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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                                                      JD
                                                       CO
                                                      4->
                                                       ro
                                                       O)
                                                       S-
                                                       cu
                                                       S-
                                                       o
                                                       CO
                                                       c
                                                       O
                                                       C0
                                                       U
                                                       O
                                                      O>
                                                      "o.
                                                      M
                                                      CO
                                                      o>
                                                      2!
                                                      CM
                                                      3
                                                      Ol
2-3

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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.

-------

BAUD SIEVE NUMBERS - HYDROMETER
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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
     79.4
     61.3
     52.1
     34.8
     25.4
     22.8
     18.9
     12.4
      9.6
               -6

-------
       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
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is!
  O
  co

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    CO
        
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PROPORTIONING a
MIXING
soil/binder mix
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ETERS

each mi
TEST PARAM

Total Pb (FAD) for
pH of each mix
                                                       co
                                                       |
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  £
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                     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

                                     5-1                              '

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-------
minimum pH  would be the most acidic leadhate produced by a binder that had lead
concentrations less than 5 mg/L  The maximum pH would be the most alkaline
leachate produced by a binder that had lead concentrations less than 5 mg/L  The
optimum pH would be one that had the lowest concentration of lead in its leachate.
Based on information in Figure 5-6, the optimum portland cement binder would be one
that produced a leachate with a pH of approximately 9.75. However, portland cement
binder mixtures that produced leachates with a pH in the range of 8.0 to 11.25 would
be predicted to work in immobilizing lead in the Brown's Battery soil.
      Because TCLP analyses are based on leachates produced by the addition of 2
acetic acid equivalents per kilogram of dry sample, the optimum binder mixture would
be the mixture that produced a leachate at the optimum pH upon addition of the acid
equivalents.  Based on information in Figure 5-6, a 20% portland cement mixture
would produce a leachate with a pH of 9.75 upon addition of 2 equivalents of acetic
acid per kilogram of sample.  The other binder mixtures were determined in the same
manner.  For each of the three binders, two, mix ratios were calculated on a dry waste
weight.  One of the two mix ratios was at thb optimum ratio as predicted by the GANG
curves in Figures 5-6, 5-7, and 5-8. The other mix ratio was prepared at a strength
approximatley four-fifths of the optimum ratio.  The six mix ratios as calculated from
the GANG curves were:
            16% portland cement
            20% portland cement
            8.5% quicklime and 12.75% fly ash
            10.5% quicklime and 15.75% fly ash
            24% kiln dust and 12% fly ash;
            28% kiln dust and 14% fly ash
      The mix sheets  used to record the  preparation of Stabilization  Mixes 1 through
6 are listed in Appendix X, along with the raw data for the GANG. The water added
for casting and the flow achieved are shown in Table 5-1. To determine if enough
binder had been added, the pH of a one-to-one dilution of the mix with deionized
water was analyzed. A pH between 11 and 12 indicated the binder added was
enough to stabilize the mixture. The amount of water added to the binder/soil mix
                                     5-10

-------
 was based on ASTM Methods C230 and C109, Section 10.3, to obtain a workable
 mixture of 60 to 85 percent flow, as determined by previous experience in working with
 concrete slumps.
                TABLE 5-1.  WATER REQUIREMENTS AND FLOW ACHIEVED
                                MIXES 1  THROUGH 6
Mix
No,
1
2
3
4
5
6
Binder recipea
16% pc
20% pc
8.5% ql/12.75%
fa
10.5% ql/15.75%
fa
24% ckd/12% fa
28% ckd/14% fa
Weight
waste
dry,
9
3000
2000
2000
2000
2000
2000
Weight
binders,
g
480
400
425
525
720
840
Weight
water,
g
2193.9
1457.3
1577.2
1540.6
1580
1561.2
Ratio
of H,0
toz
solids
0.630
0.607
0.650
0.610
0.581
0.550
Flow
table,
%
;65
66
76
66
i71
60
pH of
50/50
mix/H,0
11.62
11.64
12.49
12.51
12.39
12.45
   pc = portland  cement
   ckd/fa = cement  kiln dust/fly ash                       .     '
   ql/fa = quicklime/fly ash
5.1.2 New Mix Design
      Based on the TCLP analytical results (Section 6), it was determined that the
initial mixes used in the study failed to meet the regulatory limits for lead (5 mg/L).
Based on information provided in the initial characterization of the soil, the most
reasonable explanation for the failure of the original binder mixes was determined to
be the organic carbon content of the soil. The total organic carbon (TQC) content of
the Brown's Battery Breaking soil was measured at 17%. Based on personal
observation, as well as analytical data, the organic content was believed to be mainly
humus material.  Alkali present in the binder mixes may have acted as catalysts for
                         ••                              '         !
oxidative reactions between atmospheric oxygen and cellulose molecules  present in
the humus material. The products of these reactions are acid groups. The alkali
present in the mixes would have to neutralize the acid groups in the humus material
rather than to stabilize the lead present in the soil.                    I
                                      5-11

