formula was used to
calculate these values: i
7-1
-------
(C — C )
Percent Recovery = 100
where Cj = Value of spiked aliquot
C0 = Value of unspiked aliquot
Ct = Value of spike added.
As stated in the SAP, the QA objective for accuracy (percent recovery) was
specified to be in the range of 20 to 200 percent. Table 7-1 presents the percent
recoveries calculated from matrix spike/matrix spike duplicate samples for TCLP lead.
Accuracy in lead analysis was excellent; recoveries ranged from 79 to 109 percent.
7.3 Precision Data
Precision data were calculated from the analysis of matrix spike/matrix spike
duplicate samples. Precision is expressed as the relative percent difference (RPD)
between the matrix spike and the matrix spike duplicate concentration values. The
following formula was used to calculate relative percent difference:
RPD .
-------
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7-3
-------
TABLE 7-4. BLANK DATA FROM THE ANALYSIS OF RAW SOIL SAMPLES
Methyl ene chloride
Acetone
2-Butanone
1,1,1 -Tri chl oroethane
4-Methyl -2-pentanone
1,1,2, 2-Tetrachl oroethane
Method blank
mg/kg
NDa
0.011
ND i
NO :
ND
ND
Method blank
VBLKY5 mg/L
ND
0.005 Jb
0.004 J
ND
0.003 J
0.001 J
Trip blank
mg/L
0.003 J
ND
ND
0.002 J
ND
ND
a ND = not detected. Analyte not detected above reported detection limit.
Estimated value for analyte detected below reported detection limits.
7-6
-------
SECTIONS
!
CORRESPONDENCE AND ACTIVITIES
Table 8-1 presents the activities and correspondence that were critical to the
outcome of this study. i
TABLE 8-1. CRITICAL ACTIVITIES AND CORRESPONDENCE
Date and type of
activity or
correspondence
Contact
Subject/Action
10/30/90
Site visit
11/28/90
Reporting
Meeting
12/3/90
Meeting
12/12/90
Reporting
1/11/91
Meeting
1/161/91
Reporting
2/20/91
Site visit
3/10-3/11/91
Testing
Chris Corbett,
U.S. EPA
Laurel Tomassoni,
ITAS-Cincinnati
Richard Lauch and Jon Herrmann,
U.S. EPA; D.'Keller and J.
Isenburg, Center Hill Facility
D. Keller and J. Isenburg. Center
Hill Facility
Richard Lauch
U.S. EPA
Richard Lauch and Jon Herrmann.
U.S. EPA; J. Isenburg, M. Lambert,
and S. Hayes, Center Hill Facility
Richard Lauch, U.S. EPA
Jerry Isenburg, Center Hill
Facility
Jerry Isenburg, Center Hill
Facility
ITEP sent sampling team to drum up soil
from Brown's Battery site for treatment
studies. Soil samples were delivered to
ITAS-Cincinnati for characterization, and
approximately 20 gallons ofjsoil were
delivered to the Center Hill Research
Facility for S/S testing.
ITEP received analytical data from
characterization sample. Lead concen-
trations ranged from 5,460 to 25,800 ppm.
!
Agreed to homogenize four pails of soil to
obtain overall sample having a lead
concentration of approximately 1.5%.
Discussed procedures for GANC, MANC, and
FAD tests used by the Center Hill Facility
in their S/S studies.
Submitted draft SAP review for S/S
treatability study to U.S. EPA for review.
Discussed QA concerns and minor issues
expressed by Guy Simes during review of
SAP. :
Submitted final SAP for S/S treatability
testing to U.S. EPA.
i
Initial homogenization and sampling of the
soil was begun. Soil homogenized and
separated into batches for testing and
sampli ng.
Binder mixes were prepared for S/S
treatment process.
(continued)
8-1
-------
TABLE 8-1 (cont.)
Date and type of
activity or
correspondence
Contact
Subject/Action
3/11/91
Testing
4/5/91
Reporting
4/11/91
Meeting
4/17/91
Testi ng
5/1/91
Reporting
5/24/91
Meeting
5/29/91
Meeting
6/6/91
Testing
7/1/91
Testing
7/5/91
Testing
7/12/91
Testing
8/1/91
Reporting
8/14/91
Reporting
9/91
Reporting
Laurel Tomassoni, ITAS-Cindnnati
Laurel Tomassoni, ITAS-Cincinnati
Jerry Isenburg and Sam Hayes.
Center Hill Facility
Laurel Tomassoni, ITAS-Cincinnati
Laurel Tomassoni, ITAS-Cincinnati
Jerry Isenburg, Center Hill
Facility
Richard Lauch and Jon Herrmann, ,
U.S. EPA; Jerry Isenburg, Center
Hill Facility
Jerry Isenburg, Center Hill
Faci1i ty
Laurel Tomassoni, ITAS-Cincinnati
Jerry Isenburg, Center H111
Facility
Laurel Tomassoni, ITAS-Cincinnati
Laurel Tomassoni, ITAS-Cincinnati
Laurel Tomassoni, ITAS-Cincinnati
Richard Lauch, U.S. EPA
TCLP extracts from untreated soil delivered
to ITAS for analysis.
Analytical data for TCLP extracts from
untreated soil delivered to ITEP.
Curing of S/S monoliths from Phase I
completed.
TCLP extracts from posttreatment samples
delivered.
Analytical data from Phase I of the S/S
treatment studies delivered to ITEP.
Discussed failure of binder mixes to
stabilize lead and the potential for
conducting further tests.
Approval given to conduct further studies'
on treating soil by S/S.
Binder mixes prepared for conducting
additional tests.
TCLP extracts from untreated soil samples
delivered to ITAS for analysis.
Curing of S/S monoliths from Phase II
completed.
TCLP extracts from posttreatment samples
delivered to ITAS for analysis.
Analytical data for TCLP extracts from
untreated soil delivered to ITEP.
Analytical data for TCLP extracts from
Phase II posttreatment samples delivered to
ITEP.
ITEP submitted draft OER for review.
8-2
------- |