-------
      Though other reasons for the failure of the original binder mixes to stabilize lead
 may have existed, the only reasonable explanation was the organic content of the soil,
 based on the information available. Therefore an additional S/S study was performed
                                       i
 to determine the effect the organic carbon content had on soil stabilization capacity.
                                       I
 In addition, results of further GANG tests indicated that higher binder-to-soil ratios
 would improve the stabilization capacity b>! decreasing lead leachate levels. As a
 result, additional S/S studies were performed to determine the optimum binder mixes
 for the Brown's Battery Breaking soil.
      Assuming that the waste was more acidic than the GANG test result on the raw
 soil indicated, a correction factor was developed to compensate for this.  The actual
 pH of the leachate at 2 eq/kg of acid leachant was matched to a multiple of the
 original GANG test result at 2 eq/kg.  That .multiple was used to adjust the entire
 GANG prediction curve for the  proposed mixes.
      The water content was also included in the TCLP target value for the mix design
 based on the water contents of the previous  mixes. The water required for flow in the
 original six mixes was unknown until the mixes were actually produced. The water
 content affects the target equivalents per kilogram (eq/kg) for the leaching test. The
TCLP uses a 2 eq/kg wet sample. The GA^NC is based on the eq/kg dry sample. For
 conversion to eg/kg dry, the eq/kg wet is multiplied by the ratio of wet weight to dry
weight for the sample tested. A reasonable and conservative guess would be that the
overall water percentage would at  least be the same percentage that is in the waste as
delivered. The target eq/kg  would be

                      2 eq/kg wet x -I3!5-  = 2.75 eq/kg dry

      The new mix ratios selected were 45 percent portland cement for Mix 7; 93
percent cement kiln dust with 46.5 percent fly ash (i.e., more binder than dry waste
                                       i
solids) for Mix 8; 31 percent  dolomitic quicklime with 46.5 percent fly ash for Mix 9;
(see Appendix X for mix sheets).
                                      5-12

-------
       The last mix (Mix 10) used soil that had been heated before treatment to reduce
 the organic carbon content with 20 percent portland cement based on the soil dry
 weight before ignition.  This choice is based on the concept that the organic material
 is using the alkalinity of the binder with time beyond the 48 hours of the GANG test.  If
 the organic material is ashed or burned to a nonreactive residue, such reactions
 should cease and the original GANG estimates of binder needs should; be nearly
 correct.
       Table 5-2 shows the water required, flow achieved,  and water diluted pH of the
 mixes.                                                           ;
                TABLE  5-2.   WATER REQUIREMENTS AND FLOW ACHIEVED
                               MIXES 7 THROUGH 10
Mix
No.
7
8
9
10
Binder
recipe
45% pc
31% ql/46.5%
fa
93% ckd/46.5%
fa
20% pc
Weight
waste
dry,
9
2000
2000
2000
1660
Weight
binders,
g
900
1550
2790
400
Weight
water,
g
1652.4
1966.9
2462.7
927.3
Ratio
of H90
to*
solids
0.570
0.554
0.514
0.450
Flow
table,
%
75l5
77
79.5
78.5
pH of
50/50
mix/H,0
11.87
12.61
12.57
11.6
   pc = portland cement
   ql/fa = quick! ime/flyash
   ckd = cement kiln  dust
5.2   Set Testing
6.2.1  Vicat and Cone Tests for Set
      During the curing of the cast samples, the set was checked on a shallow disk
of material by using a Vicat apparatus commonly used to test cement for setting
qualities. A penetration of 28 mm is considered to be infinite (00), representing the
same consistency as the original mix. A penetration of 0 mm indicates;set is com-
pletes, and it usually represents more than 50 psi unconfined compressive strength.
Table 5-3 lists the Vicat values at various times for Mixes 1 through 10. i

                                     5-13

-------
TABLE 5-3. SETTING MEASUREMENTS ON MIXES 1 TO 10
Mix
No.
1






2






3



4





5
6
7C


Time since
casting,
days
2
3
4
7
8
9
10
2
3
4
7
8
9
10
0 to 28
28
29
30
0 to 23
24
25
28
29
30
Entire cure
Entire cure
1
8
15
(continued)
Vicat Cone
penetration, Cone penetrometer, UCS,
mm mm kPa
28 = 00a
0 to 1
0 to 1
0
--
i

. 23
0
0
0
1
--
__
00
00
[
00
23
00
26 i
24 '
22
13
13
00
oo !
00
0
0
5-14
--
--
17
19
23
26
23b
--
--
25
33
36
36
33b
--
9
10
6
--
10
12
14
11
--
--
--
--
'
--

,
__.
2090 .
2340
2830
3200
2830b
--
--
3080
4070
4430
4430
4070b
--
1110
1220
738
--
738
883
1034
814
•
--
•
--
--
--


-------
 TABLE 5-3 (continued)
Mix
No.

8C





9C





10C



Time since
casting,
days
18
1
8
15
18
24
28
1
8
15
18
24
28
1
8
15
18
Vicat
penetration, Cone penetrometer,
mm mm
0
00
00
18
18 --
10
3 --
00
00
18
12
11 --
6
--
0
0
0
Cone
UCS,
kPa
_ _
i
;
1 • --
'
--
— .
1
'
i
;
;
—
:
'
;
--
  00 » infinite.  Cast did not set.
b
  Decreases due to sample loss of integrity from previous multi
  pie cone penetrations of the cast disk.

c Cone penetrometer tests not performed on Mixes 7 through 10
  due to satisfactory set of these binders.
                               5-15

-------
      Another measure of penetration resistance (and thus set) that is more related to
compressive strength is the cone penetrometer.  This test is usually applied after the
                                       r
Vicat starts to decrease significantly.  The cone penetrometer values and the projected
unconfined compressive strengths (UCS) are listed for Mixes 1  through 10 in
Table 5-3.
5.2.2 Unconfined Compressive Strength, Moisture Content, Wet and Dry Densities
      Table 5-4 shows the unconfined compressive strength of the 2-in.-diameter by
4-ln.-high cylinders.  The samples made from Mixes 5 and 6 with cement kiln dust and
fly ash did not have a strength because they did not set (see Table 5-3).  Also
included in Table 5-4 is the moisture content, wet density, and dry density.  The dry
density was  calculated by the following equation:
                             DD  = WD  *  (1 -  % M)
where       DD    = Dry density
            WD    = Wet density
            % M   = Percent moisture content
Appendix V includes the detailed raw data on these tests.
                                     5-16

-------
          TABLE 5-4.  PHYSICAL CHARACTERISTICS OF CAST SAMPLES
Mix
No.
1
2
3
4
7
8
9
10
Binder recipe3
16% pc
20% pc
8.5% ql + 12.75%
fa
10.5% ql +
15.75% fa
45% pc
31% ql + 46.5%
fa
93% ckd + 46.5%
fa
20% pc
Unconfined
compress ive
strength,
kPa
462
503
241
207
2612
197
178
1618
Moisture
content,
60
55
58
55
~b
--
--
--'
Wet density,
kg/m3
1480
1510
1460
1490
--
--
--
--
i
Dry density-,
1 kg/m3
590
: 675
609
665
--
• :
i
'
pc = port!and cement
ql + fa = quicklime + fly ash
ckd + f a = cement kiln dust + fly ash

Data not available for these tests.
                                  5-17

-------

-------
                                  SECTION 6
                            ANALYTICAL RESULTS

      This section presents the results of the analyses for the critical contaminant
(TCILP lead) performed on pre- and posttreatment samples to evaluate the perfor-
mance of the S/S treatment process. Also presented are results of the analyses for
volatile organics, semivolatile organics, organochlorine pesticides, organophosphorus
insecticides, phenoxyacetic acid herbicides, total metals, TCLP metals, FAD lead, TOG,
TOX, oil and grease, moisture content, cyanide, fluoride, sulfide, sulfate, and chloride.
The TCLP and FAD extractions were performed at the CHF by University of Cincinnati
persionnel.  All analyses were performed by ITAS-Cincinnati.  The method for analyzing
TCLP lead and FAD lead are described in Subsection 4.2; the other analytical methods
used are listed in Table 4-3.
      Table 6-1 presents the IT field sample coding and the dates samples were
TCLP-extracted or FAD-extracted, received by ITAS-Cincinnati, extracted by ITAS-
Cincinnati, and analyzed in the laboratory.                          ;
                                                                i   .
6.1   Lead
6.1.1  Analytical Methodology                                     \
      All lead extracts were analyzed by inductively coupled argon plasma spectro-
scopy (ICAP) in accordance with Method 6010 in SW-846.  Table 6-2 shows the
instrument conditions used on the Perkin-Elmer Plasma II Emission Spectrometer.
Quantitative analysis was based on the intensities of element-specific atomic-line emis-
sions, which are monitored by photomultiplier tubes.  Matrix spike/matrix spike
                                      6-1

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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
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    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
    

    -------